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Sample records for synthesis raman ft-ir

  1. Vibrational microspectroscopy of food. Raman vs. FT-IR

    DEFF Research Database (Denmark)

    Thygesen, Lisbeth Garbrecht; Løkke, Mette Marie; Micklander, Elisabeth

    2003-01-01

    . The high spatial resolution makes it possible to study areas down to approximately 10x10 mum with FT-IR microspectroscopy and approximately 1 x 1 mum with Raman microspectroscopy. This presentation highlights the advantages and disadvantages of the two microspectroscopic techniques when applied...

  2. 3-Iodobenzaldehyde: XRD, FT-IR, Raman and DFT studies.

    Science.gov (United States)

    Kumar, Chandraju Sadolalu Chidan; Parlak, Cemal; Tursun, Mahir; Fun, Hoong-Kun; Rhyman, Lydia; Ramasami, Ponnadurai; Alswaidan, Ibrahim A; Keşan, Gürkan; Chandraju, Siddegowda; Quah, Ching Kheng

    2015-06-15

    The structure of 3-iodobenzaldehyde (3IB) was characterized by FT-IR, Raman and single-crystal X-ray diffraction techniques. The conformational isomers, optimized geometric parameters, normal mode frequencies and corresponding vibrational assignments of 3IB were examined using density functional theory (DFT) method, with the Becke-3-Lee-Yang-Parr (B3LYP) functional and the 6-311+G(3df,p) basis set for all atoms except for iodine. The LANL2DZ effective core basis set was used for iodine. Potential energy distribution (PED) analysis of normal modes was performed to identify characteristic frequencies. 3IB crystallizes in monoclinic space group P21/c with the O-trans form. There is a good agreement between the theoretically predicted structural parameters, and vibrational frequencies and those obtained experimentally. In order to understand halogen effect, 3-halogenobenzaldehyde [XC6H4CHO; X=F, Cl and Br] was also studied theoretically. The free energy difference between the isomers is small but the rotational barrier is about 8kcal/mol. An atypical behavior of fluorine affecting conformational preference is observed. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. DFT, FT-IR, FT-Raman and vibrational studies of 3-methoxyphenyl boronic acid

    Science.gov (United States)

    Patil, N. R.; Hiremath, Sudhir M.; Hiremath, C. S.

    2018-05-01

    The aim of this work is to study the possible stable, geometrical molecular structure, experimental and theoretical FT-IR and FT-Raman spectroscopic methods of 3-Methoxyphenyl boronic acid (3MPBA). FT-IR and FT-Raman spectra were recorded in the region of 4000-400 cm-1 and 40000-50 cm-1 respectively. The optimized geometric structure and vibrational wavenumbers of the title compound were searched by B3LYP hybrid density functional theory method with 6-311++G (d, p) basis set. The Selectedexperimentalbandswereassignedandcharacterizedonthebasisofthescaledtheoreticalwavenumbersby their potential energy distribution (PED) of the vibrational modes obtained from VEDA 4 program. Finally, the predicted calculation results were applied to simulated FT-IR and FT-Raman spectra of the title compound, which show agreement with the observed spectra. Whereas, it is observed that, the theoretical frequencies are more than the experimental one for O-H stretching vibration modes of the title molecule.

  4. FT-IR, RAMAN AND DFT STUDIES ON THE VIBRATIONAL ...

    African Journals Online (AJOL)

    Department of Physics, Science Faculty, Anadolu University, Eskişehir, Turkey ... IR spectrum was recorded using Bruker Optics IFS66v/s FTIR spectrometer at a ... spectrum was obtained using a Bruker Senterra Dispersive Raman microscope.

  5. An FT-Raman, FT-IR, and Quantum Chemical Investigation of Stanozolol and Oxandrolone

    Directory of Open Access Journals (Sweden)

    Tibebe Lemma

    2017-12-01

    Full Text Available We have studied the Fourier Transform Infrared (FT-IR and the Fourier transform Raman (FT-Raman spectra of stanozolol and oxandrolone, and we have performed quantum chemical calculations based on the density functional theory (DFT with a B3LYP/6-31G (d, p level of theory. The FT-IR and FT-Raman spectra were collected in a solid phase. The consistency between the calculated and experimental FT-IR and FT-Raman data indicates that the B3LYP/6-31G (d, p can generate reliable geometry and related properties of the title compounds. Selected experimental bands were assigned and characterized on the basis of the scaled theoretical wavenumbers by their total energy distribution. The good agreement between the experimental and theoretical spectra allowed positive assignment of the observed vibrational absorption bands. Finally, the calculation results were applied to simulate the Raman and IR spectra of the title compounds, which show agreement with the observed spectra.

  6. Detection of metanil yellow contamination in turmeric using FT-Raman and FT-IR spectroscopy

    Science.gov (United States)

    Dhakal, Sagar; Chao, Kuanglin; Qin, Jianwei; Kim, Moon; Schmidt, Walter; Chan, Dian

    2016-05-01

    Turmeric is well known for its medicinal value and is often used in Asian cuisine. Economically motivated contamination of turmeric by chemicals such as metanil yellow has been repeatedly reported. Although traditional technologies can detect such contaminants in food, high operational costs and operational complexities have limited their use to the laboratory. This study used Fourier Transform Raman Spectroscopy (FT-Raman) and Fourier Transform - Infrared Spectroscopy (FT-IR) to identify metanil yellow contamination in turmeric powder. Mixtures of metanil yellow in turmeric were prepared at concentrations of 30%, 25%, 20%, 15%, 10%, 5%, 1% and 0.01% (w/w). The FT-Raman and FT-IR spectral signal of pure turmeric powder, pure metanil yellow powder and the 8 sample mixtures were obtained and analyzed independently to identify metanil yellow contamination in turmeric. The results show that FT-Raman spectroscopy and FT-IR spectroscopy can detect metanil yellow mixed with turmeric at concentrations as low as 1% and 5%, respectively, and may be useful for non-destructive detection of adulterated turmeric powder.

  7. FT-IR, FT-Raman and UV-visible spectra of potassium 3-furoyltrifluoroborate salt

    Science.gov (United States)

    Iramain, Maximiliano A.; Davies, Lilian; Brandán, Silvia Antonia

    2018-04-01

    The potassium 3-furoyltrifluoroborate salt has been experimentally characterized by means of FT-IR, FT-Raman and UV-Visible spectroscopies. Here, the predicted FT-IR, FT-Raman and UV-visible spectra by using theoretical B3LYP/6-31G* and 6-311++G** calculations show very good correlations with the corresponding experimental ones. The solvation energies were predicted by using both levels of calculations. The NBO analyses reveal the high stability of the salt by using the B3LYP/6-31G* level of theory while the AIM studies evidence the ionic characteristics of the salt in both media. The strong blue colour observed on the K atom by using the molecular electrostatic potential mapped suggests that this region act as typical electrophilic site. The gap values have revealed that the salt in gas phase is more reactive than in solution, as was reported in the literature while, the F13⋯H6 interaction together with the Ksbnd O bond observed by the studies of their charges could probably modulate the reactivities of this salt in aqueous solution. The force fields were computed with the SQMFF methodology and the Molvib program to perform the complete vibrational analysis. Then, the 39 vibration normal modes classified as 26 A'+ 13 A″ were completely assigned and their force constants are also reported.

  8. Synthesis, spectroscopic (FT-IR, FT-Raman, NMR, UV-Visible), NLO, NBO, HOMO-LUMO, Fukui function and molecular docking study of (E)-1-(5-bromo-2-hydroxybenzylidene)semicarbazide

    Science.gov (United States)

    Raja, M.; Raj Muhamed, R.; Muthu, S.; Suresh, M.

    2017-08-01

    The title compound, (E)-1-(5-bromo-2-hydroxybenzylidene)semicarbazide (15BHS) was synthesized and characterized by FT-IR, FT-Raman, UV, 1HNMR and 13CNMR spectral analysis. The optimized molecular geometry, the vibrational wavenumbers, the infrared intensities and the Raman scattering activities were calculated by using density functional theory(DFT) B3LYP method with 6-311++G(d,p) basis set. The detailed interpretation of the vibrational spectra has been carried out by VEDA program. The calculated HOMO and LUMO energies show that charge transfer within the molecule. Stability of the molecule arising from hyperconjugative interactions, charge delocalization have been analyzed using natural bond orbital analysis (NBO). The first order hyperpolarizability, Molecular electrostatic potential (MEP) and Fukui functions were also performed. To study the biological activity of the investigation molecule, molecular docking was done to identify the hydrogen bond lengths and binding energy with different antifungal proteins. The thermodynamic properties (heat capacity, entropy, and enthalpy) of the 15BHS at different temperatures have been calculated.

  9. (2E)-1-(5-Chlorothiophen-2-yl)-3-{4-[(E)-2-phenylethenyl]phenyl}prop-2-en-1-one: Synthesis, XRD, FT-IR, Raman and DFT studies.

    Science.gov (United States)

    Parlak, Cemal; Ramasami, Ponnadurai; Kumar, Chandraju Sadolalu Chidan; Tursun, Mahir; Quah, Ching Kheng; Rhyman, Lydia; Bilge, Metin; Fun, Hoong-Kun; Chandraju, Siddegowda

    2015-01-01

    A novel (2E)-1-(5-chlorothiophen-2-yl)-3-{4-[(E)-2-phenylethenyl]phenyl}prop-2-en-1-one [C21H15ClOS] compound has been synthesized and its structure has been characterized by FT-IR, Raman and single-crystal X-ray diffraction techniques. The conformational isomers, optimized geometric parameters, normal mode frequencies and corresponding vibrational assignments of the compound have been examined by means of HF, MP2, BP86, BLYP, BMK, B3LYP, B3PW91, B3P86 and M06-2X functionals. Reliable vibrational assignments and molecular orbitals have been investigated by the potential energy distribution and natural bonding orbital analyses, respectively. The compound crystallizes in the triclinic space group P-1 with the cis-trans-trans form. There is a good agreement between the experimentally determined structural parameters and vibrational frequencies of the compound and those predicted theoretically using the density functional theory with the BLYP and BP86 functionals. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Synthesis, electronic structure investigation of 3-pentyl-2,6-di(furan-2-yl)piperidin-4-one by FT-IR, FT-Raman and UV-Visible spectral studies and ab initio/DFT calculations.

    Science.gov (United States)

    Arockia Doss, M; Savithiri, S; Rajarajan, G; Thanikachalam, V; Anbuselvan, C

    2015-12-05

    FT-IR and FT-Raman spectra of 3-pentyl-2,6-di(furan-2-yl) piperidin-4-one (3-PFPO) were recorded in the solid phase. The structural and spectroscopic analyses of 3-PFPO were made by using B3LYP/HF level with 6-311++G(d, p) basis set. The fundamental vibrations are assigned on the basis of the total energy distribution (TED) of the vibrational modes, calculated with scaled quantum mechanics (SQM) method and PQS program. Comparison of the observed fundamental vibrational frequencies of 3-PFPO with calculated results by HF and DFT methods indicates that B3LYP is superior to HF method for molecular vibrational problems. The electronic properties such as excitation energies, oscillator strength, wavelengths and HOMO-LUMO energies were obtained by time-dependent DFT (TD-DFT) approach. The polarizability and first order hyperpolarizability of the title molecule were calculated and interpreted. The hyperconjugative interaction energy (E((2))) and electron densities of donor (i) and acceptor (j) bonds were calculated using NBO analysis. In addition, MEP and atomic charges of carbon, nitrogen, oxygen and hydrogen were calculated using B3LYP/6-311++G(d, p) level theory. Moreover, thermodynamic properties (heat capacities, entropy and enthalpy) of the title compound at different temperatures were calculated in gas phase. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Synthesis, molecular structure, FT-IR, Raman, XRD and theoretical investigations of (2E)-1-(5-chlorothiophen-2-yl)-3-(naphthalen-2-yl)prop-2-en-1-one.

    Science.gov (United States)

    Chidan Kumar, Chandraju Sadolalu; Fun, Hoong Kun; Parlak, Cemal; Rhyman, Lydia; Ramasami, Ponnadurai; Tursun, Mahir; Chandraju, Siddegowda; Quah, Ching Kheng

    2014-11-11

    A novel (2E)-1-(5-chlorothiophen-2-yl)-3-(naphthalen-2-yl)prop-2-en-1-one [C17H11ClOS] compound has been synthesized and its structure has been characterized by FT-IR, Raman and single-crystal X-ray diffraction techniques. The isomers, optimized geometrical parameters, normal mode frequencies and corresponding vibrational assignments of the compound have been examined by means of the density functional theory method, employing, the Becke-3-Lee-Yang-Parr functional and the 6-311+G(3df,p) basis set. Reliable vibrational assignments and molecular orbitals have been investigated by the potential energy distribution and natural bonding orbital analyses, respectively. The compound crystallizes in the monoclinic space group P2₁/c with the unit cell parameters a=5.7827(8)Å, b=14.590(2)Å, c=16.138(2)Å and β=89.987 (°). The CC bond of the central enone group adopts an E configuration. There is a good agreement between the theoretically predicted structural parameters and vibrational frequencies and those obtained experimentally. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. Evaluation of Turmeric Powder Adulterated with Metanil Yellow Using FT-Raman and FT-IR Spectroscopy

    Directory of Open Access Journals (Sweden)

    Sagar Dhakal

    2016-05-01

    Full Text Available Turmeric powder (Curcuma longa L. is valued both for its medicinal properties and for its popular culinary use, such as being a component in curry powder. Due to its high demand in international trade, turmeric powder has been subject to economically driven, hazardous chemical adulteration. This study utilized Fourier Transform-Raman (FT-Raman and Fourier Transform-Infra Red (FT-IR spectroscopy as separate but complementary methods for detecting metanil yellow adulteration of turmeric powder. Sample mixtures of turmeric powder and metanil yellow were prepared at concentrations of 30%, 25%, 20%, 15%, 10%, 5%, 1%, and 0.01% (w/w. FT-Raman and FT-IR spectra were acquired for these mixture samples as well as for pure samples of turmeric powder and metanil yellow. Spectral analysis showed that the FT-IR method in this study could detect the metanil yellow at the 5% concentration, while the FT-Raman method appeared to be more sensitive and could detect the metanil yellow at the 1% concentration. Relationships between metanil yellow spectral peak intensities and metanil yellow concentration were established using representative peaks at FT-Raman 1406 cm−1 and FT-IR 1140 cm−1 with correlation coefficients of 0.93 and 0.95, respectively.

  13. FT-IR, FT-Raman spectra and DFT calculations of melaminium perchlorate monohydrate

    Science.gov (United States)

    Kanagathara, N.; Marchewka, M. K.; Drozd, M.; Renganathan, N. G.; Gunasekaran, S.; Anbalagan, G.

    2013-08-01

    Melaminium perchlorate monohydrate (MPM), an organic material has been synthesized by slow solvent evaporation method at room temperature. Powder X-ray diffraction analysis confirms that MPM crystal belongs to triclinic system with space group P-1. FTIR and FT Raman spectra are recorded at room temperature. Functional group assignment has been made for the melaminium cations and perchlorate anions. Vibrational spectra have also been discussed on the basis of quantum chemical density functional theory (DFT) calculations using Firefly (PC GAMESS) version 7.1 G. Vibrational frequencies are calculated and scaled values are compared with experimental values. The assignment of the bands has been made on the basis of the calculated PED. The Mulliken charges, HOMO-LUMO orbital energies are analyzed directly from Firefly program log files and graphically illustrated. HOMO-LUMO energy gap and other related molecular properties are also calculated. The theoretically constructed FT-IR and FT-Raman spectra of MPM coincide with the experimental one. The chemical structure of the compound has been established by 1H and 13C NMR spectra. No detectable signal was observed during powder test for second harmonic generation.

  14. FT-Raman and FT-IR studies of 1:2.5 piroxicam: β-cyclodextrin inclusion compound

    Science.gov (United States)

    Bertoluzza, A.; Rossi, M.; Taddei, P.; Redenti, E.; Zanol, M.; Ventura, P.

    1999-05-01

    The FT-Raman and FT-IR spectra of amorphous 1:2.5 piroxicam (P): β-cyclodextrin (βCD) inclusion compound (PβCD) are presented and discussed in comparison with the spectra of the three main modifications of piroxicam (α,β and monohydrate). In the 1700-1200 cm -1 FT-Raman spectrum of 1:2.5 PβCD inclusion compound the bands of βCD are weak and covered by those stronger of piroxicam, differently from the FT-IR spectrum where the bands of βCD are stronger, so covering a large part of the spectrum. Typical FT-Raman marker bands are assigned for the characterization of the three modifications of piroxicam. The FT-Raman spectrum of 1:2.5 PβCD inclusion compound predominantly shows the bands at about 1465 and 1400 cm -1 of the monohydrate, indicating that piroxicam assumes the zwitterionic structure stabilized by interaction with βCD via electrostatic and hydrogen bonds. The dipolar character of 1:2.5 PβCD inclusion compound improves the solubility and the dissolution rate of piroxicam and thus its rate of absorption.

  15. Sensing the Structural Differences in Cellulose from Apple and Bacterial Cell Wall Materials by Raman and FT-IR Spectroscopy

    Science.gov (United States)

    Szymańska-Chargot, Monika; Cybulska, Justyna; Zdunek, Artur

    2011-01-01

    Raman and Fourier Transform Infrared (FT-IR) spectroscopy was used for assessment of structural differences of celluloses of various origins. Investigated celluloses were: bacterial celluloses cultured in presence of pectin and/or xyloglucan, as well as commercial celluloses and cellulose extracted from apple parenchyma. FT-IR spectra were used to estimate of the Iβ content, whereas Raman spectra were used to evaluate the degree of crystallinity of the cellulose. The crystallinity index (XCRAMAN%) varied from −25% for apple cellulose to 53% for microcrystalline commercial cellulose. Considering bacterial cellulose, addition of xyloglucan has an impact on the percentage content of cellulose Iβ. However, addition of only xyloglucan or only pectins to pure bacterial cellulose both resulted in a slight decrease of crystallinity. However, culturing bacterial cellulose in the presence of mixtures of xyloglucan and pectins results in an increase of crystallinity. The results confirmed that the higher degree of crystallinity, the broader the peak around 913 cm−1. Among all bacterial celluloses the bacterial cellulose cultured in presence of xyloglucan and pectin (BCPX) has the most similar structure to those observed in natural primary cell walls. PMID:22163913

  16. Comparative FT-Raman, FT-IR and colour shifts spectroscopic evaluation of gamma irradiated experimental models of oil paintings

    International Nuclear Information System (INIS)

    Manca, M.M.; Virgolici, M.; Cutrubinis, M.; Moise, I.V.; Ponta, C.C.; Negut, C.D.; Stanculescu, I.R.; Bucharest University

    2011-01-01

    Complete text of publication follows. The present study follows the changes of gamma irradiated historic pigments and experimental models of oil paintings with non-destructive and non-contact spectroscopic analytical techniques which are the only ones accepted by the conservators/restorers community. Molecular structure characterization was performed by FT-IR / Raman spectroscopy using a Bruker Vertex 70 class equipped with two mobile probes: a MIR fibre module for MIR probes (with LN2 cooled detector) and a Raman RAM II module (LN2 Ge detector) with a RAMPROBE fibre. Colour was measured by a portable reflectance spectrophotometer (Miniscan XE Plus, HunterLab) in diffuse/8 deg geometry with a beam diameter of 4 mm and specular component included. Correlations between colour shifts and changes in molecular structure induced by gamma irradiation were further investigated.

  17. Characterisation of 1,3-diammonium propylselenate monohydrate by XRD, FT-IR, FT-Raman, DSC and DFT studies

    Science.gov (United States)

    Thirunarayanan, S.; Arjunan, V.; Marchewka, M. K.; Mohan, S.; Atalay, Yusuf

    2016-03-01

    The crystals of 1,3-diammonium propylselenate monohydrate (DAPS) were prepared and characterised X-ray diffraction (XRD), FT-IR, FT-Raman spectroscopy, and DFT/B3LYP methods. It comprises protonated propyl ammonium moieties (diammonium propyl cations), selenate anions and water molecule which are held together by a number of hydrogen bonds and form infinite chains. The XRD data confirm the transfer of two protons from selenic acid to 1,3-diaminopropane molecule. The DAPS complex is stabilised by the presence of O-H···O and N-H···O hydrogen bonds and the electrostatic interactions as well. The N···O and O···O bond distances are 2.82-2.91 and 2.77 Å, respectively. The FT-IR and FT-Raman spectra of 1,3-diammonium propyl selenate monohydrate are recorded and the complete vibrational assignments have been discussed. The geometry is optimised by B3LYP method using 6-311G, 6-311+G and 6-311+G* basis sets and the energy, structural parameters, vibrational frequencies, IR and Raman intensities are determined. Differential scanning colorimetry (DSC) data were also presented to analyse the possibility of the phase transition. Complete natural bonding orbital (NBO) analysis is carried out to analyse the intramolecular electronic interactions and their stabilisation energies. The electrostatic potential of the complex lies in the range +1.902e × 10-2 to -1.902e × 10-2. The limits of total electron density of the complex is +8.43e × 10-2 to -8.43e × 10-2.

  18. FT-IR, FT-Raman, and DFT computational studies of melaminium nitrate molecular-ionic crystal

    Science.gov (United States)

    Tanak, Hasan; Marchewka, Mariusz K.

    2013-02-01

    The experimental and theoretical vibrational spectra of melaminium nitrate were studied. The Raman and infrared (FT-IR) spectra of the melaminium nitrate and its deuterated analogue were recorded in the solid phase. Molecular geometry and vibrational frequency values of melaminium nitrate in the electronic ground state were calculated using the density functional method (B3LYP) with the 6-31++G(d,p) basis set. The calculated results show that the optimized geometry can well reproduce the crystal structure, and the theoretical vibrational frequency values show good agreement with experimental values. The NBO analysis reveals that the N-H···O and N-H···N intermolecular interactions significantly influence crystal packing in this molecule.

  19. Helium ion irradiated polyamidoimide films: a FT-IR and Raman follow-up

    International Nuclear Information System (INIS)

    Merhari, L.; Belorgeot, C.; Quintard, P.

    1994-01-01

    The evolution of polyamidoimide (PAI) at a molecular level has been studied by infrared and Raman spectroscopy after several He + ion irradiations. The infrared investigation made it possible to study the appearance of CO 2 and HCN molecules and, for example, to correlate CO 2 with C-O vanishing bands during He + ion irradiation. Preliminary Raman spectroscopy results confirmed a graphite-like structure for strongly irradiated PAI. In situ spectroscopic measurements versus fluence during irradiation with other ions are expected to give further information about the polymer structure evolution. (6 figures, 10 references) (UK)

  20. Energy profile, spectroscopic (FT-IR, FT-Raman and FT-NMR) and DFT studies of 4-bromoisophthalic acid

    Science.gov (United States)

    Arjunan, V.; Thirunarayanan, S.; Mohan, S.

    2018-04-01

    The stable conformer of 4-bromoisophthalic acid (BIPA) has been identified by potential energy profile analysis. All the structural parameters of 4-bromoisophthalic acid are determined by B3LYP method with 6-311++G**, 6-31G** and cc-pVTZ basis sets. The fundamental vibrations are analysed with the use of FT-IR (4000-400 cm-1) and FT-Raman (4000-100 cm-1) spectra. The harmonic vibrational frequencies are theoretically calculated and compared with experimental FTIR and FT-Raman frequencies. The 1H and 13C NMR spectra have been analysed and compared with theoretical 1H and 13C NMR chemical shifts calculated by gauge independent atomic orbital (GIAO) method. The electronic properties, such as HOMO (highest occupied molecular orbital) and LUMO (lowest unoccupied molecular orbital) energies are determined by B3LYP/cc-pVTZ method. The electron density distribution and site of chemical reactivity of BIPA molecule have been obtained by mapping electron density isosurface with molecular electrostatic potential (MEP). Stability of the molecules arising from hyperconjugative interactions, charge delocalizations have been analysed by using natural bond orbital (NBO) analysis. The thermodynamic properties and atomic natural charges of the compound are analysed and the reactive sites of the molecule are identified. The global and local reactivity descriptors are evaluated to analyse the chemical reactivity and site selectivity of molecule through Fukui functions.

  1. Experimental (FT-IR, FT-Raman, 1H, 13C NMR) and theoretical study of alkali metal 2-aminobenzoates

    Science.gov (United States)

    Samsonowicz, M.; Świsłocka, R.; Regulska, E.; Lewandowski, W.

    2008-09-01

    The influence of lithium, sodium, potassium, rubidium and cesium on the electronic system of the 2-aminobenzoic acid was studied by the methods of molecular spectroscopy. The vibrational (FT-IR, FT-Raman) and NMR ( 1H and 13C) spectra for 2-aminobenzoic acid and its alkali metal salts were recorded. The assignment of vibrational spectra was done on the basis of literature data, theoretical calculations and our previous experience. Characteristic shifts of bands and changes in intensities of bands along the metal series were observed. The changes of chemical shifts of protons ( 1H NMR) and carbons ( 13C NMR) in the series of studied alkali metal 2-aminobenzoates were observed too. Optimized geometrical structures of studied compounds were calculated by B3LYP method using 6-311++G ∗∗ basis set. Geometric aromaticity indices, dipole moments and energies were also calculated. The theoretical wavenumbers and intensities of IR and Raman spectra were obtained. The calculated parameters were compared to experimental characteristic of studied compounds.

  2. Evaluation of Salmon Adhesion on PET-Metal Interface by ATR, FT-IR, and Raman Spectroscopy

    Directory of Open Access Journals (Sweden)

    E. Zumelzu

    2015-01-01

    Full Text Available The material employed in this study is an ecoefficient, environmentally friendly, chromium (VI-free (noncarcinogenic metal polymer. The originality of the research lies in the study of the effect of new production procedures of salmon on metal packaging with multilayer polyethylene terephthalate (PET polymer coatings. Our hypothesis states that the adhesion of postmortem salmon muscles to the PET polymer coating produces surface and structural changes that affect the functionality and limit the useful life of metal containers, compromising therefore their recycling capacity as ecomaterials. This work is focused on studying the effects of the biochemical changes of postmortem salmon on the PET coating and how muscle degradation favors adhesion to the container. The experimental design considered a series of laboratory tests of containers simulating the conditions of canned salmon, chemical and physical tests of food-contact canning to evaluate the adhesion, and characterization of changes in the multilayer PET polymer by electron microscopy, ATR, FT-IR, and Raman spectroscopy analyses. The analyses determined the effect of heat treatment of containers on the loss of freshness of canned fish and the increased adhesion to the container wall, and the limited capability of the urea treatment to remove salmon muscle from the container for recycling purposes.

  3. FT-Raman and FT-IR spectroscopy of synthetic Mg/Zn/Al-hydrotalcites

    International Nuclear Information System (INIS)

    Leishman, N.; Kloprogge, J.T.; Fry, R.; Frost, R.L.

    1998-01-01

    Full text: Hydrotalcites, also known as layered double hydroxides, are less well known and more diffuse in nature than cationic clays. They can be visualised as positively charged hydroxide layers comparable to brucite in which a part of the Mg 2+ is substituted by a trivalent metal like Al 3+ or Fe 3+ separated by charge compensating mostly hydrated interlayer anions. In synthetic hydrotalcites a broad range of compositions are possible of the type [M 2+ 1-x M 3+ x (OH) 2 ][A n- ] x/n -yH 2 O, where M 2+ and M 3+ are the di- and trivalent cations in the octahedral positions within the hydroxide layers with x between 0.17 and 0.33. A n- is an exchangeable interlayer anion. The hydrotalcites with Mg/Zn/Al atomic ratios of 6/0/2, 4/2/2, 2/4/2 and 0/6/2 were synthesised by the slow simultaneous addition of a mixed aluminum-magnesium-zinc nitrate solution and a NaOH solution under vigorous stirring buffering the pH at ± 10. The products were washed to eliminate excess salt and dried at 60 deg C. The nature of the resulting material was checked by XRD and TEM. Both proved the materials to exist of only crystalline hydrotalcite except for the Zn 6 Al 2 (OH) 16 CO 3 .nH 2 O, which contained some unidentified products. The infrared and Raman spectra of synthetic hydrotalcites with different Mg/Zn ratios reveal complicated spectra. Based on the differences in the spectra between the various hydrotalcites and comparison to the comparable hydroxides and hydroxycarbonates a much more detailed band assignment can be made than has been published before

  4. Effects of Low Carbohydrate High Protein (LCHP) diet on atherosclerotic plaque phenotype in ApoE/LDLR-/- mice: FT-IR and Raman imaging.

    Science.gov (United States)

    Wrobel, T P; Marzec, K M; Chlopicki, S; Maślak, E; Jasztal, A; Franczyk-Żarów, M; Czyżyńska-Cichoń, I; Moszkowski, T; Kostogrys, R B; Baranska, M

    2015-09-22

    Low Carbohydrate High Protein (LCHP) diet displays pro-atherogenic effects, however, the exact mechanisms involved are still unclear. Here, with the use of vibrational imaging, such as Fourier transform infrared (FT-IR) and Raman (RS) spectroscopies, we characterize biochemical content of plaques in Brachiocephalic Arteries (BCA) from ApoE/LDLR(-/-) mice fed LCHP diet as compared to control, recomended by American Institute of Nutrition, AIN diet. FT-IR images were taken from 6-10 sections of BCA from each mice and were complemented with RS measurements with higher spatial resolution of chosen areas of plaque sections. In aortic plaques from LCHP fed ApoE/LDLR(-/-) mice, the content of cholesterol and cholesterol esters was increased, while that of proteins was decreased as evidenced by global FT-IR analysis. High resolution imaging by RS identified necrotic core/foam cells, lipids (including cholesterol crystals), calcium mineralization and fibrous cap. The decreased relative thickness of the outer fibrous cap and the presence of buried caps were prominent features of the plaques in ApoE/LDLR(-/-) mice fed LCHP diet. In conclusion, FT-IR and Raman-based imaging provided a complementary insight into the biochemical composition of the plaque suggesting that LCHP diet increased plaque cholesterol and cholesterol esters contents of atherosclerotic plaque, supporting the cholesterol-driven pathogenesis of LCHP-induced atherogenesis.

  5. Raman and Fourier Transform Infrared (FT-IR) Mineral to Matrix Ratios Correlate with Physical Chemical Properties of Model Compounds and Native Bone Tissue.

    Science.gov (United States)

    Taylor, Erik A; Lloyd, Ashley A; Salazar-Lara, Carolina; Donnelly, Eve

    2017-10-01

    Raman and Fourier transform infrared (FT-IR) spectroscopic imaging techniques can be used to characterize bone composition. In this study, our objective was to validate the Raman mineral:matrix ratios (ν 1 PO 4 :amide III, ν 1 PO 4 :amide I, ν 1 PO 4 :Proline + hydroxyproline, ν 1 PO 4 :Phenylalanine, ν 1 PO 4 :δ CH 2 peak area ratios) by correlating them to ash fraction and the IR mineral:matrix ratio (ν 3 PO 4 :amide I peak area ratio) in chemical standards and native bone tissue. Chemical standards consisting of varying ratios of synthetic hydroxyapatite (HA) and collagen, as well as bone tissue from humans, sheep, and mice, were characterized with confocal Raman spectroscopy and FT-IR spectroscopy and gravimetric analysis. Raman and IR mineral:matrix ratio values from chemical standards increased reciprocally with ash fraction (Raman ν 1 PO 4 /Amide III: P Raman ν 1 PO 4 /Amide I: P Raman ν 1 PO 4 /Proline + Hydroxyproline: P Raman ν 1 PO 4 /Phenylalanine: P Raman ν 1 PO 4 /δ CH 2 : P Raman and IR mineral:matrix ratio values were strongly correlated ( P Raman mineral:matrix bone composition parameter correlates strongly to ash fraction and to its IR counterpart. Finally, the mineral:matrix ratio values of the native bone tissue are similar to those of both chemical standards and theoretical values, confirming the biological relevance of the chemical standards and the characterization techniques.

  6. A Raman scattering and FT-IR spectroscopic study on the effect of the solar radiation in Antarctica on bovine cornea

    Science.gov (United States)

    Yamamoto, Tatsuyuki; Murakami, Naoki; Yoshikiyo, Keisuke; Takahashi, Tetsuya; Yamamoto, Naoyuki

    2010-01-01

    The Raman scattering and FT-IR spectra of the corneas, transported to the Syowa station in Antarctica and exposed to the solar radiation of the mid-summer for four weeks, were studied to reveal that type IV collagen involved in corneas were fragmented. The amide I and III Raman bands were observed at 1660 and 1245 cm -1, respectively, and the amide I and II infrared bands were observed at 1655 and 1545 cm -1, respectively, for original corneas before exposure. The background of Raman signals prominently increased and the ratio of amide II infrared band versus amide I decreased by the solar radiation in Antarctica. The control experiment using an artificial UV lamp was also performed in laboratory. The decline rate of the amide II/amide I was utilized for estimating the degree of fragmentation of collagen, to reveal that the addition of vitamin C suppressed the reaction while the addition of sugars promoted it. The effect of the solar radiation in Antarctica on the corneas was estimated as the same as the artificial UV lamp of four weeks (Raman) or one week (FT-IR) exposure.

  7. Effect of microwave treatment on structure of binders based on sodium carboxymethyl starch: FT-IR, FT-Raman and XRD investigations

    Science.gov (United States)

    Kaczmarska, Karolina; Grabowska, Beata; Spychaj, Tadeusz; Zdanowicz, Magdalena; Sitarz, Maciej; Bobrowski, Artur; Cukrowicz, Sylwia

    2018-06-01

    The paper deals with the influence of the microwave treatment on sodium carboxymethyl starch (CMS-Na) applied as a binder for moulding sands. The Fourier transformation infrared spectrometry (FT-IR), Raman spectroscopy (FT-Raman) and XRD analysis data of native potato starch and three different carboxymethyl starches (CMS-Na) with various degree of substitution (DS) before and after exposition to microwave radiation have been compared. FT-IR studies showed that polar groups present in CMS-Na structure take part in the formation of new hydrogen bonds network after water evaporation. However, these changes depend on DS value of the modified starch. The FT-Raman study confirmed that due to the impact on the samples by microwave, the changes of intensity in the characteristic bands associated with the crystalline regions in the sample were noticed. The X-ray diffraction data for microwave treated CMS-Na samples have been compared with the diffractograms of initial materials and analysis of XRD patterns confirmed that microwave-treated samples exhibit completely amorphous structure. Analysis of structural changes allows to state that the binding of sand grains in moulding sand with CMS-Na polymeric binder consists in the formation of hydrogen bonds networks (physical cross-linking).

  8. Effect of microwave treatment on structure of binders based on sodium carboxymethyl starch: FT-IR, FT-Raman and XRD investigations.

    Science.gov (United States)

    Kaczmarska, Karolina; Grabowska, Beata; Spychaj, Tadeusz; Zdanowicz, Magdalena; Sitarz, Maciej; Bobrowski, Artur; Cukrowicz, Sylwia

    2018-06-15

    The paper deals with the influence of the microwave treatment on sodium carboxymethyl starch (CMS-Na) applied as a binder for moulding sands. The Fourier transformation infrared spectrometry (FT-IR), Raman spectroscopy (FT-Raman) and XRD analysis data of native potato starch and three different carboxymethyl starches (CMS-Na) with various degree of substitution (DS) before and after exposition to microwave radiation have been compared. FT-IR studies showed that polar groups present in CMS-Na structure take part in the formation of new hydrogen bonds network after water evaporation. However, these changes depend on DS value of the modified starch. The FT-Raman study confirmed that due to the impact on the samples by microwave, the changes of intensity in the characteristic bands associated with the crystalline regions in the sample were noticed. The X-ray diffraction data for microwave treated CMS-Na samples have been compared with the diffractograms of initial materials and analysis of XRD patterns confirmed that microwave-treated samples exhibit completely amorphous structure. Analysis of structural changes allows to state that the binding of sand grains in moulding sand with CMS-Na polymeric binder consists in the formation of hydrogen bonds networks (physical cross-linking). Copyright © 2018 Elsevier B.V. All rights reserved.

  9. The use of UV, FT-IR and Raman spectra for the identification of the newest penem analogs: solutions based on mathematic procedure and the density functional theory.

    Science.gov (United States)

    Cielecka-Piontek, J; Lewandowska, K; Barszcz, B; Paczkowska, M

    2013-02-15

    The application of ultraviolet, FT-IR and Raman spectra was proposed for identification studies of the newest penem analogs (doripenem, biapenem and faropenem). An identification of the newest penem analogs based on their separation from related substances was achieved after the application of first derivative of direct spectra in ultraviolet which permitted elimination of overlapping effects. A combination of experimental and theoretical studies was performed for analyzing the structure and vibrational spectra (FT-IR and Raman spectra) of doripenem, biapenem and faropenem. The calculations were conducted using the density functional theory with the B3LYP hybrid functional and 6-31G(d,p) basis set. The confirmation of the applicability of the DFT methodology for interpretation of vibrational IR and Raman spectra of the newest penem analogs contributed to determination of changes of vibrations in the area of the most labile bonds. By employing the theoretical approach it was possible to eliminate necessity of using reference standards which - considering the instability of penem analogs - require that correction coefficients are factored in. Copyright © 2012 Elsevier B.V. All rights reserved.

  10. Vibrational spectra (FT-IR, FT-Raman), frontier molecular orbital, first hyperpolarizability, NBO analysis and thermodynamics properties of Piroxicam by HF and DFT methods

    Science.gov (United States)

    Suresh, S.; Gunasekaran, S.; Srinivasan, S.

    2015-03-01

    The solid phase FT-IR and FT-Raman spectra of 4-Hydroxy-2-methyl-N-(2-pyridinyl)-2H-1,2-benzothiazine-3-carboxamide-1,1-dioxide (Piroxicam) have been recorded in the region 4000-400 and 4000-100 cm-1 respectively. The molecular geometry, harmonic vibrational frequencies and bonding features of piroxicam in the ground state have been calculated by Hartree-Fock (HF) and density functional theory (DFT) methods using 6-311++G(d,p) basis set. The calculated harmonic vibrational frequencies are scaled and they are compared with experimental obtained by FT-IR and FT-Raman spectra. A detailed interpretation of the vibrational spectra of the title compound has been made on the basis of the calculated potential energy distribution (PED). The electronic properties, such as HOMO and LUMO energies, molecular electrostatic potential (MESP) are also performed. The linear polarizability (α) and the first order hyper polarizability (β) values of the title compound have been computed. The molecular stability arising from hyper conjugative interaction, charge delocalization has been analyzed using natural bond orbital (NBO) analysis.

  11. Synthesis and characterization of the polystyrene - asphaltene graft copolymer BY FT-IR spectroscopy

    International Nuclear Information System (INIS)

    Leo, Adan Yovani; Salazar Ramiro

    2008-01-01

    The creation of new polymer compounds to be added to asphalt has drawn considerable attention because these substances have succeeded in modifying the asphalt rheological characteristics and physical properties for the enhancement of its behavior during the time of use. This work explains the synthesis of a new graft copolymer based on an asphalt fraction called asphaltene, modified with maleic anhydride. Polystyrene functionalization is conducted in a parallel fashion in order to obtain polybenzylamine resin with an amine - NH2 free group that reacts with the anhydride graft groups in the asphaltene, thus obtaining the new Polystyrene/Asphaltene graft copolymer

  12. FT-IR, FT-Raman, UV spectra and DFT calculations on monomeric and dimeric structure of 2-amino-5-bromobenzoic acid.

    Science.gov (United States)

    Karabacak, Mehmet; Cinar, Mehmet

    2012-02-01

    In this work, the molecular conformation, vibrational and electronic transition analysis of 2-amino-5-bromobenzoic acid (2A5BrBA) were presented for the ground state using experimental techniques (FT-IR, FT-Raman and UV) and density functional theory (DFT) employing B3LYP exchange correlation with the 6-311++G(d,p) basis set. FT-IR and FT-Raman spectra were recorded in the regions of 400-4000 cm(-1) and 50-4000 cm(-1), respectively. There are four conformers, C1, C2, C3 and C4 for this molecule. The geometrical parameters, energies and wavenumbers have been obtained for all four conformers. The computational results diagnose the most stable conformer of 2A5BrBA as the C1 form. The complete assignments of fundamental vibrations were performed on the basis of the total energy distribution (TED) of the vibrational modes, calculated with scaled quantum mechanics (SQM) method. Raman activities calculated by DFT method have been converted to the corresponding Raman intensities using Raman scattering theory. The UV spectra of investigated compound were recorded in the region of 200-400 nm for ethanol and water solutions. The electronic properties were evaluated with help of time-dependent DFT (TD-DFT) theoretically and results were compared with experimental observations. The thermodynamic properties of the studied compound at different temperatures were calculated, revealing the correlations between standard heat capacity, standard entropy, standard enthalpy changes and temperatures. The observed and the calculated geometric parameters, vibrational wavenumbers and electronic transitions were compared with observed data and found to be in good agreement. Copyright © 2011 Elsevier B.V. All rights reserved.

  13. Synthesis of 2,4-disubstituted thiazole combinatorial unit on solid-phase: microwave assisted conversion of alcohol to amine monitored by FT-IR

    International Nuclear Information System (INIS)

    Antonow, Dyeison; Eifler-Lima, Vera Lucia; Mahler, S. Graciela; Serra, Gloria L.; Manta, Eduardo

    2005-01-01

    Microwave-assisted solid-phase synthesis of the 2,4-disubstituted thiazole 3 on Merrifield Resin is described. The hydroxyl moiety was converted to amine in five steps - including coupling and cleavage - within a total reaction time of 2 hours and 26% overall yield. The entire solid-phase synthesis was efficiently monitored by FT-IR/KBr pellets and allows potential use in combinatorial chemistry. (author)

  14. Evaluation of a setting reaction pathway in the novel composite TiHA-CSD bone cement by FT-Raman and FT-IR spectroscopy

    Science.gov (United States)

    Paluszkiewicz, Czesława; Czechowska, Joanna; Ślósarczyk, Anna; Paszkiewicz, Zofia

    2013-02-01

    The aim of this study was to determine a setting reaction pathway in a novel, surgically handy implant material, based on calcium sulfate hemihydrate (CSH) and titanium doped hydroxyapatite (TiHA). The previous studies confirmed superior biological properties of TiHA in comparison to the undoped hydroxyapatite (HA) what makes it highly attractive for future medical applications. In this study the three types of titanium modified HA powders: untreated, calcined at 800 °C, sintered at 1250 °C and CSH were used to produce bone cements. The Fourier Transform-InfraRed (FT-IR) spectroscopy and Raman spectroscopy were applied to evaluate processes taking place during the setting of the studied materials. Our results undoubtedly confirmed that the reaction pathways and the phase compositions differed significantly for set cements and were dependent on the initial heat treatment of TiHA powder. Final materials were multiphase composites consisting of calcium sulfate dihydrate, bassanite, tricalcium phosphate, hydroxyapatite and calcium titanate (perovskite). The FT-IR and Scanning Electron Microscopy (SEM) measurements performed after the incubation of the cement samples in the simulated body fluid (SBF), indicate on high bioactive potential of the obtained bone cements.

  15. The spectroscopic (FT-IR, FT-Raman, dispersive Raman and NMR) study of ethyl-6-chloronicotinate molecule by combined density functional theory.

    Science.gov (United States)

    Karabacak, Mehmet; Calisir, Zuhre; Kurt, Mustafa; Kose, Etem; Atac, Ahmet

    2016-01-15

    In this study, ethyl-6-chloronicotinate (E-6-ClN) molecule is recorded in the region 4000-400 cm(-1) and 3500-100 cm(-1) (FT-IR, FT-Raman and dispersive Raman, respectively) in the solid phase. ((1))H and ((13))C nuclear magnetic resonance (NMR) spectra are recorded in DMSO solution. The structural and spectroscopic data of the molecule are obtained for two possible isomers (S1 and S2) from DFT (B3LYP) with 6-311++G(d,p) basis set calculations. The geometry of the molecule is fully optimized, vibrational spectra are calculated and fundamental vibrations are assigned on the basis of the potential energy distribution (PED) of the vibrational modes. ((1))H and ((13))C NMR chemical shifts are calculated by using the gauge-invariant atomic orbital (GIAO) method. The electronic properties, such as excitation energies, oscillator strengths, wavelengths, HOMO and LUMO energies, are performed by time-dependent density functional theory (TD-DFT). Total and partial density of state and overlap population density of state diagrams analysis are presented for E-6-ClN molecule. Furthermore, frontier molecular orbitals (FMO), molecular electrostatic potential, and thermodynamic features are performed. In addition to these, reduced density gradient of the molecule is performed and discussed. As a conclusion, the calculated results are compared with the experimental spectra of the title compound. The results of the calculations are applied to simulate the vibrational spectra of the molecule, which show excellent agreement with the observed ones. The theoretical and tentative results will give us a detailed description of the structural and physicochemical properties of the molecule. Natural bond orbital analysis is done to have more information stability of the molecule arising from charge delocalization, and to reveal the information regarding charge transfer within the molecules. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Characterization of Meldrum's acid derivative 5-(5-Ethyl-1,3,4-thiadiazol-2-ylamino)methylene-2,2-dimethyl-1,3-dioxane-4,6-dione by Raman and FT-IR spectroscopy and DFT calculations

    Science.gov (United States)

    de Toledo, T. A.; da Silva, L. E.; Teixeira, A. M. R.; Freire, P. T. C.; Pizani, P. S.

    2015-07-01

    In this study, the structural and vibrational properties of Meldrum's acid derivative 5-(5-Ethyl-1,3,4-thiadiazol-2-ylamino)methylene-2,2-dimethyl-1,3-dioxane-4,6-dione, C11H13N3O4S were studied combining experimental techniques such as Raman and FT-IR spectroscopy and density functional theory (DFT) calculations. The Raman and FT-IR spectra were recorded at room conditions in the regions from 80 to 3400 cm-1 and 400 to 4000 cm-1, respectively. Vibrational wavenumbers were predicted using DFT calculations with the hybrid functional B3LYP and basis set 6-31G(d,p). A comparison between experimental and theoretical data is provided for the Raman and FT-IR spectra. The descriptions of the normal modes were carried by means of potential energy distribution (PED).

  17. Spectroscopic investigation (FT-IR, FT-Raman), HOMO-LUMO, NBO, and molecular docking analysis of N-ethyl-N-nitrosourea, a potential anticancer agent

    Science.gov (United States)

    Singh, Priyanka; Islam, S. S.; Ahmad, Hilal; Prabaharan, A.

    2018-02-01

    Nitrosourea plays an important role in the treatment of cancer. N-ethyl-N-nitrosourea, also known as ENU, (chemical formula C3H7N3O2), is a highly potent mutagen. The chemical is an alkylating agent and acts by transferring the ethyl group of ENU to nucleobases (usually thymine) in nucleic acids. The molecular structure of N-ethyl-N-nitrosourea has been elucidated using experimental (FT-IR and FT-Raman) and theoretical (DFT) techniques. APT charges, Mulliken atomic charges, Natural bond orbital, Electrostatic potential, HOMO-LUMO and AIM analysis were performed to identify the reactive sites and charge transfer interactions. Furthermore, to evaluate the anticancer activity of ENU molecular docking studies were carried out against 2JIU protein.

  18. Investigation of the Cross-Section Stratifications of Icons Using Micro-Raman and Micro-Fourier Transform Infrared (FT-IR) Spectroscopy.

    Science.gov (United States)

    Lazidou, Dimitra; Lampakis, Dimitrios; Karapanagiotis, Ioannis; Panayiotou, Costas

    2018-01-01

    The cross-section stratifications of samples, which were removed from six icons, are studied using optical microscopy, micro-Raman spectroscopy, and micro-Fourier transform infrared (FT-IR) spectroscopy. The icons, dated from the 14th to 19th centuries, are prominent examples of Byzantine painting art and are attributed to different artistic workshops of ​​northern Greece. The following materials are identified in the cross-sections of the icon samples using micro-Raman spectroscopy: anhydrite; calcite; carbon black; chrome yellow; cinnabar; gypsum; lead white; minium; orpiment; Prussian blue; red ochre; yellow ochre; and a paint of organic origin which can be either indigo ( Indigofera tinctoria L. and others) or woad ( Isatis tinctoria L.). The same samples are investigated using micro-FT-IR which leads to the following identifications: calcite; calcium oxalates; chrome yellow; gypsum; kaolinite; lead carboxylates; lead sulfate (or quartz); lead white; oil; protein; Prussian blue; saponified oil; shellac; silica; and tree resin. The study of the cross-sections of the icon samples reveals the combinations of the aforementioned inorganic and organic materials. Although the icons span over a long period of six centuries, the same stratification comprising gypsum ground layer, paint layers prepared by modified "egg tempera" techniques (proteinaceous materials mixed with oil and resins), and varnish layer is revealed in the investigated samples. Moreover, the presence of three layers of varnishes, one at the top and other two as intermediate layers, in the cross-section analysis of a sample from Virgin and Child provide evidence of later interventions.

  19. FT-Raman, FT-IR spectra and total energy distribution of 3-pentyl-2,6-diphenylpiperidin-4-one: DFT method.

    Science.gov (United States)

    Subashchandrabose, S; Saleem, H; Erdogdu, Y; Rajarajan, G; Thanikachalam, V

    2011-11-01

    FT-Raman and FT-IR spectra were recorded for 3-pentyl-2,6-diphenylpiperidin-4-one (PDPO) sample in solid state. The equilibrium geometries, harmonic vibrational frequencies, infrared and the Raman scattering intensities were computed using DFT/6-31G(d,p) level. Results obtained at this level of theory were used for a detailed interpretation of the infrared and Raman spectra, based on the total energy distribution (TED) of the normal modes. Molecular parameters such as bond lengths, bond angles and dihedral angles were calculated and compared with X-ray diffraction data. This comparison was good agreement. The intra-molecular charge transfer was calculated by means of natural bond orbital analysis (NBO). Hyperconjugative interaction energy was more during the π-π* transition. Energy gap of the molecule was found using HOMO and LUMO calculation, hence the less band gap, which seems to be more stable. Atomic charges of the carbon, nitrogen and oxygen were calculated using same level of calculation. Copyright © 2011 Elsevier B.V. All rights reserved.

  20. Quantum mechanical, spectroscopic studies (FT-IR, FT-Raman, NMR, UV) and normal coordinates analysis on 3-([2-(diaminomethyleneamino) thiazol-4-yl] methylthio)-N'-sulfamoylpropanimidamide

    Science.gov (United States)

    Muthu, S.; Uma Maheswari, J.; Sundius, Tom

    2013-05-01

    Famotidine (3-([2-(diaminomethyleneamino) thiazol-4-yl] methylthio)-N'-sulfamoylpropanimidamide) is a histamine H2-receptor antagonist that inhibits stomach acid production, and it is commonly used in the treatment of peptic ulcer disease (PUD) and gastroesophageal reflux disease (GERD/GORD). Quantum chemical calculations of the equilibrium geometry of famotidine in the ground state were carried out using density functional theory (DFT/B3LYP) with the 6-311G(d,p) basis set. In addition, harmonic vibrational frequencies, infrared intensities and Raman activities were calculated at the same level of theory. A detailed interpretation of the infrared and Raman spectrum of the drug is also reported. Theoretical simulations of the FT-IR, and FT-Raman spectra of the title compound have been calculated. Good correlations between the experimental 1H and 13C NMR chemical shifts and calculated GIAO shielding tensors were found. The results of the energy and oscillator strength calculations by time-dependent density functional theory (TD-DFT) supplement the experimental findings. Total and partial density of state (TDOS and PDOS) and also overlap population density of state (COOP or OPDOS) diagrams analysis were presented. The dipole moment, linear polarizability and first order hyperpolarizability values were also computed. The linear polarizability and first order hyperpolarizabilities of the studied molecule indicate that the compound is a good candidate for nonlinear optical materials.

  1. The spectroscopic (FT-IR, FT-Raman, UV and NMR) first order hyperpolarizability and HOMO-LUMO analysis of dansyl chloride

    Science.gov (United States)

    Karabacak, M.; Cinar, M.; Kurt, M.; Poiyamozhi, A.; Sundaraganesan, N.

    2014-01-01

    The solid phase FT-IR and FT-Raman spectra of dansyl chloride (DC) have been recorded in the regions 400-4000 and 50-4000 cm-1, respectively. The spectra have been interpreted in terms of fundamentals modes, combination and overtone bands. The structure of the molecule has been optimized and the structural characteristics have been determined by density functional theory (B3LYP) method with 6-311++G(d,p) as basis set. The vibrational frequencies were calculated for most stable conformer and were compared with the experimental frequencies, which yield good agreement between observed and calculated frequencies. The infrared and Raman spectra have also been predicted from the calculated intensities. 1H and 13C NMR spectra were recorded and 1H and 13C nuclear magnetic resonance chemical shifts of the molecule were calculated using the gauge independent atomic orbital (GIAO) method. UV-Visible spectrum of the compound was recorded in the region 200-600 nm and the electronic properties HOMO and LUMO energies were measured by time-dependent TD-DFT approach. Nonlinear optical and thermodynamic properties were interpreted. All the calculated results were compared with the available experimental data of the title molecule.

  2. FT-IR, FT-Raman, NMR studies and ab initio-HF, DFT-B3LYP vibrational analysis of 4-chloro-2-fluoroaniline.

    Science.gov (United States)

    Arivazhagan, M; Anitha Rexalin, D

    2012-10-01

    The Fourier transform infrared (FT-IR) and Fourier transform Raman (FT-Raman) spectra of 4-chloro-2-fluoroaniline (CFA) have been recorded and analyzed. The equilibrium geometry, bonding features and harmonic vibrational frequencies have been investigated with the help of ab initio and density functional theory (DFT) methods. The assignments of the vibrational spectra have been carried out with the help of normal coordinate analysis (NCA) following the scaled quantum mechanical force field methodology. The (1)H and (13)C nuclear magnetic resonance (NMR) chemical shifts of the molecule are calculated by the Gauge including atomic orbital (GIAO) method. The first order hyperpolarizability (β(0)) of this novel molecular system and related properties (β, α(0) and Δα) of CFA are calculated using B3LYP/6-311++G(d,p) and HF/6-311++G(d,p) methods on the finite-field approach. The calculated results also show that the CFA molecule might have microscopic nonlinear optical (NLO) behavior with non-zero values. Stability of the molecule arising from hyper conjugative interactions, charge delocalization has been analyzed using natural bond orbital (NBO) analysis. The result confirms the occurrence of intramolecular charge transfer (ICT) within the molecule. The HOMO-LUMO energies UV-vis spectral analysis and MEP are performed by B3LYP/6-311++G(d,p) approach. A detailed interpretation of the infrared and Raman spectra of CFA is also reported based on total energy distribution (TED). The difference between the observed and scaled wave number values of the most of the fundamentals is very small. Copyright © 2012 Elsevier B.V. All rights reserved.

  3. Curcumin-β-cyclodextrin inclusion complex: stability, solubility, characterisation by FT-IR, FT-Raman, X-ray diffraction and photoacoustic spectroscopy, and food application.

    Science.gov (United States)

    Mangolim, Camila Sampaio; Moriwaki, Cristiane; Nogueira, Ana Claudia; Sato, Francielle; Baesso, Mauro Luciano; Neto, Antônio Medina; Matioli, Graciette

    2014-06-15

    Curcumin was complexed with β-CD using co-precipitation, freeze-drying and solvent evaporation methods. Co-precipitation enabled complex formation, as indicated by the FT-IR and FT-Raman techniques via the shifts in the peaks that were assigned to the aromatic rings of curcumin. In addition, photoacoustic spectroscopy and X-ray diffraction, with the disappearance of the band related to aromatic rings, by Gaussian fitting, and modifications in the spectral lines, respectively, also suggested complex formation. The possible complexation had an efficiency of 74% and increased the solubility of the pure colourant 31-fold. Curcumin-β-CD complex exhibited a sunlight stability 18% higher than the pure colourant. This material was stable to pH variations and storage at -15 and 4°C. With an isothermal heating at 100 and 150°C for 2h, the material exhibited a colour retention of approximately 99%. The application of curcumin-β-CD complex in vanilla ice creams intensified the colour of the products and produced a great sensorial acceptance. Copyright © 2013 Elsevier Ltd. All rights reserved.

  4. Acid-base properties, FT-IR, FT-Raman spectroscopy and computational study of 1-(pyrid-4-yl)piperazine.

    Science.gov (United States)

    Mary, Y Sheena; Panicker, C Yohannan; Varghese, Hema Tresa; Van Alsenoy, Christian; Procházková, Markéta; Sevčík, Richard; Pazdera, Pavel

    2014-01-01

    We report the vibrational spectral analysis was carried out using FT-IR and FT-Raman spectroscopy for 1-(pyrid-4-yl)piperazine (PyPi). Single crystals of PyPi suitable for X-ray structural analysis were obtained. The acid-base properties are also reported. PyPi supported on a weak acid cation-exchanger in the single protonated form and this system can be used efficiently as the solid supported analogue of 4-N,N-dimethyl-aminopyridine. The complete vibrational assignments of wavenumbers were made on the basis of potential energy distribution. The HOMO and LUMO analysis is used to determine the charge transfer within the molecule and with the molecular electrostatic potential map was applied for the reactivity assessment of PyPi molecule toward proton, electrophiles and nucleopholes as well. The stability of the molecule arising from hyper-conjugative interaction and charge delocalization has been analyzed using NBO analysis. The calculated first hyperpolarizability of PyPi is 17.46 times that of urea. Copyright © 2013 Elsevier B.V. All rights reserved.

  5. Ab initio and DFT study of hydrogen bond interactions between ascorbic acid and dimethylsulfoxide based on FT-IR and FT-Raman spectra

    Science.gov (United States)

    Niazazari, Naser; Zatikyan, Ashkhen L.; Markarian, Shiraz A.

    2013-06-01

    The hydrogen bonding of 1:1 complexes formed between L-ascorbic acid (LAA) and dimethylsulfoxide (DMSO) has been studied by means of ab initio and density functional theory (DFT) calculations. Solutions of L-ascorbic acid (AA) in dimethylsulfoxide (DMSO) have been studied by means of both FT-IR (4000-220 cm-1) and FT-Raman spectroscopy. Ab initio Hartree-Fock (HF) and DFT methods have been used to determine the structure and energies of stable conformers of various types of L-AA/DMSO complexes in gas phase and solution. The basis sets 6-31++G∗∗ and 6-311+G∗ were used to describe the structure, energy, charges and vibrational frequencies of interacting complexes in the gas phase. The optimized geometric parameters and interaction energies for various complexes at different theories have been estimated. Binding energies have been corrected for basis set superposition error (BSSE) and harmonic vibrational frequencies of the structures have been calculated to obtain the stable forms of the complexes. The self-consistent reaction field (SCRF) has been used to calculate the effect of DMSO as the solvent on the geometry, energy and charges of complexes. The solvent effect has been studied using the Onsager models. It is shown that the polarity of the solvent plays an important role on the structures and relative stabilities of different complexes. The results obtained show that there is a satisfactory correlation between experimental and theoretical predictions.

  6. Molecular vibrational investigation [FT-IR, FT-Raman, UV-Visible and NMR] on Bis(thiourea) Nickel chloride using HF and DFT calculations

    Science.gov (United States)

    Anand, S.; Sundararajan, R. S.; Ramachandraraja, C.; Ramalingam, S.; Durga, R.

    2015-03-01

    In the present research work, the FT-IR, FT-Raman spectra of the Bis(thiourea) Nickel chloride (BTNC) were recorded and analyzed. The observed fundamental frequencies in finger print and functional group regions were assigned according to their uniqueness region. The computational calculations were carried out by HF and DFT (B3LYP and B3PW91) methods with 6-31++G(d,p) and 6-311++G(d,p) basis sets and the corresponding results were tabulated. The present organo-metallic compound was made up of covalent and coordination covalent bonds. The modified vibrational pattern of the complex molecule associated with ligand group was analyzed. Furthermore, the 13C NMR and 1H NMR spectral data were calculated by using the gauge independent atomic orbital (GIAO) method with B3LYP/6-311++G(d,p) basis set and their spectra were simulated and the chemical shifts linked to TMS were compared. A investigation on the electronic and optical properties; absorption wavelengths, excitation energy, dipole moment and frontier molecular orbital energies were carried out. The kubo gap of the present compound was calculated related to HOMO and LUMO energies which confirm the occurring of charge transformation between the base and ligand. Besides frontier molecular orbitals (FMO), molecular electrostatic potential (MEP) was performed. The NLO properties related to Polarizability and hyperpolarizability based on the finite-field approach were also discussed.

  7. Spectroscopic [FT-IR and FT-Raman] and theoretical [UV-Visible and NMR] analysis on α-Methylstyrene by DFT calculations

    Science.gov (United States)

    Karthikeyan, N.; Joseph Prince, J.; Ramalingam, S.; Periandy, S.

    2015-05-01

    In the present research work, the FT-IR, FT-Raman and 13C and 1H NMR spectra of the α-Methylstyrene were recorded. The observed fundamental frequencies in finger print as well as functional group regions were assigned according to their uniqueness region. The Gaussian computational calculations are carried out by HF and DFT (B3LYP and B3PW91) methods with 6-31++G(d,p) and 6-311++G(d,p) basis sets and the corresponding results were tabulated. The impact of the presence of vinyl group in phenyl structure of the compound is investigated. The modified vibrational pattern of the molecule associated vinyl group was analyzed. Moreover, 13C NMR and 1H NMR were calculated by using the gauge independent atomic orbital (GIAO) method with B3LYP methods and the 6-311++G(d,p) basis set and their spectra were simulated and the chemical shifts linked to TMS were compared. A study on the electronic and optical properties; absorption wavelengths, excitation energy, dipole moment and frontier molecular orbital energies were carried out. The kubo gap of the present compound was calculated related to HOMO and LUMO energies which confirm the occurring of charge transformation between the base and ligand. Besides frontier molecular orbitals (FMO), molecular electrostatic potential (MEP) was performed. The NLO properties related to Polarizability and hyperpolarizability based on the finite-field approach were also discussed.

  8. Experimental and theoretical studies of (FT-IR, FT-Raman, UV-Visible and DFT) 4-(6-methoxynaphthalen-2-yl) butan-2-one.

    Science.gov (United States)

    Govindasamy, P; Gunasekaran, S

    2015-01-01

    In this work, the vibrational spectral analysis was carried out by using FT-Raman and FT-IR spectroscopy in the range 4000-50 cm(-1) and 4000-450 cm(-1) respectively for 4-(6-methoxynaphthalen-2-yl) butan-2-one (abbreviated as 4MNBO) molecule. Theoretical calculations were performed by density functional theory (DFT/B3LYP) method using 6-311G(d,p) and 6-311++G(d,p) basis sets. The difference between the observed and calculated wavenumber value of most of the fundamentals were very small. The complete vibrational assignments of wavenumbers were made on the basis of potential energy distribution (PED). The UV-Vis spectrum was recorded in the methanol solution. The energy, wavelength and oscillator's strength were calculated by Time Dependent Density Functional Theory (TD-DFT) and matched to the experimental findings. The intramolecular contacts have been interpreted using natural bond orbital (NBO) and natural localized molecular orbital (NLMO) analysis. Thermodynamic properties of 4MNBO at different temperature have been calculated. The molecular electrostatic potential surface (MESP) and Frontier molecular orbital's (FMO's) analysis were investigated using theoretical calculations. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Molecular vibrational investigation [FT-IR, FT-Raman, UV-Visible and NMR] on Bis(thiourea) Nickel chloride using HF and DFT calculations.

    Science.gov (United States)

    Anand, S; Sundararajan, R S; Ramachandraraja, C; Ramalingam, S; Durga, R

    2015-03-05

    In the present research work, the FT-IR, FT-Raman spectra of the Bis(thiourea) Nickel chloride (BTNC) were recorded and analyzed. The observed fundamental frequencies in finger print and functional group regions were assigned according to their uniqueness region. The computational calculations were carried out by HF and DFT (B3LYP and B3PW91) methods with 6-31++G(d,p) and 6-311++G(d,p) basis sets and the corresponding results were tabulated. The present organo-metallic compound was made up of covalent and coordination covalent bonds. The modified vibrational pattern of the complex molecule associated with ligand group was analyzed. Furthermore, the (13)C NMR and (1)H NMR spectral data were calculated by using the gauge independent atomic orbital (GIAO) method with B3LYP/6-311++G(d,p) basis set and their spectra were simulated and the chemical shifts linked to TMS were compared. A investigation on the electronic and optical properties; absorption wavelengths, excitation energy, dipole moment and frontier molecular orbital energies were carried out. The kubo gap of the present compound was calculated related to HOMO and LUMO energies which confirm the occurring of charge transformation between the base and ligand. Besides frontier molecular orbitals (FMO), molecular electrostatic potential (MEP) was performed. The NLO properties related to Polarizability and hyperpolarizability based on the finite-field approach were also discussed. Crown Copyright © 2014. Published by Elsevier B.V. All rights reserved.

  10. Preparation and characterizations of SnO2 nanopowder and spectroscopic (FT-IR, FT-Raman, UV-Visible and NMR) analysis using HF and DFT calculations.

    Science.gov (United States)

    Ayeshamariam, A; Ramalingam, S; Bououdina, M; Jayachandran, M

    2014-01-24

    In this work, pure and singe phase SnO2 Nano powder is successfully prepared by simple sol-gel combustion route. The photo luminescence and XRD measurements are made and compared the geometrical parameters with calculated values. The FT-IR and FT-Raman spectra are recorded and the fundamental frequencies are assigned. The optimized parameters and the frequencies are calculated using HF and DFT (LSDA, B3LYP and B3PW91) theory in bulk phase of SnO2 and are compared with its Nano phase. The vibrational frequency pattern in nano phase gets realigned and the frequencies are shifted up to higher region of spectra when compared with bulk phase. The NMR and UV-Visible spectra are simulated and analyzed. Transmittance studies showed that the HOMO-LUMO band gap (Kubo gap) is reduced from 3.47 eV to 3.04 eV while it is heated up to 800°C. The Photoluminescence spectra of SnO2 powder showed a peak shift towards lower energy side with the change of Kubo gap from 3.73 eV to 3.229 eV for as-prepared and heated up to 800°C. Crown Copyright © 2013. Published by Elsevier B.V. All rights reserved.

  11. Analysis of 19th century ceramic fragments excavated from Pirenópolis (Goiás, Brazil) using FT-IR, Raman, XRF and SEM

    Science.gov (United States)

    Freitas, Renato P.; Coelho, Filipe A.; Felix, Valter S.; Pereira, Marcelo O.; de Souza, Marcos André Torres; Anjos, Marcelino J.

    2018-03-01

    This study used Raman, FT-IR and XRF spectroscopy and SEM to analyze ceramic fragments dating from the 19th century, excavated from an old farm in the municipality of Pirenópolis, Goiás, Brazil. The results show that the samples were produced in an open oven at a firing temperature below 500 °C, using raw materials including kaolinite, hematite, magnetite, quartz, microcline, albite, anhydrite, calcite, illite, orthoclase and MnO2. Although the analyses showed similarities in the manufacturing process and the presence of many minerals was common in all samples, multivariate statistical methods (PCA) allowed a more detailed assessment of similarities and differences in the mineral composition of the samples. The results of the PCA showed that the samples excavated in one of the slave quarters (senzalas) group with those excavated at the farmhouse, where the landowner lived, which indicates a paternalistic attitude towards captives, including the sharing of ceramic materials of everyday use.

  12. Quantum computational studies, spectroscopic (FT-IR, FT-Raman and UV-Vis) profiling, natural hybrid orbital and molecular docking analysis on 2,4 Dibromoaniline

    Science.gov (United States)

    Abraham, Christina Susan; Prasana, Johanan Christian; Muthu, S.; Rizwana B, Fathima; Raja, M.

    2018-05-01

    The research exploration will comprise of investigating the molecular structure, vibrational assignments, bonding and anti-bonding nature, nonlinear optical, electronic and thermodynamic nature of the molecule. The research is conducted at two levels: First level employs the spectroscopic techniques - FT-IR, FT-Raman and UV-Vis characterizing techniques; at second level the data attained experimentally is analyzed through theoretical methods using and Density Function Theories which involves the basic principle of solving the Schrodinger equation for many body systems. A comparison is drawn between the two levels and discussed. The probability of the title molecule being bio-active theoretically proved by the electrophilicity index leads to further property analyzes of the molecule. The target molecule is found to fit well with Centromere associated protein inhibitor using molecular docking techniques. Higher basis set 6-311++G(d,p) is used to attain results more concurrent to the experimental data. The results of the organic amine 2, 4 Dibromoaniline is analyzed and discussed.

  13. Experimental (FT-IR, FT-Raman, 1H NMR) and theoretical study of magnesium, calcium, strontium, and barium picolinates.

    Science.gov (United States)

    Swiderski, G; Kalinowska, M; Wojtulewski, S; Lewandowski, W

    2006-05-01

    The experimental IR, Raman, and 1H NMR spectra of picolinic acid, as well as magnesium, calcium, strontium, and barium picolinates were registered, assigned and studied. Characteristic changes in the spectra of metal picolinates in comparison with the spectrum of ligand were observed, which lead to the conclusion that perturbation of the aromatic system of picolinates increases along with the series Mg-->Ca-->Sr-->Ba. Theoretical structures of beryllium and magnesium picolinates, as well as theoretical IR spectrum of magnesium picolinate were calculated in B3PW91/6-311++G(d, p) level. On the basis of calculated bond lengths in pyridine ring geometric, aromaticity indexes HOMA were calculated. The idea of these indexes is based on the fact that the essential factor in aromatic stabilization is the pi delocalization manifested in: planar geometry, equalization of the bond lengths and angles, and symmetry. The decidedly lower value of HOMA for magnesium picolinate (i.e. 0.545; 0.539) than that for beryllium picolinate (i.e. 0.998; 0.998) indicate higher aromatic properties of Be picolinate than of Mg picolinate. The comparison of theoretical and literature experimental structures of magnesium picolinate was done. The experimental structure contains two water molecules, so the calculations for hydrated magnesium picolinate were carried on, and the influence of coordinated water molecule on the structure of picolinates was discussed. The HOMAs for hydrated experimental and calculated Mg picolinate amount to 0.870; 0.743, and 0.900; 0.890, respectively, whereas for anhydrous structure, it is as described above, i.e. 0.545; 0.539. Thus, the calculations clearly showed that water molecules coordinated to the central atom weakens the effect of metal on the electronic system of ligand.

  14. Minerals from Macedonia. XII. The dependence of quartz and opal color on trace element composition - AAS, FT IR and micro-Raman spectroscopy study

    International Nuclear Information System (INIS)

    Makreski, Petre; Jovanovski, Gligor; Stafilov, Trajce; Boev, Blazho

    2004-01-01

    The dependence of the color of quartz and opal natural minerals, collected from different localities in the Republic of Macedonia (Alinci, Belutche, Budinarci, Mariovo, Sasa, Sazhdevo, Chanishte, Cheshinovo, Zletovo) on their element composition is studied using Fourier transform infrared spectroscopy (FT IR), micro-Raman spectroscopy and atomic absorption spectrometry (AAS). In order to determine the content of different trace elements (Al, Cd, Ca, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb and Zn), 15 quartz and 2 opal mineral samples, using flame atomic absorption spectrometry (FAAS) and Zeeman electrothermal atomic absorption spectrometry (ETAAS) are studied. To avoid matrix interferences, the method for elimination of silicium is proposed. Optimal instrumental parameters for ETAAS determination (temperature and time for drying, pyrolysis and atomizing) are established by extensive testing for each investigated element. It is found that the milky white color of quartz minerals is due to the presence of traces of Ca, the appearance of black color is the result of the existence of Pb, Mn and Al impurities, and the occurrence of Fe and Cr introduce appearance of red and green color, respectively. Preliminary identification of the minerals is based on the comparison of our results, obtained by using the infrared and Raman vibrational spectroscopy, with the corresponding literature data for the analogous mineral species originating all over the world. An overview of the basic morphological and physico-chemical characteristics of the quartz and opal minerals and the geology of the localities is given. The colored pictures of the studied quartz and opal minerals are presented as well. (Author)

  15. Spectroscopic [FT-IR and FT-Raman] and molecular modeling (MM) study of benzene sulfonamide molecule using quantum chemical calculations

    Science.gov (United States)

    Vinod, K. S.; Periandy, S.; Govindarajan, M.

    2016-07-01

    The spectroscopic and molecular modeling (MM) study includes, FT-IR, FT-Raman and 13C NMR and 1H NMR spectra of the Benzene sulfonamide were recorded for the analysis. The observed experimental and theoretical frequencies (IR and Raman) were assigned according to their distinctive region. The present study of this title molecule have been carried out by hybrid computational calculations of HF and DFT (B3LYP) methods with 6-311+G(d,p) and 6-311++G(d,p) basis sets and the corresponding results are tabulated. The structural modifications of the compound due to the substitutions of NH2 and SO2 were investigated. The minimum energy conformers of the compound were studied using conformational analysis. The alternations of the vibrational pattern of the base structure related to the substitutions were analyzed. The thermodynamic parameters (such as zero-point vibrational energy, thermal energy, specific heat capacity, rotational constants, entropy, and dipole moment) of Benzene sulfonamide have been calculated. The donor acceptor interactions of the compound and the corresponding UV transitions are found out using NBO analysis. The NMR spectra were simulated by using the gauge independent atomic orbital (GIAO) method with B3LYP methods and the 6-311++G(d,p) basis set and their spectra were simulated and the chemical shifts related to TMS were compared. A quantum computational study on the electronic and optical properties absorption wavelengths, excitation energy, dipole moment and frontier molecular orbital energies, were performed by HF and DFT methods. The energy gap of the present compound was calculated related to HOMO and LUMO energies which confirm the occurring of charge transformation between the base and ligand group. Besides frontier molecular orbitals (FMO), molecular electrostatic potential (MEP) was performed. The thermodynamic properties (heat capacity, entropy, and enthalpy) of the title compound at different temperatures were calculated in gas phase and

  16. Characterization of prepared In2O3 thin films: The FT-IR, FT-Raman, UV-Visible investigation and optical analysis.

    Science.gov (United States)

    Panneerdoss, I Joseph; Jeyakumar, S Johnson; Ramalingam, S; Jothibas, M

    2015-08-05

    In this original work, the Indium oxide (In2O3) thin film is deposited cleanly on microscope glass substrate at different temperatures by spray pyrolysis technique. The physical properties of the films are characterized by XRD, SEM, AFM and AFM measurements. The spectroscopic investigation has been carried out on the results of FT-IR, FT-Raman and UV-Visible. XRD analysis exposed that the structural transformation of films from stoichiometric to non-stoichiometric orientation of the plane vice versa and also found that, the film is polycrystalline in nature having cubic crystal structure with a preferred grain orientation along (222) plane. SEM and AFM studies revealed that, the film with 0.1M at 500°C has spherical grains with uniform dimension. The complete vibrational analysis has been carried out and the optimized parameters are calculated using HF and DFT (CAM-B3LYP, B3LYP and B3PW91) methods with 3-21G(d,p) basis set. Furthermore, NMR chemical shifts are calculated by using the gauge independent atomic orbital (GIAO) technique. The molecular electronic properties; absorption wavelengths, excitation energy, dipole moment and frontier molecular orbital energies, molecular electrostatic potential energy (MEP) analysis and Polarizability first order hyperpolarizability calculations are performed by time dependent DFT (TD-DFT) approach. The energy excitation on electronic structure is investigated and the assignment of the absorption bands in the electronic spectra of steady compound is discussed. The calculated HOMO and LUMO energies showed the enhancement of energy gap by the addition of substitutions with the base molecule. The thermodynamic properties (heat capacity, entropy, and enthalpy) at different temperatures are calculated and interpreted in gas phase. Crown Copyright © 2015. Published by Elsevier B.V. All rights reserved.

  17. FT-IR, FT-Raman, UV-visible, and NMR spectroscopy and vibrational properties of the labdane-type diterpene 13-epi-sclareol.

    Science.gov (United States)

    Chain, Fernando E; Leyton, Patricio; Paipa, Carolina; Fortuna, Mario; Brandán, Silvia A

    2015-03-05

    In this work, FT-IR, FT-Raman, UV-Visible and NMR spectroscopies and density functional theory (DFT) calculations were employed to study the structural and vibrational properties of the labdane-type diterpene 13-epi-sclareol using the hybrid B3LYP method together with the 6-31G(∗) basis set. Three stable structures with minimum energy found on the potential energy curves (PES) were optimized, and the corresponding molecular electrostatic potentials, atomic charges, bond orders, stabilization energies and topological properties were computed at the same approximation level. The complete assignment of the bands observed in the vibrational spectrum of 13-epi-sclareol was performed taking into account the internal symmetry coordinates for the three structures using the scaled quantum mechanical force field (SQMFF) methodology at the same level of theory. In addition, the force constants were calculated and compared with those reported in the literature for similar compounds. The predicted vibrational spectrum and the calculated (1)H NMR and (13)C NMR chemical shifts are in good agreement with the corresponding experimental results. The theoretical UV-Vis spectra for the most stable structure of 13-epi-sclareol demonstrate a better correlation with the corresponding experimental spectrum. The study of the three conformers by means of the theory of atoms in molecules (AIM) revealed different H bond interactions and a strong dependence of the interactions on the distance between the involved atoms. Furthermore, the natural bond orbital (NBO) calculations showed the characteristics of the electronic delocalization for the two six-membered rings with chair conformations. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Spectroscopic [FT-IR and FT-Raman] and theoretical [UV-Visible and NMR] analysis on α-Methylstyrene by DFT calculations.

    Science.gov (United States)

    Karthikeyan, N; Joseph Prince, J; Ramalingam, S; Periandy, S

    2015-05-15

    In the present research work, the FT-IR, FT-Raman and (13)C and (1)H NMR spectra of the α-Methylstyrene were recorded. The observed fundamental frequencies in finger print as well as functional group regions were assigned according to their uniqueness region. The Gaussian computational calculations are carried out by HF and DFT (B3LYP and B3PW91) methods with 6-31++G(d,p) and 6-311++G(d,p) basis sets and the corresponding results were tabulated. The impact of the presence of vinyl group in phenyl structure of the compound is investigated. The modified vibrational pattern of the molecule associated vinyl group was analyzed. Moreover, (13)C NMR and (1)H NMR were calculated by using the gauge independent atomic orbital (GIAO) method with B3LYP methods and the 6-311++G(d,p) basis set and their spectra were simulated and the chemical shifts linked to TMS were compared. A study on the electronic and optical properties; absorption wavelengths, excitation energy, dipole moment and frontier molecular orbital energies were carried out. The kubo gap of the present compound was calculated related to HOMO and LUMO energies which confirm the occurring of charge transformation between the base and ligand. Besides frontier molecular orbitals (FMO), molecular electrostatic potential (MEP) was performed. The NLO properties related to Polarizability and hyperpolarizability based on the finite-field approach were also discussed. Crown Copyright © 2015. Published by Elsevier B.V. All rights reserved.

  19. Molecular structure, electronic properties, NLO, NBO analysis and spectroscopic characterization of Gabapentin with experimental (FT-IR and FT-Raman) techniques and quantum chemical calculations

    Science.gov (United States)

    Sinha, Leena; Karabacak, Mehmet; Narayan, V.; Cinar, Mehmet; Prasad, Onkar

    2013-05-01

    Gabapentin (GP), structurally related to the neurotransmitter GABA (gamma-aminobutyric acid), mimics the activity of GABA and is also widely used in neurology for the treatment of peripheral neuropathic pain. It exists in zwitterionic form in solid state. The present communication deals with the quantum chemical calculations of energies, geometrical structure and vibrational wavenumbers of GP using density functional (DFT/B3LYP) method with 6-311++G(d,p) basis set. In view of the fact that amino acids exist as zwitterions as well as in the neutral form depending on the environment (solvent, pH, etc.), molecular properties of both the zwitterionic and neutral form of GP have been analyzed. The fundamental vibrational wavenumbers as well as their intensities were calculated and compared with experimental FT-IR and FT-Raman spectra. The fundamental assignments were done on the basis of the total energy distribution (TED) of the vibrational modes, calculated with scaled quantum mechanical (SQM) method. The electric dipole moment, polarizability and the first hyperpolarizability values of the GP have been calculated at the same level of theory and basis set. The nonlinear optical (NLO) behavior of zwitterionic and neutral form has been compared. Stability of the molecule arising from hyper-conjugative interactions and charge delocalization has been analyzed using natural bond orbital analysis. Ultraviolet-visible (UV-Vis) spectrum of the title molecule has also been calculated using TD-DFT method. The thermodynamic properties of both the zwitterionic and neutral form of GP at different temperatures have been calculated.

  20. Synthesis, geometry optimization, spectroscopic investigations (UV/Vis, excited states, FT-IR) and application of new azomethine dyes

    Science.gov (United States)

    Shahab, Siyamak; Sheikhi, Masoome; Filippovich, Liudmila; Kumar, Rakesh; Dikusar, Evgenij; Yahyaei, Hooriye; Khaleghian, Mehrnoosh

    2017-11-01

    In the present work, the quantum theoretical calculations of the molecular structures of the four new synthesized azomethine dyes such as: (E)-N-(4-butoxybenzylidene)-4-((E)-phenyldiazenyl)aniline (PAZB-6), (E)-N-(4-(benzyloxy)benzylidene)-4-((E))-phenyldiazenyl)aniline (PAZB-7), 4-((E)-4-((E)-phenyldiazenyl)phenyl)imino)methyl)phenol (PAZB-8), (E)-N-(4-methoxybenzylidene)-4-((E))-phenyldiazenyl)aniline (PAZB-9) have been predicted using Density Functional Theory in the solvent Dimethylformamide. The geometries of the azomethine dyes were optimized by PBE1PBE/6-31+G* level of theory. The electronic spectra of the title compounds in the solvent DMF was carried out by TDPBE1PBE/6-31+G* method. FT-IR spectra of the title compounds are recorded and discussed. Frontier molecular orbitals, molecular electrostatic potential, electronic properties, natural charges and Natural Bond Orbital (NBO) analysis of the mentioned compounds were investigated and discussed by theoretical calculations. The azomethine dyes were synthesized after quantum chemical modeling for optical applications. A new study of anisotropy of thermal and electrical conductivity of the colored stretched PVA-films have been undertaken.

  1. Spectroscopic (FT-IR, FT-Raman, NMR and UV-Visible) and quantum chemical studies of molecular geometry, Frontier molecular orbital, NLO, NBO and thermodynamic properties of salicylic acid.

    Science.gov (United States)

    Suresh, S; Gunasekaran, S; Srinivasan, S

    2014-11-11

    The solid phase FT-IR and FT-Raman spectra of 2-hydroxybenzoic acid (salicylic acid) have been recorded in the region 4000-400 and 4000-100 cm(-1) respectively. The optimized molecular geometry and fundamental vibrational frequencies are interpreted with the aid of structure optimizations and normal coordinate force field calculations based on density functional theory (DFT) method and a comparative study between Hartree Fork (HF) method at 6-311++G(d,p) level basis set. The calculated harmonic vibrational frequencies are scaled and they are compared with experimentally obtained FT-IR and FT-Raman spectra. A detailed interpretation of the vibrational spectra of this compound has been made on the basis of the calculated potential energy distribution (PED). The time dependent DFT method is employed to predict its absorption energy and oscillator strength. The linear polarizability (α) and the first order hyper polarizability (β) values of the investigated molecule have been computed. The electronic properties, such as HOMO and LUMO energies, molecular electrostatic potential (MEP) are also performed. Stability of the molecule arising from hyper conjugative interaction, charge delocalization has been analyzed using natural bond orbital (NBO) analysis. Published by Elsevier B.V.

  2. Spectroscopic investigations (FT-IR & FT-Raman) and molecular docking analysis of 6-[1-methyl-4-nitro-1H-imidazol-5-yl) sulfonyl]-7H-purine

    Science.gov (United States)

    Prasath, M.; Govindammal, M.; Sathya, B.

    2017-10-01

    The Azathioprine is used as anticancer agent. Azathioprine is chemically called 6-[1-methyl-4-nitro-1H-imidazol-5-yl) sulfonyl]-7H-purine (6M4N5P). The vibrational analysis of the 6M4N5P compound was carried out by using FT-IR and FT-Raman spectroscopic techniques and compared with aspects. The optimized geometry, frequency and intensity of the vibrational bands of 6M4N5P were obtained from the HF and DFT methods with 6-31G (d,p) basis set. The harmonic vibrational frequencies were calculated and the scaled values have been compared with experimental FT-IR and FT-Raman spectra. The calculated Highest Occupied Molecular Orbital (HOMO) and Lowest Unoccupied Molecular Orbital (LUMO) energies show that charge transfer occur within the molecule. MEP (Molecular Electrostatic Potential) is very useful in the investigation of the charge distributions and molecular structure. The molecule orbital contributions were determined by using the total density of states (TDOS). A molecular docking analysis has been carried out to understand the conformational change and electrostatic properties of 6M4N5P in the active site of Rac1-Receptor.

  3. Thiol-thione tautomeric analysis, spectroscopic (FT-IR, Laser-Raman, NMR and UV-vis) properties and DFT computations of 5-(3-pyridyl)-4H-1,2,4-triazole-3-thiol molecule.

    Science.gov (United States)

    Gökce, Halil; Öztürk, Nuri; Ceylan, Ümit; Alpaslan, Yelda Bingöl; Alpaslan, Gökhan

    2016-06-15

    In this study, the 5-(3-pyridyl)-4H-1,2,4-triazole-3-thiol molecule (C7H6N4S) molecule has been characterized by using FT-IR, Laser-Raman, NMR and UV-vis spectroscopies. Quantum chemical calculations have been performed to investigate the molecular structure (thione-thiol tautomerism), vibrational wavenumbers, electronic transition absorption wavelengths in DMSO solvent and vacuum, proton and carbon-13 NMR chemical shifts and HOMOs-LUMOs energies at DFT/B3LYP/6-311++G(d,p) level for all five tautomers of the title molecule. The obtained results show that the calculated vibrational wavenumbers, NMR chemical shifts and UV-vis wavelengths are in a good agreement with experimental data. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. Theoretical (in B3LYP/6-3111++G** level), spectroscopic (FT-IR, FT-Raman) and thermogravimetric studies of gentisic acid and sodium, copper(II) and cadmium(II) gentisates.

    Science.gov (United States)

    Regulska, E; Kalinowska, M; Wojtulewski, S; Korczak, A; Sienkiewicz-Gromiuk, J; Rzączyńska, Z; Swisłocka, R; Lewandowski, W

    2014-11-11

    The DFT calculations (B3LYP method with 6-311++G(d,p) mixed with LanL2DZ for transition metals basis sets) for different conformers of 2,5-dihydroxybenzoic acid (gentisic acid), sodium 2,5-dihydroxybenzoate (gentisate) and copper(II) and cadmium(II) gentisates were done. The proposed hydrated structures of transition metal complexes were based on the results of experimental findings. The theoretical geometrical parameters and atomic charge distribution were discussed. Moreover Na, Cu(II) and Cd(II) gentisates were synthesized and the composition of obtained compounds was revealed by means of elemental and thermogravimetric analyses. The FT-IR and FT-Raman spectra of gentisic acid and gentisates were registered and the effect of metals on the electronic charge distribution of ligand was discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Spectroscopic investigation (FT-IR and FT-Raman), vibrational assignments, HOMO-LUMO analysis and molecular docking study of 1-hydroxy-4,5,8-tris(4-methoxyphenyl) anthraquinone

    Science.gov (United States)

    Renjith, R.; Sheena Mary, Y.; Tresa Varghese, Hema; Yohannan Panicker, C.; Thiemann, Thies; Shereef, Anas; Al-Saadi, Abdulaziz A.

    2015-12-01

    FT-IR and FT-Raman spectra of 1-hydroxy-4,5,8-tris(4-methoxyphenyl)anthraquinone were recorded and analyzed. The vibrational wavenumbers were computed using DFT quantum chemical calculations. The data obtained from wavenumber calculations were used to assign the vibrational bands obtained experimentally. A detailed molecular picture of the title compound and its interactions were obtained from NBO analysis. From the MEP plot it is clear that the negative electrostatic potential regions are mainly localized over carbonyl group. There is some evidence of a region of negative electrostatic potential due to π-electron density of the benzo groups. Molecular docking study shows that methoxy groups attached to the phenyl rings and hydroxyl group are crucial for binding and the title compound might exhibit inhibitory activity against PI3K and may act as an anti-neoplastic agent.

  6. Determination of alkaloids in capsules, milk and ethanolic extracts of poppy (Papaver somniferum L.) by ATR-FT-IR and FT-Raman spectroscopy.

    Science.gov (United States)

    Schulz, Hartwig; Baranska, Malgorzata; Quilitzsch, Rolf; Schütze, Wolfgang

    2004-10-01

    Fourier transform (FT) infrared spectroscopy using a diamond composite ATR crystal and NIR-FT-Raman spectroscopy techniques were applied for the simultaneous identification and quantification of the most important alkaloids in poppy capsules. Most of the characteristic Raman signals of the alkaloids can be identified in poppy milk isolated from unripe capsules. But also poppy extracts present specific bands relating clearly to the alkaloid fraction. Raman spectra obtained by excitation with a Nd:YAG laser at 1064 nm show no disturbing fluorescence effects; therefore the plant tissue can be recorded without any special preparation. The used diamond ATR technique allows to measure very small sample amounts (5-10 microL or 2-5 mg) without the necessity to perform time-consuming pre-treatments. When applying cluster analysis a reliable discrimination of "low-alkaloid" and "high-alkaloid" poppy single-plants can be easily achieved. The examples presented in this study provide clear evidence of the benefits of Raman and ATR-IR spectroscopy in efficient quality control, forensic analysis and high-throughput evaluation of poppy breeding material.

  7. A new tridentate Schiff base Cu(II) complex: synthesis, experimental and theoretical studies on its crystal structure, FT-IR and UV-Visible spectra.

    Science.gov (United States)

    Saheb, Vahid; Sheikhshoaie, Iran; Setoodeh, Nasim; Rudbari, Hadi Amiri; Bruno, Giuseppe

    2013-06-01

    A new Cu(II) complex [Cu(L)(NCS)] has been synthesized, using 1-(N-salicylideneimino)-2-(N,N-methyl)-aminoethane as tridentate ONN donor Schiff base ligand (HL). The dark green crystals of the compound are used for single-crystal X-ray analysis and measuring Fourier Transform Infrared (FT-IR) and UV-Visible spectra. Electronic structure calculations at the B3LYP and MP2 levels of theory are performed to optimize the molecular geometry and to calculate the UV-Visible and FT-IR spectra of the compound. Vibrational assignments and analysis of the fundamental modes of the compound are performed. Time-dependent density functional theory (TD-DFT) method is used to calculate the electronic transitions of the complex. A scaling factor of 1.015 is obtained for vibrational frequencies computed at the B3LYP level using basis sets 6-311G(d,p). It is found that solvent has a profound effect on the electronic absorption spectrum. The UV-Visible spectrum of the complex recorded in DMSO and DMF solution can be correctly predicted by a model in which DMSO and DMF molecules are coordinated to the central Cu atom via their oxygen atoms. Copyright © 2013 Elsevier B.V. All rights reserved.

  8. Spectroscopic (FT-IR, FT-Raman, 1H- and 13C-NMR, Theoretical and Microbiological Study of trans o-Coumaric Acid and Alkali Metal o-Coumarates

    Directory of Open Access Journals (Sweden)

    Małgorzata Kowczyk-Sadowy

    2015-02-01

    Full Text Available This work is a continuation of research on a correlation between the molecular structure and electronic charge distribution of phenolic compounds and their biological activity. The influence of lithium, sodium, potassium, rubidium and cesium cations on the electronic system of trans o-coumaric (2-hydroxy-cinnamic acid was studied. We investigated the relationship between the molecular structure of the tested compounds and their antimicrobial activity. Complementary molecular spectroscopic techniques such as infrared (FT-IR, Raman (FT-Raman, ultraviolet-visible (UV-VIS and nuclear magnetic resonance (1H- and 13C-NMR were applied. Structures of the molecules were optimized and their structural characteristics were calculated by the density functional theory (DFT using the B3LYP method with 6-311++G** as a basis set. Geometric and magnetic aromaticity indices, atomic charges, dipole moments and energies were also calculated. Theoretical parameters were compared to the experimental characteristics of investigated compounds. Correlations between certain vibrational bands and some metal parameters, such as electronegativity, ionization energy, atomic and ionic radius, were found. The microbial activity of studied compounds was tested against Escherichia coli, Bacillus subtilis, Pseudomonas aeruginosa, Staphylococcus aureus, Proteus vulgaris and Candida albicans.

  9. Quantum mechanical and spectroscopic (FT-IR, FT-Raman) study, NBO analysis, HOMO-LUMO, first order hyperpolarizability and molecular docking study of methyl[(3R)-3-(2-methylphenoxy)-3-phenylpropyl]amine by density functional method

    Science.gov (United States)

    Kuruvilla, Tintu K.; Prasana, Johanan Christian; Muthu, S.; George, Jacob; Mathew, Sheril Ann

    2018-01-01

    Quantum chemical techniques such as density functional theory (DFT) have become a powerful tool in the investigation of the molecular structure and vibrational spectrum and are finding increasing use in application related to biological systems. The Fourier transform infrared (FT-IR) and Fourier transform Raman (FT-Raman) techniques are employed to characterize the title compound. The vibrational frequencies were obtained by DFT/B3LYP calculations with 6-31G(d,p) and 6-311 ++G(d,p) as basis sets. The geometry of the title compound was optimized. The vibrational assignments and the calculation of Potential Energy Distribution (PED) were carried out using the Vibrational Energy Distribution Analysis (VEDA) software. Molecular electrostatic potential was calculated for the title compound to predict the reactive sites for electrophilic and nucleophilic attack. In addition, the first-order hyperpolarizability, HOMO and LUMO energies, Fukui function and NBO were computed. The thermodynamic properties of the title compound were calculated at different temperatures, revealing the correlations between heat capacity (C), entropy (S) and enthalpy changes (H) with temperatures. Molecular docking studies were also conducted as part of this study. The paper further explains the experimental results which are in line with the theoretical calculations and provide optimistic evidence through molecular docking that the title compound can act as a good antidepressant. It also provides sufficient justification for the title compound to be selected as a good candidate for further studies related to NLO properties.

  10. Characterization of writing materials of books of great historical-artistic value by FT-IR and micro-raman spectroscopy

    Directory of Open Access Journals (Sweden)

    Vito Librando

    2014-12-01

    Full Text Available This work describes the application of Fourier-Transform Infrared and Raman spectroscopic techniques for the characterization of cellulose paper samples and inks used on ancient writing materials. These samples from books of high historical and artistic interest were provided by the Public Library of Syracuse.The ancient paper showed a characteristic pattern of carbonyl groups, whose vibration modes were observed in FTIR spectra. The spectra of ancient paper samples were compared to each other and to modern paper in order to highlight differences in conservation state between new and old papers. The paper aging process is related to the presence of acid substances and oxidative agents that result in cellulose hydrolysis leading to the shortening of its chain along with changes in the amount of the crystalline form. This hydrolysis causes changes in hydrogen bonds and consequently change the CCH, COH, OCH and HCH bending vibrations mode. In this work, the FTIR and Raman spectra of inks used on ancient paper and parchment samples were also discussed.

  11. QM/MM methodology, docking and spectroscopic (FT-IR/FT-Raman, NMR, UV) and Fukui function analysis on adrenergic agonist

    Science.gov (United States)

    Uma Maheswari, J.; Muthu, S.; Sundius, Tom

    2015-02-01

    The Fourier transform infrared, FT-Raman, UV and NMR spectra of Ternelin have been recorded and analyzed. Harmonic vibrational frequencies have been investigated with the help of HF with 6-31G (d,p) and B3LYP with 6-31G (d,p) and LANL2DZ basis sets. The 1H and 13C nuclear magnetic resonance (NMR) chemical shifts of the molecule were calculated by GIAO method. The polarizability (α) and the first hyperpolarizability (β) values of the investigated molecule have been computed using DFT quantum mechanical calculations. Stability of the molecule arising from hyper conjugative interactions, and charge delocalization has been analyzed using natural bond orbital (NBO) analysis. The electron density-based local reactivity descriptors such as Fukui functions were calculated to explain the chemical selectivity or reactivity site in Ternelin. Finally the calculated results were compared to simulated infrared and Raman spectra of the title compound which show good agreement with observed spectra. Molecular docking studies have been carried out in the active site of Ternelin and reactivity with ONIOM was also investigated.

  12. FT-IR, FT-Raman spectra, density functional computations of the vibrational spectra and molecular conformational analysis of 2,5-di-tert-butyl-hydroquinone

    Science.gov (United States)

    Subramanian, N.; Sundaraganesan, N.; Dereli, Ö.; Türkkan, E.

    2011-12-01

    The purpose of finding conformer among six different possible conformers of 2,5-di-tert-butyl-hydroquinone (DTBHQ), its equilibrium geometry and harmonic wavenumbers were calculated by the B3LYP/6-31G(d,p) method. The infrared and Raman spectra of DTBHQ were recorded in the region 400-4000 cm -1 and 50-3500 cm -1, respectively. In addition, the IR spectra in CCl 4 at various concentrations of DTBHQ are also recorded. The computed vibrational wavenumbers were compared with the IR and Raman experimental data. Computational calculations at B3LYP level with two different basis sets 6-31G(d,p) and 6-311++G(d,p) are also employed in the study of the possible conformer of DTBHQ. The complete assignments were performed on the basis of the potential energy distribution (PED) of the vibrational modes, calculated using VEDA 4 program. The general agreement between the observed and calculated frequencies was established.

  13. FT-Raman, FT-IR and UV-visible spectral investigations and ab initio computations of anti-epileptic drug: Vigabatrin

    Science.gov (United States)

    Edwin, Bismi; Joe, I. Hubert

    2013-10-01

    Vibrational analysis of anti-epileptic drug vigabatrin, a structural GABA analog was carried out using NIR FT-Raman and FTIR spectroscopic techniques. The equilibrium geometry, various bonding features and harmonic vibrational wavenumbers were studied using density functional theory method. The detailed interpretation of the vibrational spectra has been carried out with the aid of VEDA.4 program. Vibrational spectra, natural bond orbital analysis and optimized molecular structure show clear evidence for the effect of electron charge transfer on the activity of the molecule. Predicted electronic absorption spectrum from TD-DFT calculation has been compared with the UV-vis spectrum. The Mulliken population analysis on atomic charges and the HOMO-LUMO energy were also calculated. Good consistency is found between the calculated results and experimental data for the electronic absorption as well as IR and Raman spectra. The blue-shifting of the Csbnd C stretching wavenumber reveals that the vinyl group is actively involved in the conjugation path. The NBO analysis confirms the occurrence of intramolecular hyperconjugative interactions resulting in ICT causing stabilization of the system.

  14. FT-Raman, FT-IR and UV-visible spectral investigations and ab initio computations of anti-epileptic drug: vigabatrin.

    Science.gov (United States)

    Edwin, Bismi; Joe, I Hubert

    2013-10-01

    Vibrational analysis of anti-epileptic drug vigabatrin, a structural GABA analog was carried out using NIR FT-Raman and FTIR spectroscopic techniques. The equilibrium geometry, various bonding features and harmonic vibrational wavenumbers were studied using density functional theory method. The detailed interpretation of the vibrational spectra has been carried out with the aid of VEDA.4 program. Vibrational spectra, natural bond orbital analysis and optimized molecular structure show clear evidence for the effect of electron charge transfer on the activity of the molecule. Predicted electronic absorption spectrum from TD-DFT calculation has been compared with the UV-vis spectrum. The Mulliken population analysis on atomic charges and the HOMO-LUMO energy were also calculated. Good consistency is found between the calculated results and experimental data for the electronic absorption as well as IR and Raman spectra. The blue-shifting of the C-C stretching wavenumber reveals that the vinyl group is actively involved in the conjugation path. The NBO analysis confirms the occurrence of intramolecular hyperconjugative interactions resulting in ICT causing stabilization of the system. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. Electronic [UV-Visible] and vibrational [FT-IR, FT-Raman] investigation and NMR-mass spectroscopic analysis of terephthalic acid using quantum Gaussian calculations

    Science.gov (United States)

    Karthikeyan, N.; Joseph Prince, J.; Ramalingam, S.; Periandy, S.

    2015-03-01

    In this research work, the vibrational IR, polarization Raman, NMR and mass spectra of terephthalic acid (TA) were recorded. The observed fundamental peaks (IR, Raman) were assigned according to their distinctiveness region. The hybrid computational calculations were carried out for calculating geometrical and vibrational parameters by DFT (B3LYP and B3PW91) methods with 6-31++G(d,p) and 6-311++G(d,p) basis sets and the corresponding results were tabulated. The molecular mass spectral data related to base molecule and substitutional group of the compound was analyzed. The modification of the chemical property by the reaction mechanism of the injection of dicarboxylic group in the base molecule was investigated. The 13C and 1H NMR spectra were simulated by using the gauge independent atomic orbital (GIAO) method and the absolute chemical shifts related to TMS were compared with experimental spectra. The study on the electronic and optical properties; absorption wavelengths, excitation energy, dipole moment and frontier molecular orbital energies, were performed by hybrid Gaussian calculation methods. The orbital energies of different levels of HOMO and LUMO were calculated and the molecular orbital lobe overlapping showed the inter charge transformation between the base molecule and ligand group. From the frontier molecular orbitals (FMO), the possibility of electrophilic and nucleophilic hit also analyzed. The NLO activity of the title compound related to Polarizability and hyperpolarizability were also discussed. The present molecule was fragmented with respect to atomic mass and the mass variation depends on the substitutions have also been studied.

  16. Electronic [UV-Visible] and vibrational [FT-IR, FT-Raman] investigation and NMR-mass spectroscopic analysis of terephthalic acid using quantum Gaussian calculations.

    Science.gov (United States)

    Karthikeyan, N; Prince, J Joseph; Ramalingam, S; Periandy, S

    2015-03-15

    In this research work, the vibrational IR, polarization Raman, NMR and mass spectra of terephthalic acid (TA) were recorded. The observed fundamental peaks (IR, Raman) were assigned according to their distinctiveness region. The hybrid computational calculations were carried out for calculating geometrical and vibrational parameters by DFT (B3LYP and B3PW91) methods with 6-31++G(d,p) and 6-311++G(d,p) basis sets and the corresponding results were tabulated. The molecular mass spectral data related to base molecule and substitutional group of the compound was analyzed. The modification of the chemical property by the reaction mechanism of the injection of dicarboxylic group in the base molecule was investigated. The (13)C and (1)H NMR spectra were simulated by using the gauge independent atomic orbital (GIAO) method and the absolute chemical shifts related to TMS were compared with experimental spectra. The study on the electronic and optical properties; absorption wavelengths, excitation energy, dipole moment and frontier molecular orbital energies, were performed by hybrid Gaussian calculation methods. The orbital energies of different levels of HOMO and LUMO were calculated and the molecular orbital lobe overlapping showed the inter charge transformation between the base molecule and ligand group. From the frontier molecular orbitals (FMO), the possibility of electrophilic and nucleophilic hit also analyzed. The NLO activity of the title compound related to Polarizability and hyperpolarizability were also discussed. The present molecule was fragmented with respect to atomic mass and the mass variation depends on the substitutions have also been studied. Crown Copyright © 2014. Published by Elsevier B.V. All rights reserved.

  17. Quantum mechanical study and spectroscopic (FT-IR, FT-Raman, UV-Visible) study, potential energy surface scan, Fukui function analysis and HOMO-LUMO analysis of 3-tert-butyl-4-methoxyphenol by DFT methods.

    Science.gov (United States)

    Saravanan, S; Balachandran, V

    2014-09-15

    This study represents an integral approach towards understanding the electronic and structural aspects of 3-tert-butyl-4-methoxyphenol (TBMP). Fourier-transform Infrared (FT-IR) and Fourier-transform Raman (FT-Raman) spectra of TBMP was recorded in the region 4000-400 cm(-1) and 3500-100 cm(-1), respectively. The molecular structures, vibrational wavenumbers, infrared intensities and Raman activities were calculated using DFT (B3LYP and LSDA) methods using 6-311++G (d,p) basis set. The most stable conformer of TBMP was identified from the computational results. The assignments of vibrational spectra have been carried out with the help of normal co-ordinate analysis (NCA) following the scaled quantum mechanical force field (SQMFF) methodology. The first order hyperpolarizability (β0) and related properties (β, α0 and Δα) of TBMP have been discussed. The stability and charge delocalization of the molecule was studied by Natural Bond Orbital (NBO) analysis. UV-Visible spectrum and effects of solvents have been discussed and the electronic properties such as HOMO and LUMO energies were determined by time-dependent TD-DFT approach with B3LYP/6-311++G (d,p) level of theory. The molecule orbital contributions are studied by density of energy states (DOSs). The reactivity sites are identified by mapping the electron density into electrostatic potential surface (MEP). Mulliken analysis of atomic charges is also calculated. The thermodynamic properties at different temperatures were calculated, revealing the correlations between standard heat capacities, standard entropy and standard enthalpy changes with temperatures. Global hardness, global softness, global electrophilicity and ionization potential of the title compound are determined. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. FT-IR and Raman vibrational analysis, B3LYP and M06-2X simulations of 4-bromomethyl-6-tert-butyl-2H-chromen-2-one

    Science.gov (United States)

    Sert, Yusuf; Puttaraju, K. B.; Keskinoğlu, Sema; Shivashankar, K.; Ucun, Fatih

    2015-01-01

    In this study, the experimental and theoretical vibrational frequencies of a newly synthesized bacteriostatic and anti-tumor molecule namely, 4-bromomethyl-6-tert-butyl-2H-chromen-2-one have been investigated. The experimental FT-IR (4000-400 cm-1) and Raman spectra (4000-100 cm-1) of the compound in solid phase have been recorded. The theoretical vibrational frequencies and optimized geometric parameters have been calculated using density functional theory (DFT/B3LYP: Becke, 3-parameter, Lee-Yang-Parr and DFT/M06-2X: highly parametrized, empirical exchange correlation function) with 6-311++G(d, p) basis set by Gaussian 03 software, for the first time. The assignments of the vibrational frequencies have been done by potential energy distribution (PED) analysis using VEDA 4 software. The theoretical optimized geometric parameters and vibrational frequencies have been found to be in good agreement with the corresponding experimental data and results in the literature. In addition, the highest occupied molecular orbital (HOMO) energy, the lowest unoccupied molecular orbital (LUMO) energy and the other related molecular energy values of the compound have been investigated using the same theoretical calculations.

  19. Experimental FT-IR, Laser-Raman and DFT spectroscopic analysis of a potential chemotherapeutic agent 6-(2-methylpropyl)-4-oxo-2-sulfanylidene-1,2,3,4-tetrahydropyrimidine-5-carbonitrile.

    Science.gov (United States)

    Sert, Yusuf; Al-Turkistani, Abdulghafoor A; Al-Deeb, Omar A; El-Emam, Ali A; Ucun, Fatih; Çırak, Çağrı

    2014-01-01

    In this study, the experimental and theoretical vibrational frequencies of a newly synthesized potential chemotherapeutic agent namely, 6-(2-methylpropyl)-4-oxo-2-sulfanylidene-1,2,3,4-tetrahydropyrimidine-5-carbonitrile have been investigated. The experimental FT-IR (4000-400 cm(-1)) and Laser-Raman spectra (4000-100 cm(-1)) of the molecule in solid phase have been recorded. The theoretical vibrational frequencies and optimized geometric parameters (bond lengths and bond angles) have been calculated by using density functional theory (DFT/B3LYP: Becke, 3-parameter, Lee-Yang-Parr) and M06-2X (the highly parametrized, empirical exchange correlation function) quantum chemical methods with 6-311++G(d,p) basis set by Gaussian 09 W software, for the first time. The assignments of the vibrational frequencies have been done by potential energy distribution (PED) analysis by using VEDA 4 software. The theoretical optimized geometric parameters and vibrational frequencies have been found to be in good agreement with the corresponding experimental data, and with the results in the literature. In addition, the highest occupied molecular orbital (HOMO) and the lowest unoccupied molecular orbital (LUMO) energies and the other related molecular energy values have been calculated and depicted. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Vibrational spectroscopy (FT-IR and Laser-Raman) investigation, and computational (M06-2X and B3LYP) analysis on the structure of 4-(3-fluorophenyl)-1-(propan-2-ylidene)-thiosemicarbazone.

    Science.gov (United States)

    Sert, Yusuf; Miroslaw, Barbara; Çırak, Çağrı; Doğan, Hatice; Szulczyk, Daniel; Struga, Marta

    2014-07-15

    In this study, the experimental and theoretical vibrational spectral analysis of 4-(3-fluorophenyl)-1-(propan-2-ylidene)-thiosemicarbazone have been carried out. The experimental FT-IR (4000-400 cm(-1)) and Laser-Raman spectra (4000-100 cm(-1)) have been recorded for the solid state samples. The theoretical vibrational frequencies and the optimized geometric parameters (bond lengths and angles) have been calculated for gas phase using density functional theory (DFT/B3LYP: Becke, 3-parameter, Lee-Yang-Parr) and M06-2X (the highly parametrized, empirical exchange correlation function) quantum chemical methods with 6-311++G(d,p) basis set. The diversity in molecular geometry of fluorophenyl substituted thiosemicarbazones has been discussed based on the X-ray crystal structure reports and theoretical calculation results from the literature. The assignments of the vibrational frequencies have been done on the basis of potential energy distribution (PED) analysis by using VEDA4 software. A good correlation was found between the computed and experimental geometric and vibrational data. In addition, the highest occupied (HOMO) and lowest unoccupied (LUMO) molecular orbital energy levels and other related molecular energy values of the compound have been determined using the same level of theoretical calculations. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Structural, Spectroscopic (FT-IR, Raman and NMR, Non-linear Optical (NLO, HOMO-LUMO and Theoretical (DFT/CAM-B3LYP Analyses of N-Benzyloxycarbonyloxy-5-Norbornene-2,3-Dicarboximide Molecule

    Directory of Open Access Journals (Sweden)

    Nuri ÖZTÜRK

    2018-02-01

    Full Text Available The experimental spectroscopic investigation of N-benzyloxycarbonyloxy-5-norbornene-2,3-dicarboximide (C17H15NO5 molecule has been done using 1H and 13C NMR chemical shifts, FT-IR and Raman spectroscopies. Conformational forms have been determined depending on orientation of N-benzyloxycarbonyloxy and 5-norbornene-2,3-dicarboximide (NDI groups of the title compound. The structural geometric optimizations, vibrational wavenumbers, NMR chemical shifts (in vacuum and chloroform and HOMO-LUMO analyses for all conformers of the title molecule have been done with DFT/CAM-B3LYP method at the 6-311++G(d,p basis set. Additionally, based on the calculated HOMO and LUMO energy values, some molecular properties such as ionization potential (I, electron affinity (A, electronegativity (χ, chemical hardness (h, chemical softness (z, chemical potential (μ and electrophilicity index (w parameters are determined for all conformers. The non-linear optical (NLO properties have been studied for the title molecule. We can say that the experimental spectral data are in accordance with calculated values.

  2. Spectroscopic studies (FT-IR, FT-Raman, UV-Visible), normal co-ordinate analysis, first-order hyperpolarizability and HOMO, LUMO studies of 3,4-dichlorobenzophenone by using Density Functional Methods.

    Science.gov (United States)

    Venkata Prasad, K; Samatha, K; Jagadeeswara Rao, D; Santhamma, C; Muthu, S; Mark Heron, B

    2015-01-01

    The vibrational frequencies of 3,4-dichlorobenzophenone (DCLBP) were obtained from the FT-IR and Raman spectral data, and evaluated based on the Density Functional Theory using the standard method B3LYP with 6-311+G(d,p) as the basis set. On the basis of potential energy distribution together with the normal-co-ordinate analysis and following the scaled quantum mechanical force methodology, the assignments for the various frequencies were described. The values of the electric dipole moment (μ) and the first-order hyperpolarizability (β) of the molecule were computed. The UV-absorption spectrum was also recorded to study the electronic transitions. The calculated HOMO and LUMO energies show that charge transfer occurs within the molecule. The NBO analysis, to study the intramolecular hyperconjugative interactions, was carried out. Mulliken's net charges were evaluated. The MEP and thermodynamic properties were also calculated. The electron density-based local reactivity descriptor, such as Fukui functions, was calculated to explain the chemical selectivity or reactivity site in 3,4-dichlorobenzophenone. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Spectroscopic (FT-IR, FT-Raman, and UV-visible) and quantum chemical studies on molecular geometry, Frontier molecular orbitals, NBO, NLO and thermodynamic properties of 1-acetylindole.

    Science.gov (United States)

    Shukla, Vikas K; Al-Abdullah, Ebtehal S; El-Emam, Ali A; Sachan, Alok K; Pathak, Shilendra K; Kumar, Amarendra; Prasad, Onkar; Bishnoi, Abha; Sinha, Leena

    2014-12-10

    Quantum chemical calculations of ground state energy, geometrical structure and vibrational wavenumbers of 1-acetylindole were carried out using density functional (DFT/B3LYP) method with 6-311++G(d,p) basis set. The FT-IR and FT-Raman spectra were recorded in the condensed state. The fundamental vibrational wavenumbers were calculated and a good correlation between experimental and scaled calculated wavenumbers has been accomplished. Electric dipole moment, polarizability and first static hyperpolarizability values of 1-acetylindole have been calculated at the same level of theory and basis set. The results show that the 1-acetylindole molecule possesses nonlinear optical (NLO) behavior with non-zero values. Stability of the molecule arising from hyper-conjugative interactions and charge delocalization has been analyzed using natural bond orbital (NBO) analysis. UV-Visible spectrum of the molecule was recorded in the region 200-500nm and the electronic properties like HOMO and LUMO energies and composition were obtained using TD-DFT method. The calculated energies and oscillator strengths are in good correspondence with the experimental data. The thermodynamic properties of the compound under investigation were calculated at different temperatures. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Effect of alkali metal ions on the pyrrole and pyridine π-electron systems in pyrrole-2-carboxylate and pyridine-2-carboxylate molecules: FT-IR, FT-Raman, NMR and theoretical studies

    Science.gov (United States)

    Świderski, G.; Wojtulewski, S.; Kalinowska, M.; Świsłocka, R.; Lewandowski, W.

    2011-05-01

    The FT-IR, FT-Raman and 1H and 13C NMR spectra of pyrrole-2-carboxylic acid (PCA) and lithium, sodium, potassium, rubidium and caesium pyrrole-2-carboxylates were recorded, assigned and compared in the Li → Na → K → Rb → Cs salt series. The effect of alkali metal ions on the electronic system of ligands was discussed. The obtained results were compared with previously reported ones for pyridine-2-carboxylic acid and alkali metal pyridine-2-carboxylates. Calculations for pyrrole-2-carboxylic acid and Li, Na, K pyrrole-2-carboxylates in B3LYP/6-311++G ** level and Møller-Plesset method in MP2/6-311++G ** level were made. Bond lengths, angles and dipole moments as well as aromaticity indices (HOMA, EN, GEO, I 6) for the optimized structures of pyrrole-2-carboxylic acid (PCA) and lithium, sodium, potassium pyrrole-2-carboxylates were also calculated. The degree of perturbation of the aromatic system of ligand under the influence of metals in the Li → Cs series was investigated with the use of statistical methods (linear correlation), calculated aromaticity indices and Mulliken, NBO and ChelpG population analysis method. Additionally, the Bader theory (AIM) was applied to setting the characteristic of the bond critical points what confirmed the influence of alkali metals on the pyrrole ring.

  5. Quantum mechanical study of the structure and spectroscopic (FT-IR, FT-Raman, 13C, 1H and UV), first order hyperpolarizabilities, NBO and TD-DFT analysis of the 4-methyl-2-cyanobiphenyl.

    Science.gov (United States)

    Sebastian, S; Sundaraganesan, N; Karthikeiyan, B; Srinivasan, V

    2011-02-01

    The Fourier transform infrared (FT-IR) and FT-Raman of 4-methyl-2-cyanobiphenyl (4M2CBP) have been recorded and analyzed. The equilibrium geometry, bonding features and harmonic vibrational frequencies have been investigated with the help of density functional theory (DFT) method. The assignments of the vibrational spectra have been carried out with the help of normal coordinate analysis (NCA) following the scaled quantum mechanical force field methodology (SQMFF). The 1H and 13C nuclear magnetic resonance (NMR) chemical shifts of the molecule were calculated by the Gauge including atomic orbital (GIAO) method. The first order hyperpolarizability (β0) of this novel molecular system and related properties (β, α0 and Δα) of 4M2CBP are calculated using HF/6-311G(d,p) method on the finite-field approach. Stability of the molecule arising from hyperconjugative interactions, charge delocalization have been analyzed using natural bond orbital (NBO) analysis. The results show that charge in electron density (ED) in the σ* and π* antibonding orbitals and second order delocalization energies (E2) confirms the occurrence of intramolecular charge transfer (ICT) within the molecule. UV-vis spectrum of the compound was recorded and the electronic properties, such as HOMO and LUMO energies, were performed by time-dependent density functional theory (TD-DFT) approach. Finally the calculations results were applied to simulated infrared and Raman spectra of the title compound which show good agreement with observed spectra. Copyright © 2010 Elsevier B.V. All rights reserved.

  6. Synthesis, molecular structure, FT-IR and XRD investigations of 2-(4-chlorophenyl)-2-oxoethyl 2-chlorobenzoate: a comparative DFT study.

    Science.gov (United States)

    Chidan Kumar, C S; Fun, Hoong Kun; Tursun, Mahir; Ooi, Chin Wei; Chandraju, Siddegowda; Quah, Ching Kheng; Parlak, Cemal

    2014-04-24

    2-(4-Chlorophenyl)-2-oxoethyl 2-chlorobenzoate has been synthesized, its structural and vibrational properties have been reported using FT-IR and single-crystal X-ray diffraction (XRD) studies. The conformational analysis, optimized geometric parameters, normal mode frequencies and corresponding vibrational assignments of the synthesized compound (C15H10Cl2O3) have been examined by means of Becke-3-Lee-Yang-Parr (B3LYP) density functional theory (DFT) method together with 6-31++G(d,p) basis set. Furthermore, reliable conformational investigation and vibrational assignments have been made by the potential energy surface (PES) and potential energy distribution (PED) analyses, respectively. Calculations are performed with two possible conformations. The title compound crystallizes in orthorhombic space group Pbca with the unit cell dimensions a=12.312(5) Å, b=8.103(3) Å, c=27.565(11) Å, V=2750.0(19) Å(3). B3LYP method provides satisfactory evidence for the prediction of vibrational wavenumbers and structural parameters. Copyright © 2014 Elsevier B.V. All rights reserved.

  7. Quantum chemical modeling of new derivatives of (E,E)-azomethines: Synthesis, spectroscopic (FT-IR, UV/Vis, polarization) and thermophysical investigations

    Science.gov (United States)

    Shahab, Siyamak; Sheikhi, Masoome; Filippovich, Liudmila; Anatol'evich, Dikusar Evgenij; Yahyaei, Hooriye

    2017-06-01

    In the present work, the molecular structures of three new azomethine dyes: N-benzylidene-4-((E)-phenyldiazenyl)aniline (PAZB-1), 2-methoxy-4-(((4-((E)- phenyldiazenyl)phenyl)imino)methyl)phenol (PAZB-2) and 2-methoxy-5-((E)-((4-((E)- phenyldiazenyl)phenyl)imino)methyl)phenol (PAZB-8) have been predicted and investigated using Density Functional Theory (DFT) in dimethylformamide (DMF). The geometries of the azomethine dyes were optimized by PBE0/6-31 + G* level of theory. The electronic spectra of these azomethine dyes in a DMF solution was carried out by TDPBE0/6-31 + G* method. After quantum-chemical calculations three new azomethine dyes for optoelectronic applications were synthesized. FT-IR spectra of the title compounds are recorded and discussed. The computed absorption spectral data of the azomethine dyes are in good agreement with the experimental data, thus allowing an assignment of the UV/Vis spectra. On the basis of polyvinyl alcohol (PVA) and the new synthesized azomethine dyes polarizing films for Visible region of spectrum were developed. The main optical parameters of polarizing PVA-films (Transmittance, Polarization Efficiency and Dichroic Ratio) have been measured and discussed. Anisotropy of thermal conductivity of the PVA-films has been studied.

  8. An improved synthesis, spectroscopic (FT-IR, NMR) study and DFT computational analysis (IR, NMR, UV-Vis, MEP diagrams, NBO, NLO, FMO) of the 1,5-methanoazocino[4,3-b]indole core structure

    Science.gov (United States)

    Uludağ, Nesimi; Serdaroğlu, Goncagül

    2018-03-01

    This study examines the synthesis of azocino[4,3-b]indole structure, which constitutes the tetracyclic framework of uleine, dasycarpidoneand tubifolidineas well as ABDE substructure of the strychnosalkaloid family. It has been synthesized by Fischer indolization of 2 and through the cylization of 4 by 2,3-dichlor-5-6-dicyanobenzoquinone (DDQ). 1H and 1C NMR chemical shifts have been predicted with GIAO approach and the calculated chemical shifts show very good agreement with observed shifts. FT-IR spectroscopy is important for the analysis of functional groups of synthesized compounds and we also supported FT-IR vibrational analysis with computational IR analysis. The vibrational spectral analysis was performed at B3LYP level of the theory in both the gas and the water phases and it was compared with the observed IR values for the important functional groups. The DFT calculations have been conducted to determine the most stable structure of the 1,2,3,4,5,6,7-Hexahydro-1,5-methanoazocino [4,3-b] indole (5). The Frontier Molecular Orbital Analysis, quantum chemical parameters, physicochemical properties have been predicted by using the same theory of level in both gas phase and the water phase, at 631 + g** and 6311++g** basis sets. TD- DFT calculations have been performed to predict the UV- Vis spectral analysis for this synthesized molecule. The Natural Bond Orbital (NBO) analysis have been performed at B3LYP level of theory to elucidate the intra-molecular interactions such as electron delocalization and conjugative interactions. NLO calculations were conducted to obtain the electric dipole moment and polarizability of the title compound.

  9. Biochemical applications of FT-IR spectroscopy

    NARCIS (Netherlands)

    Pistorius, A.M.A.

    1996-01-01

    This thesis describes the use of (FT-)IR spectroscopy in general biochemical research. In chapter 3, IR spectroscopy is used in the quantitation of residual detergent after reconstitution of an integral membrane protein in a pre-defined lipid matrix. This chapter discusses the choice of the

  10. Quantitative gas analysis with FT-IR

    DEFF Research Database (Denmark)

    Bak, J.; Larsen, A.

    1995-01-01

    Calibration spectra of CO in the 2.38-5100 ppm concentration range (22 spectra) have been measured with a spectral resolution of 4 cm(-1), in the mid-IR (2186-2001 cm(-1)) region, with a Fourier transform infrared (FT-IR) instrument. The multivariate calibration method partial least-squares (PLS1...

  11. Collaborative Student Laboratory Exercise Using FT-IR Spectroscopy for the Kinetics Study of a Biotin Analogue

    Science.gov (United States)

    Leong, Jhaque; Ackroyd, Nathan C.; Ho, Karen

    2014-01-01

    The synthesis of N-methoxycarbonyl-2-imidazolidone, an analogue of biotin, was conducted by organic chemistry students and confirmed using FT-IR and H NMR. Spectroscopy students used FT-IR to measure the rate of hydrolysis of the product and determined the rate constant for the reaction using the integrated rate law. From the magnitude of the rate…

  12. Vibrational investigation on FT-IR and FT-Raman spectra, IR intensity, Raman activity, peak resemblance, ideal estimation, standard deviation of computed frequencies analyses and electronic structure on 3-methyl-1,2-butadiene using HF and DFT (LSDA/B3LYP/B3PW91) calculations.

    Science.gov (United States)

    Ramalingam, S; Jayaprakash, A; Mohan, S; Karabacak, M

    2011-11-01

    FT-IR and FT-Raman (4000-100 cm(-1)) spectral measurements of 3-methyl-1,2-butadiene (3M12B) have been attempted in the present work. Ab-initio HF and DFT (LSDA/B3LYP/B3PW91) calculations have been performed giving energies, optimized structures, harmonic vibrational frequencies, IR intensities and Raman activities. Complete vibrational assignments on the observed spectra are made with vibrational frequencies obtained by HF and DFT (LSDA/B3LYP/B3PW91) at 6-31G(d,p) and 6-311G(d,p) basis sets. The results of the calculations have been used to simulate IR and Raman spectra for the molecule that showed good agreement with the observed spectra. The potential energy distribution (PED) corresponding to each of the observed frequencies are calculated which confirms the reliability and precision of the assignment and analysis of the vibrational fundamentals modes. The oscillation of vibrational frequencies of butadiene due to the couple of methyl group is also discussed. A study on the electronic properties such as HOMO and LUMO energies, were performed by time-dependent DFT (TD-DFT) approach. The calculated HOMO and LUMO energies show that charge transfer occurs within the molecule. The thermodynamic properties of the title compound at different temperatures reveal the correlations between standard heat capacities (C) standard entropies (S), and standard enthalpy changes (H). Crown Copyright © 2011. Published by Elsevier B.V. All rights reserved.

  13. Synthesis, X-ray diffraction method, spectroscopic characterization (FT-IR, 1H and 13C NMR), antimicrobial activity, Hirshfeld surface analysis and DFT computations of novel sulfonamide derivatives

    Science.gov (United States)

    Demircioğlu, Zeynep; Özdemir, Fethi Ahmet; Dayan, Osman; Şerbetçi, Zafer; Özdemir, Namık

    2018-06-01

    Synthesized compounds of N-(2-aminophenyl)benzenesulfonamide 1 and (Z)-N-(2-((2-nitrobenzylidene)amino)phenyl)benzenesulfonamide 2 were characterized by antimicrobial activity, FT-IR, 1H and 13C NMR. Two new Schiff base ligands containing aromatic sulfonamide fragment of (Z)-N-(2-((3-nitrobenzylidene)amino)phenyl)benzenesulfonamide 3 and (Z)-N-(2-((4-nitrobenzylidene)amino)phenyl)benzenesulfonamide 4 were synthesized and investigated by spectroscopic techniques including 1H and 13C NMR, FT-IR, single crystal X-ray diffraction, Hirshfeld surface, theoretical method analyses and by antimicrobial activity. The molecular geometry obtained from the X-ray structure determination was optimized Density Functional Theory (DFT/B3LYP) method with the 6-311++G(d,p) basis set in ground state. From the optimized geometry of the molecules of 3 and 4, the geometric parameters, vibrational wavenumbers and chemical shifts were computed. The optimized geometry results, which were well represented the X-ray data, were shown that the chosen of DFT/B3LYP 6-311G++(d,p) was a successful choice. After a successful optimization, frontier molecular orbitals, chemical activity, non-linear optical properties (NLO), molecular electrostatic mep (MEP), Mulliken population method, natural population analysis (NPA) and natural bond orbital analysis (NBO), which cannot be obtained experimentally, were calculated and investigated.

  14. Characterization of Momordica charantia Ussing FT-IR Spectroscopy

    Directory of Open Access Journals (Sweden)

    Attila Keseru

    2016-11-01

    In this paper, because earlier claim shows that the plant used as stomachic, carminative, tonic, antipyretic, antidiabetic, in rheumatoid arthritis and gout, the present investigation was carried to characterized a principal components of plant using FT-IR technique

  15. Study of the Pyrrol/Diphenylamine Copolymer by FT-IR spectroscopy and conductivity

    Directory of Open Access Journals (Sweden)

    Carlos Alberto Perez

    2004-01-01

    Full Text Available The main goal of this study was to analyze the physical properties of the copolymer formed by the electrochemical deposition of the polydiphenylamine (PDPA on polypyrrole (Ppy and Ppy on PDPA, in different conditions, through the characterization of the materials formed by the resonant Raman, FT-IR and conductivity techniques. The interactions among the species which are present in the new copolymer structure and the changes in electronic conductivity, were verified. The copolymer was also synthesized electrochemically in the presence of iodide species and the material was characterized by FT-IR spectroscopy and conductivity. The role of the dopant was studied in the process of charge transfer between the copolymer-dopant, acting in the stabilization of the species in the polymer backbone and the increase of the electronic conductivity.

  16. FT-IR, FT-Raman spectra and ab initio HF and DFT calculations of 7-chloro-5-(2-chlorophenyl)-3-hydroxy-2,3-dihydro-1H-1,4-benzodiazepin-2-one.

    Science.gov (United States)

    Muthu, S; Prasath, M; Paulraj, E Isac; Balaji, R Arun

    2014-01-01

    The Fourier Transform infrared and Fourier Transform Raman spectra of 7-chloro-5 (2-chlorophenyl)-3-hydroxy-2,3-dihydro-1H-1,4-benzodiazepin-2-one (7C3D4B) were recorded in the regions 4000-400 and 4000-100 cm(-1), respectively. The appropriate theoretical spectrograms for the IR and Raman spectra of the title molecule were also constructed. The calculated results show that the predicted geometry can well reproduce the structural parameters. Predicted vibrational frequencies have been assigned and compared with experimental IR spectra and they supported each other. Stability of the molecule arising from hyperconjugative interactions, charge delocalization and intramolecular hydrogen bond-like weak interaction has been analyzed using natural bond orbital (NBO) analysis by using B3LYP/6-31G(d,p) method. The results show that electron density (ED) in the σ* and π* antibonding orbitals and second-order delocalization energies E(2) confirm the occurrence of intramolecular charge transfer (ICT) within the molecule. The first order hyperpolarizability (βtotal) of this molecular system and related properties (β, μ, and Δα) are calculated using HF/6-31G(d,p) and B3LYP/6-31G(d,p) methods based on the finite-field approach. Copyright © 2013 Elsevier B.V. All rights reserved.

  17. FT-IR and FT-Raman spectra of 5-chlorocytosine: Solid state simulation and tautomerism. Effect of the chlorine substitution in the Watson-Crick base pair 5-chlorodeoxycytidine-deoxyguanosine

    Science.gov (United States)

    Alcolea Palafox, M.; Rastogi, V. K.; Singh, S. P.

    2018-01-01

    The laser Raman and IR spectra of 5-chlorocytosine have been recorded and accurately assigned in the solid state using Density functional calculations (DFT) together with the linear scaling equation procedure (LSE) and the solid state simulation of the crystal unit cell through a tetramer form. These results remarkably improve those reported previously by other authors. Several new scaling equations were proposed to be used in related molecules. The six main tautomers of the biomolecule 5-chlorocytosine were determined and optimized at the MP2 and CCSD levels, using different basis sets. The relative stabilities were compared with those obtained in cytosine and their 5-halo derivatives. Several relationships between energies, geometric parameters and NBO atomic charges were established. The effect of the chlorine substitution in the fifth position was evaluated through the stability of the Watson-Crick (WC) base pair of 5-chlorodeoxycytidine with deoxyguanosine, and through their vibrational spectra.

  18. Analysis of the structure and the FT-IR and Raman spectra of 2-(4-nitrophenyl)-4H-3,1-benzoxazin-4-one. Comparisons with the chlorinated and methylated derivatives

    Science.gov (United States)

    Castillo, María V.; Rudyk, Roxana A.; Davies, Lilian; Brandán, Silvia Antonia

    2017-07-01

    In this work, the structural, topological and vibrational properties of the monomer and three dimers of the 2-(4-nitrophenyl)-4H-3,1-benzoxazin-4-one (NPB) derivative were studied combining the experimental FTIR and FT-Raman spectra in the solid phase with DFT calculations. Here, Natural Bond Orbital (NBO), Atoms in Molecules (AIM) and HOMO and LUMO calculations were performed by using the hybrid B3LYP/6-31G*and B3LYP/6-311++G** methods in order to compute those properties and to predict their reactivities. The comparisons with the properties reported for the chlorinated (Cl-PB) and methylated (CH3-PB) derivatives at the same levels of theory can be clearly justified by the activating (CH3) and deactivating (NO2 and Cl) characteristics of the different groups linked to oxaxin rings. The NBO and AIM studies evidence the following stability orders: Cl-PB > NO2-PB > CH3-PB in very good concordance with the f(νC23-X26) force constants values. The frontier orbitals analyses reveal that the Cl-PB and NO2-PB derivatives have good stabilities and high chemical hardness while CH3-PB has a higher chemical reactivity. On the other hand, the complete vibrational assignments for monomer and dimers species of NPB were presented. The presence of the IR bands at 1574 and 1037 cm-1 and, of the Raman bands at 1571 and 1038 cm-1 support clearly the presence of the different dimeric species proposed for NPB.

  19. Use of FT-IR, FT-Raman and thermal analysis to evaluate the gel formation of curdlan produced by Agrobacterium sp. IFO 13140 and determination of its rheological properties with food applicability.

    Science.gov (United States)

    Mangolim, Camila Sampaio; da Silva, Thamara Thaiane; Fenelon, Vanderson Carvalho; do Nascimento, Adriane; Sato, Francielle; Matioli, Graciette

    2017-10-01

    Curdlan is a linear polysaccharide composed of glucose units joined by β-(1,3) bonds that possesses unique gelation properties. This study aimed to characterize the structure and evaluate the gelling properties of curdlan produced by Agrobacterium sp. IFO 13140 and its gels, as well as apply it in food. FT-Raman analysis highlighted the structural changes that occurred during the formation of gels, with variations related to the hydrogen bonds and hydrophobic interactions, which occur with the formation of the low-set and high-set gels, respectively. Rheological analysis showed that the pre-gelled commercial curdlan and the curdlan produced by Agrobacterium sp. IFO 13140 differed in terms of gelation properties, which depends of the degree of polymerization of the polysaccharide, but when applied to pasta products, both improved the texture parameters. The curdlan gels were found to have great potential as gelling agents to improve texture, water retention capacity and stability of food products. Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. FT-IR, FT-Raman, NMR spectra, density functional computations of the vibrational assignments (for monomer and dimer) and molecular geometry of anticancer drug 7-amino-2-methylchromone

    Science.gov (United States)

    Mariappan, G.; Sundaraganesan, N.

    2014-04-01

    Vibrational assignments for the 7-amino-2-methylchromone (abbreviated as 7A2MC) molecule using a combination of experimental vibrational spectroscopic measurements and ab initio computational methods are reported. The optimized geometry, intermolecular hydrogen bonding, first order hyperpolarizability and harmonic vibrational wavenumbers of 7A2MC have been investigated with the help of B3LYP density functional theory method. The calculated molecular geometry parameters, the theoretically computed vibrational frequencies for monomer and dimer and relative peak intensities were compared with experimental data. DFT calculations using the B3LYP method and 6-31 + G(d,p) basis set were found to yield results that are very comparable to experimental IR and Raman spectra. Detailed vibrational assignments were performed with DFT calculations and the potential energy distribution (PED) obtained from the Vibrational Energy Distribution Analysis (VEDA) program. Natural Bond Orbital (NBO) study revealed the characteristics of the electronic delocalization of the molecular structure. 13C and 1H NMR spectra have been recorded and 13C and 1H nuclear magnetic resonance chemical shifts of the molecule have been calculated using the gauge independent atomic orbital (GIAO) method. Furthermore, All the possible calculated values are analyzed using correlation coefficients linear fitting equation and are shown strong correlation with the experimental data.

  1. Spectroscopic (FT-IR, FT-Raman, UV, 1H and 13C NMR insights, electronic profiling and DFT computations on ({(E-[3-(1H-imidazol-1-yl-1-phenylpropylidene] amino}oxy(4-nitrophenylmethanone, an imidazole-bearing anti-Candida agent

    Directory of Open Access Journals (Sweden)

    Al-Wahaibi Lamya H.

    2018-02-01

    Full Text Available The anti-Candida agent, ({(E-[3-(1H-imidazol-1-yl-1-phenylpropylidene]amnio}oxy(4-nitropheny methanone (IPAONM, was subjected to comprehensive spectroscopic (FT-IR, FT-Raman, UV–Vis 1H and 13C NMR characterization as well as Hartree Fock and density functional theory computation studies. The selected optimized geometric bond lengths and bond angles of the IPAONM molecule were compared with the experimental values. The calculated wavenumbers have been scaled and compared with the experimental spectra. Mulliken charges and natural bond orbital analysis of the title molecule were calculated and interpreted. The energy and oscillator strengths of the IPAONM molecule were calculated by time-dependent density functional theory (TD-DFT. In addition, frontier molecular orbitals and molecular electrostatic potential diagram of the title compound were computed and analyzed. A study on the electronic properties, such as HOMO, HOMO-1, LUMO and LUMO+1 energies was carried out using TD-DFT approach. The 1H and 13C NMR chemical shift values of the title compound were calculated by the gauge independent atomic orbital method and compared with the experimental results.

  2. Design of geometry, synthesis, spectroscopic (FT-IR, UV/Vis, excited state, polarization) and anisotropy (thermal conductivity and electrical) properties of new synthesized derivatives of (E,E)-azomethines in colored stretched poly (vinyl alcohol) matrix

    Science.gov (United States)

    Shahab, Siyamak; Sheikhi, Masoome; Filippovich, Liudmila; Dikusar, Evgenij; Yahyaei, Hooriye; Kumar, Rakesh; Khaleghian, Mehrnoosh

    2018-04-01

    In the present work, the molecular structures of two new azomethine dyes: have been predicted and investigated using Density Functional Theory (DFT) in dimethylformamide (DMF). The geometries of the azomethine dyes were optimized by B3LYP/6-31+G* level of theory. The electronic spectra of these azomethine dyes in a DMF solvent was carried out by using TD-B3LYP/6-31+G* method. After quantum-chemical calculations two new azomethine dyes for optoelectronic applications were synthesized. FT-IR spectra of the title compounds are recorded and discussed. The computed absorption spectral data of the azomethine dyes are in good agreement with the experimental data, thus allowing an assignment of the UV/Vis spectra. On the basis of polyvinyl alcohol (PVA) and the new synthesized azomethine dyes polarizing films for visible region of spectrum were developed. The main optical parameters of the polarizing PVA-films (Transmittance, Polarization Efficiency and Dichroic Ratio) have been measured and discussed. Anisotropy of thermal and electrical conductivity of the PVA-films have been studied and explained.

  3. Synthesis, single crystal X-ray, spectroscopic (FT-IR, UV-vis, fluorescence, 1H &13C NMR), computational (DFT/B3LYP) studies of some imidazole based picrates

    Science.gov (United States)

    Arockia doss, M.; Rajarajan, G.; Thanikachalam, V.; Selvanayagam, S.; Sridhar, B.

    2018-04-01

    2,4,5-triphenyl-1H-imidazol-3-ium picrate (1), 2-(4-fluorophenyl)-4,5-diphenyl-1H-imidazol-3-ium picrate (2), 2-(4-methylphenyl)-4,5-diphenyl-1H-imidazol-3-ium picrate (3) were synthesised. These compounds 1-3 were characterized by elemental, FT-IR, 1H NMR and 13C NMR analyses. The structure of compound 3 was further confirmed by single crystal X-ray diffraction. The studies reveal that the molecule is associated with weak Nsbnd H⋯O and Csbnd H⋯N and van der Waals interactions which are responsible for the formation and strengthening of supramolecular assembly. The nature of the interactions and their importance are explored using the Hirshfeld surface method. The physicochemical properties of the compounds 1-3 were evaluated by UV-vis spectroscopy, fluorescence spectroscopy, and thermogravimetric analysis. According to thermal data the salts possess excellent thermal stabilities with decomposition temperatures ranging from 220 to 280 °C. Second-harmonic generation (SHG) results exposed that the picrates 1-3 were about 1.13-1.50 times greater than potassium dihydrogen phosphate (KDP). Here we also used Density functional theory (DFT) calculations in order to investigate the opto-electronic properties. The obtained theoretical results validate with available experimental data.

  4. Application of FT-IR Classification Method in Silica-Plant Extracts Composites Quality Testing

    Science.gov (United States)

    Bicu, A.; Drumea, V.; Mihaiescu, D. E.; Purcareanu, B.; Florea, M. A.; Trică, B.; Vasilievici, G.; Draga, S.; Buse, E.; Olariu, L.

    2018-06-01

    Our present work is concerned with the validation and quality testing efforts of mesoporous silica - plant extracts composites, in order to sustain the standardization process of plant-based pharmaceutical products. The synthesis of the silica support were performed by using a TEOS based synthetic route and CTAB as a template, at room temperature and normal pressure. The silica support was analyzed by advanced characterization methods (SEM, TEM, BET, DLS and FT-IR), and loaded with Calendula officinalis and Salvia officinalis standardized extracts. Further desorption studies were performed in order to prove the sustained release properties of the final materials. Intermediate and final product identification was performed by a FT-IR classification method, using the MID-range of the IR spectra, and statistical representative samples from repetitive synthetic stages. The obtained results recommend this analytical method as a fast and cost effective alternative to the classic identification methods.

  5. Vibrational spectroscopic (FT-IR, FT-Raman) and quantum mechanical study of 4-(2-chlorophenyl)-2-ethyl-9-methyl-6H-thieno[3,2-f] [1,2,4]triazolo[4,3-a][1,4] diazepine

    Science.gov (United States)

    Kuruvilla, Tintu K.; Prasana, Johanan Christian; Muthu, S.; George, Jacob

    2018-04-01

    The spectroscopic properties of 4-(2-chlorophenyl)-2-ethyl-9-methyl-6H-thieno [3,2-f] [1,2,4] triazolo [4,3-a] [1,4] diazepine were investigated in the present study using FT-IR and FT-Raman techniques. The results obtained were compared with quantum mechanical methods, as it serves as an important tool in interpreting and predicting vibrational spectra. The optimized molecular geometry, the vibrational wavenumbers, the infrared intensities and Raman scattering were calculated using density functional theory B3LYP method with 6-311++g (d,p) basis set. All the experimental results were in line with the theoretical data. The molecular electrostatic potential (MEP) and HOMO LUMO energies of the title compound were accounted. The results indicated that the title compound has a lower softness value (0.27) and high electrophilicity index (4.98) hence describing its biological activity. Further, natural bond orbital was also analyzed as part of the work. Fukui functions were calculated in order to explain the chemical selectivity or the reactivity site in 4-(2-chlorophenyl)-2-ethyl-9-methyl-6H-thieno [3,2-f] [1,2,4] triazolo [4,3-a] [1,4] diazepine. The thermodynamic properties of the title compound were closely examined at different temperatures. It revealed the correlations between heat capacity (C), entropy (S) and enthalpy changes (H) with temperatures. The paper further explains that the title compound can act as good antidepressant through molecular docking studies.

  6. FT-IR Microspectroscopy of Rat Ear Cartilage.

    Directory of Open Access Journals (Sweden)

    Benedicto de Campos Vidal

    Full Text Available Rat ear cartilage was studied using Fourier transform-infrared (FT-IR microspectroscopy to expand the current knowledge which has been established for relatively more complex cartilage types. Comparison of the FT-IR spectra of the ear cartilage extracellular matrix (ECM with published data on articular cartilage, collagen II and 4-chondroitin-sulfate standards, as well as of collagen type I-containing dermal collagen bundles (CBs with collagen type II, was performed. Ear cartilage ECM glycosaminoglycans (GAGs were revealed histochemically and as a reduction in ECM FT-IR spectral band heights (1140-820 cm-1 after testicular hyaluronidase digestion. Although ear cartilage is less complex than articular cartilage, it contains ECM components with a macromolecular orientation as revealed using polarization microscopy. Collagen type II and GAGs, which play a structural role in the stereo-arrangement of the ear cartilage, contribute to its FT-IR spectrum. Similar to articular cartilage, ear cartilage showed that proteoglycans add a contribution to the collagen amide I spectral region, a finding that does not recommend this region for collagen type II quantification purposes. In contrast to articular cartilage, the symmetric stretching vibration of -SO3- groups at 1064 cm-1 appeared under-represented in the FT-IR spectral profile of ear cartilage. Because the band corresponding to the asymmetric stretching vibration of -SO3- groups (1236-1225 cm-1 overlapped with that of amide III bands, it is not recommended for evaluation of the -SO3- contribution to the FT-IR spectrum of the ear cartilage ECM. Instead, a peak (or shoulder at 1027-1016 cm-1 could be better considered for this intent. Amide I/amide II ratios as calculated here and data from the literature suggest that protein complexes of the ear cartilage ECM are arranged with a lower helical conformation compared to pure collagen II. The present results could motivate further studies on this tissue

  7. Applications of FT-IR spectrophotometry in cancer diagnostics.

    Science.gov (United States)

    Bunaciu, Andrei A; Hoang, Vu Dang; Aboul-Enein, Hassan Y

    2015-01-01

    This review provides a brief background to the application of infrared spectroscopy, including Fourier transform-infrared spectroscopy, in biological fluids. It is not meant to be complete or exhaustive but to provide the reader with sufficient background for selected applications in cancer diagnostics. Fourier transform-infrared spectroscopy (FT-IR) is a fast and nondestructive analytical method. The infrared spectrum of a mixture serves as the basis to quantitate its constituents, and a number of common clinical chemistry tests have proven to be feasible using this approach. This review focuses on biomedical FT-IR applications, published in the period 2009-2013, used for early detection of cancer through qualitative and quantitative analysis.

  8. FT-IR spectroscopy of lipoproteins—A comparative study

    Science.gov (United States)

    Krilov, Dubravka; Balarin, Maja; Kosović, Marin; Gamulin, Ozren; Brnjas-Kraljević, Jasminka

    2009-08-01

    FT-IR spectra, in the frequency region 4000-600 cm -1, of four major lipoprotein classes: very low density lipoprotein (VLDL), low density lipoprotein (LDL) and two subclasses of high density lipoproteins (HDL 2 and HDL 3) were analyzed to obtain their detailed spectral characterization. Information about the protein domain of particle was obtained from the analysis of amide I band. The procedure of decomposition and curve fitting of this band confirms the data already known about the secondary structure of two different apolipoproteins: apo A-I in HDL 2 and HDL 3 and apo B-100 in LDL and VLDL. For information about the lipid composition and packing of the particular lipoprotein the well expressed lipid bands in the spectra were analyzed. Characterization of spectral details in the FT-IR spectrum of natural lipoprotein is necessary to study the influence of external compounds on its structure.

  9. Laser Spark Formamide Decomposition Studied by FT-IR Spectroscopy

    Czech Academy of Sciences Publication Activity Database

    Ferus, Martin; Kubelík, Petr; Civiš, Svatopluk

    2011-01-01

    Roč. 115, č. 44 (2011), s. 12132-12141 ISSN 1089-5639 R&D Projects: GA AV ČR IAA400400705; GA AV ČR IAAX00100903; GA ČR GAP208/10/2302 Institutional research plan: CEZ:AV0Z40400503 Keywords : FT-IR spectroscopy * high-power laser * induced dielectric-breakdown Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.946, year: 2011

  10. Completely automated open-path FT-IR spectrometry.

    Science.gov (United States)

    Griffiths, Peter R; Shao, Limin; Leytem, April B

    2009-01-01

    Atmospheric analysis by open-path Fourier-transform infrared (OP/FT-IR) spectrometry has been possible for over two decades but has not been widely used because of the limitations of the software of commercial instruments. In this paper, we describe the current state-of-the-art of the hardware and software that constitutes a contemporary OP/FT-IR spectrometer. We then describe advances that have been made in our laboratory that have enabled many of the limitations of this type of instrument to be overcome. These include not having to acquire a single-beam background spectrum that compensates for absorption features in the spectra of atmospheric water vapor and carbon dioxide. Instead, an easily measured "short path-length" background spectrum is used for calculation of each absorbance spectrum that is measured over a long path-length. To accomplish this goal, the algorithm used to calculate the concentrations of trace atmospheric molecules was changed from classical least-squares regression (CLS) to partial least-squares regression (PLS). For calibration, OP/FT-IR spectra are measured in pristine air over a wide variety of path-lengths, temperatures, and humidities, ratioed against a short-path background, and converted to absorbance; the reference spectrum of each analyte is then multiplied by randomly selected coefficients and added to these background spectra. Automatic baseline correction for small molecules with resolved rotational fine structure, such as ammonia and methane, is effected using wavelet transforms. A novel method of correcting for the effect of the nonlinear response of mercury cadmium telluride detectors is also incorporated. Finally, target factor analysis may be used to detect the onset of a given pollutant when its concentration exceeds a certain threshold. In this way, the concentration of atmospheric species has been obtained from OP/FT-IR spectra measured at intervals of 1 min over a period of many hours with no operator intervention.

  11. Characterization and identification of microorganisms by FT-IR microspectrometry

    Science.gov (United States)

    Ngo-Thi, N. A.; Kirschner, C.; Naumann, D.

    2003-12-01

    We report on a novel FT-IR approach for microbial characterization/identification based on a light microscope coupled to an infrared spectrometer which offers the possibility to acquire IR-spectra of microcolonies containing only few hundred cells. Microcolony samples suitable for FT-IR microspectroscopic measurements were obtained by a replica technique with a stamping device that transfers spatially accurate cells of microcolonies growing on solid culture plates to a special, IR-transparent or reflecting stamping plate. High quality spectra could be recorded either by applying the transmission/absorbance or the reflectance/absorbance mode of the infrared microscope. Signal to noise ratios higher than 1000 were obtained for microcolonies as small as 40 μm in diameter. Reproducibility levels were established that allowed species and strain identification. The differentiation and classification capacity of the FT-IR microscopic technique was tested for different selected microorganisms. Cluster and factor analysis methods were used to evaluate the complex spectral data. Excellent discrimination between bacteria and yeasts, and at the same time Gram-negative and Gram-positive bacterial strains was obtained. Twenty-two selected strains of different species within the genus Staphylococcus were repetitively measured and could be grouped into correct species cluster. Moreover, the results indicated that the method allows also identifications at the subspecies level. Additionally, the new approach allowed spectral mapping analysis of single colonies which provided spatially resolved characterization of growth heterogeneity within complex microbial populations such as colonies.

  12. Differentiation of Leishmania species by FT-IR spectroscopy

    Science.gov (United States)

    Aguiar, Josafá C.; Mittmann, Josane; Ferreira, Isabelle; Ferreira-Strixino, Juliana; Raniero, Leandro

    2015-05-01

    Leishmaniasis is a parasitic infectious disease caused by protozoa that belong to the genus Leishmania. It is transmitted by the bite of an infected female Sand fly. The disease is endemic in 88 countries Desjeux (2001) [1] (16 developed countries and 72 developing countries) on four continents. In Brazil, epidemiological data show the disease is present in all Brazilian regions, with the highest incidences in the North and Northeast. There are several methods used to diagnose leishmaniasis, but these procedures have many limitations, are time consuming, have low sensitivity, and are expensive. In this context, Fourier Transform Infrared Spectroscopy (FT-IR) analysis has the potential to provide rapid results and may be adapted for a clinical test with high sensitivity and specificity. In this work, FT-IR was used as a tool to investigate the promastigotes of Leishmaniaamazonensis, Leishmaniachagasi, and Leishmaniamajor species. The spectra were analyzed by cluster analysis and deconvolution procedure base on spectra second derivatives. Results: cluster analysis found four specific regions that are able to identify the Leishmania species. The dendrogram representation clearly indicates the heterogeneity among Leishmania species. The band deconvolution done by the curve fitting in these regions quantitatively differentiated the polysaccharides, amide III, phospholipids, proteins, and nucleic acids. L. chagasi and L. major showed a greater biochemistry similarity and have three bands that were not registered in L. amazonensis. The L. amazonensis presented three specific bands that were not recorded in the other two species. It is evident that the FT-IR method is an indispensable tool to discriminate these parasites. The high sensitivity and specificity of this technique opens up the possibilities for further studies about characterization of other microorganisms.

  13. Hydrogenated fullerenes in space: FT-IR spectra analysis

    International Nuclear Information System (INIS)

    El-Barbary, A. A.

    2016-01-01

    Fullerenes and hydrogenated fullerenes are found in circumstellar and interstellar environments. But the determination structures for the detected bands in the interstellar and circumstellar space are not completely understood so far. For that purpose, the aim of this article is to provide all possible infrared spectra for C 20 and C 60 fullerenes and their hydrogenated fullerenes. Density Functional theory (DFT) is applied using B3LYP exchange-functional with basis set 6–31G(d, p). The Fourier transform infrared spectroscopy (FT-IR) is found to be capable of distinguishing between fullerenes, mono hydrogenated fullerenes and fully hydrogenated fullerenes. In addition, deposition of one hydrogen atom outside the fully hydrogenated fullerenes is found to be distinguished by forming H 2 molecule at peak around 4440 cm −1 . However, deposition of one hydrogen atom inside the fully hydrogenated fullerenes cannot be distinguished. The obtained spectral structures are analyzed and are compared with available experimental results.

  14. Study of the deuterated albumin by FT-IR spectroscopy

    International Nuclear Information System (INIS)

    Stoenescu, Daniela; Sahini, V.E.

    2000-01-01

    The albumin is a protein from the soluble or corpuscular protein class, which exists in cells, in dissolved state or in form of a hydrated gel. Proteins are essential constituents beside water, inorganic salts, lipids, carbon hydrates, vitamins, enzymes. The albumin is also a protein soluble in water and in diluted electrolyte solutions (acids, bases and salts). The investigation of the vibration isotopic effect has a great importance both for the diatomic molecules and for the polyatomic molecules. This paper is the first from a series of works which are intended to study the physico-chemical properties of the deuterated albumin and of the albumin solutions in heavy water by an isotopic exchange method. To put in evidence H-D exchange, the FT-IR spectroscopy is used when the deuterated albumin has different layer thickness. It is also of interest to elucidate the isotopic exchange between the hydrogen and oxygen atoms in bovine serum albumin macromolecules. (authors)

  15. Hydrogenated fullerenes in space: FT-IR spectra analysis

    Energy Technology Data Exchange (ETDEWEB)

    El-Barbary, A. A. [Physics Department, Faculty of Education, Ain-Shams University, Cairo, Egypt Physics Department, Faculty of Science, Jazan University, Jazan (Saudi Arabia)

    2016-06-10

    Fullerenes and hydrogenated fullerenes are found in circumstellar and interstellar environments. But the determination structures for the detected bands in the interstellar and circumstellar space are not completely understood so far. For that purpose, the aim of this article is to provide all possible infrared spectra for C{sub 20} and C{sub 60} fullerenes and their hydrogenated fullerenes. Density Functional theory (DFT) is applied using B3LYP exchange-functional with basis set 6–31G(d, p). The Fourier transform infrared spectroscopy (FT-IR) is found to be capable of distinguishing between fullerenes, mono hydrogenated fullerenes and fully hydrogenated fullerenes. In addition, deposition of one hydrogen atom outside the fully hydrogenated fullerenes is found to be distinguished by forming H{sub 2} molecule at peak around 4440 cm{sup −1}. However, deposition of one hydrogen atom inside the fully hydrogenated fullerenes cannot be distinguished. The obtained spectral structures are analyzed and are compared with available experimental results.

  16. Characterization of additives typically employed in EPDM formulations by using FT-IR of gaseous pyrolyzates

    Directory of Open Access Journals (Sweden)

    Natália Beck Sanches

    2014-06-01

    Full Text Available In this study, Fourier transform infrared spectroscopy (FT-IR was employed to investigate the gaseous pyrolysis products of ethylene - propylene - diene rubber (EPDM. The objective was to evaluate the potential of FT-IR analysis of gaseous pyrolyzates (PY-G/FT-IR for characterization of EPDM additives. Two EPDM formulations, containing additives typically employed in EPDM rubbers, were analyzed. Initially, gaseous pyrolysis products from paraffin oil, stearic acid, 2,2,4-trimethyl-1,2-dihydroquinoline, tetramethylthiuram monosulfide (TMTM, tetramethylthiuram disulfide (TMTD, and 2-mercaptobenzothiazole (MBT were characterized separately, and their main absorptions were identified. Subsequently, the gaseous pyrolysis products of raw, unvulcanized, and vulcanized EPDM formulations were analyzed. The similarities observed in the FT-IR spectra of unvulcanized and vulcanized EPDM show that the vulcanization process does not interfere with the pyrolysis products. The identification of the functional groups of the studied additives was possible in both unvulcanized and vulcanized EPDM samples, without solvent extraction. Results also demonstrate that the PY-G/FT-IR technique can identify additives containing sulfur in concentrations as low as 1.4 phr (1.26% in both unvulcanized and vulcanized EPDM. However, the method showed some limitation due to overlapping and to similarities of TMTM and TMTD PY-G/FT-IR spectra, which could not be distinguished from each other. The PY-G/FT-IR technique is a faster and cheaper alternative to the sophisticated techniques usually applied to detection of additives in rubbers.

  17. Intramolecular hydrogen bonding in N-salicylideneaniline: FT-IR spectrum and quantum chemical calculations

    Science.gov (United States)

    Moosavi-Tekyeh, Zainab; Dastani, Najmeh

    2015-12-01

    FT-IR and FT-Raman spectra of N-salicylideneaniline (SAn) and its deuterated analogue (D-SAn) are recorded, and the theoretical calculations are performed on their molecular structures and vibrational frequencies. The same calculations are performed for SAn in different solutions using the polarizable conductor continuum model (CPCM) method. Comparisons between the spectra obtained and the corresponding theoretical calculations are used to assign the vibrational frequencies for these compounds. The spectral behavior of SAn upon deuteration is also used to distinguish the positions of OH vibrational frequencies. The hydrogen bond strength of SAn is investigated by applying the atoms-in-molecules (AIM) theory, natural bond orbital (NBO) analysis, and geometry calculations. The harmonic vibrational frequencies of SAn are calculated at B3LYP and X3LYP levels of theory using 6-31G*, 6-311G**, and 6-311++G** basis sets. The AIM results support a medium hydrogen bonding in SAn. The observed νOH/νOD and γOH/γOD for SAn appear at 2940/2122 and 830/589 cm-1, respectively.

  18. TG/FT-IR characterization of additives typically employed in EPDM formulations

    Directory of Open Access Journals (Sweden)

    Natália Beck Sanches

    2015-06-01

    Full Text Available AbstractThermogravimetric analysis coupled to Fourier transform infrared spectroscopy (TG/FT-IR is a very popular technique for rubbers characterization. It involves analyses of the base polymer and additives. Ethylene–propylene–diene (EPDM rubbers are frequently investigated by TG/FT-IR; however, the focus has been the degradation temperature range of the polymer. In this study, unvulcanized and vulcanized EPDM rubber and its additives were investigated by TG/FT-IR, without solvent extraction, and in a wide temperature range. Initially, the additives were individually characterized. TG/FT-IR identified the characteristic groups of all the additives analyzed and distinguished them from each other. Afterwards, unvulcanized and vulcanized EPDM rubbers were investigated without prior extraction.TG/FT-IR detected absorptions due to the additives tetramethylthiuram monosulfide and 2-mercaptobenzothiazole. Both of these sulfur-containing additives were present in the EPDM formulation at concentrations of 0.7 phr (0.63 wt %. The TG/FT-IR technique had some limitations, because not all the additives in EPDM rubber were detected. Paraffin oil, stearic acid and 2,2,4-trimethyl-1,2-dihydroquinoline functional groups were not observed in either the unvulcanized or vulcanized EPDM. Nevertheless, in addition to the ability of this method to detect sulfur-containing groups, the lack of a pre-extraction reduces the time and effort required for additive analysis in rubbers.

  19. Application of Fourier transform infrared (FT-IR) spectroscopy in determination of microalgal compositions.

    Science.gov (United States)

    Meng, Yingying; Yao, Changhong; Xue, Song; Yang, Haibo

    2014-01-01

    Fourier transform infrared spectroscopy (FT-IR) was applied in algal strain screening and monitoring cell composition dynamics in a marine microalga Isochrysis zhangjiangensis during algal cultivation. The content of lipid, carbohydrate and protein of samples determined by traditional methods had validated the accuracy of FT-IR method. For algal screening, the band absorption ratios of lipid/amide I and carbo/amide I from FT-IR measurements allowed for the selection of Isochrysis sp. and Tetraselmis subcordiformis as the most potential lipid and carbohydrate producers, respectively. The cell composition dynamics of I. zhangjiangensis measured by FT-IR revealed the diversion of carbon allocation from protein to carbohydrate and neutral lipid when nitrogen-replete cells were subjected to nitrogen limitation. The carbo/amide I band absorption ratio had also been demonstrated to depict physiological status under nutrient stress in T. subcordiformis. FT-IR serves as a tool for the simultaneous measurement of lipid, carbohydrate, and protein content in cell. Copyright © 2013 Elsevier Ltd. All rights reserved.

  20. FT-IR spectrum of grape seed oil and quantum models of fatty acids triglycerides

    Science.gov (United States)

    Berezin, K. V.; Antonova, E. M.; Shagautdinova, I. T.; Chernavina, M. L.; Dvoretskiy, K. N.; Grechukhina, O. N.; Vasilyeva, L. M.; Rybakov, A. V.; Likhter, A. M.

    2018-04-01

    FT-IR spectra of grape seed oil and glycerol were registered in the 650-4000 cm-1 range. Molecular models of glycerol and some fatty acids that compose the oil under study - linoleic, oleic, palmitic and stearic acids - as well as their triglycerides were developed within B3LYP/6-31G(d) density functional model. A vibrating FT-IR spectrum of grape seed oil was modeled on the basis of calculated values of vibrating wave numbers and IR intensities of the fatty acids triglycerides and with regard to their percentage. Triglyceride spectral bands that were formed by glycerol linkage vibrations were revealed. It was identified that triglycerol linkage has a small impact on the structure of fatty acids and, consequently, on vibrating wave numbers. The conducted molecular modeling became a basis for theoretical interpretation on 10 experimentally observed absorption bands in FT-IR spectrum of grape seed oil.

  1. Evaluation of Fungal Deterioration in Liquidambar orientalis Mill. heartwood by FT-IR and light microscopy.

    Science.gov (United States)

    Nural Yilgor; Dilek Dogu; Roderquita Moore; Evren Terzi; S. Nami Kartal

    2013-01-01

    The chemical and morphological changes in heartwood specimens of Liquidambar orientalis Mill. caused by the white-rot fungus Trametes versicolor and the brown-rot fungi Tyromyces palustris and Gloeophyllum trabeum were studied by wet chemistry, FT-IR, GC-MS analyses, and photo-...

  2. Assessment of Azithromycin in Pharmaceutical Formulation by Fourier-transform Infrared (FT-IR Transmission Spectroscopy

    Directory of Open Access Journals (Sweden)

    Muhammad Ali Mallah

    2011-12-01

    Full Text Available A simple, rapid and economical method for azithromycin quantification in solid tablet and capsule formulations has been developed by applying Fourier-transform Infrared (FT-IR transmission spectroscopy for regular quality monitoring. The newly developed method avoids the sample preparation, except grinding for pellet formation and does not involve consumption of any solvent as it absolutely eliminates the need of extraction. KBr pellets were employed for the appraisal of azithromycin while acquiring spectra of standards as well as samples on FT-IR. By selecting the FT-IR carbonyl band (C=O in the region 1,744–1,709 cm−1 the calibration model was developed based on simple Beer’s law. The excellent regression coefficient (R2 0.999 was accomplished for calibration set having standard error of calibration equal to 0.01 mg. The current work exposes that transmission FT-IR spectroscopy can definitely be applied to determine the exact amount of azithromycin to control the processing and quality of solid formulations with reduced cost and short analysis time.

  3. Attenuated total reflectance-FT-IR spectroscopy for gunshot residue analysis: potential for ammunition determination.

    Science.gov (United States)

    Bueno, Justin; Sikirzhytski, Vitali; Lednev, Igor K

    2013-08-06

    The ability to link a suspect to a particular shooting incident is a principal task for many forensic investigators. Here, we attempt to achieve this goal by analysis of gunshot residue (GSR) through the use of attenuated total reflectance (ATR) Fourier transform infrared spectroscopy (FT-IR) combined with statistical analysis. The firearm discharge process is analogous to a complex chemical process. Therefore, the products of this process (GSR) will vary based upon numerous factors, including the specific combination of the firearm and ammunition which was discharged. Differentiation of FT-IR data, collected from GSR particles originating from three different firearm-ammunition combinations (0.38 in., 0.40 in., and 9 mm calibers), was achieved using projection to latent structures discriminant analysis (PLS-DA). The technique was cross (leave-one-out), both internally and externally, validated. External validation was achieved via assignment (caliber identification) of unknown FT-IR spectra from unknown GSR particles. The results demonstrate great potential for ATR-FT-IR spectroscopic analysis of GSR for forensic purposes.

  4. Monitoring lipase-catalyzed interesterification for bulky fats modification with FT-IR/NIR spectroscopy

    DEFF Research Database (Denmark)

    Chang, Tinghong; Lai, Xuxin; Zhang, Hong

    2005-01-01

    This work demonstrates the application of FT-IR and FT-NIR spectroscopy to monitor the enzymatic interesterification process for bulky fat modification. The reaction was conducted between palm stearin and coconut oil (70/30, w/w) with the catalysis of Lipozyme TL IM at 70°C in a batch reactor...

  5. The application of FT-IR spectrum method in photocuring process for polyester acrylate

    International Nuclear Information System (INIS)

    Cao Jin; Lu Xianliang; Zhang Zhenli

    1995-01-01

    This paper describes that the UV curing process of polyester acrylate can be monitored by measuring the degree of double bonds conversion with FT-IR spectroscopy. The various factors effect the UV curing rate. The relation between the curing rate and the concentration of photoinitiator, crosslinking agent, UV light intensity was discussed. (author)

  6. Advanced sampling techniques for hand-held FT-IR instrumentation

    Science.gov (United States)

    Arnó, Josep; Frunzi, Michael; Weber, Chris; Levy, Dustin

    2013-05-01

    FT-IR spectroscopy is the technology of choice to identify solid and liquid phase unknown samples. The challenging ConOps in emergency response and military field applications require a significant redesign of the stationary FT-IR bench-top instruments typically used in laboratories. Specifically, field portable units require high levels of resistance against mechanical shock and chemical attack, ease of use in restrictive gear, extreme reliability, quick and easy interpretation of results, and reduced size. In the last 20 years, FT-IR instruments have been re-engineered to fit in small suitcases for field portable use and recently further miniaturized for handheld operation. This article introduces the HazMatID™ Elite, a FT-IR instrument designed to balance the portability advantages of a handheld device with the performance challenges associated with miniaturization. In this paper, special focus will be given to the HazMatID Elite's sampling interfaces optimized to collect and interrogate different types of samples: accumulated material using the on-board ATR press, dispersed powders using the ClearSampler™ tool, and the touch-to-sample sensor for direct liquid sampling. The application of the novel sample swipe accessory (ClearSampler) to collect material from surfaces will be discussed in some detail. The accessory was tested and evaluated for the detection of explosive residues before and after detonation. Experimental results derived from these investigations will be described in an effort to outline the advantages of this technology over existing sampling methods.

  7. Antioxidant activity and FT-IR analysis of Datura innoxia and Datura ...

    African Journals Online (AJOL)

    Materials and Methods: Determination of total phenolic content and total flavonoid content and antioxidant activity in terms of total antioxidant assay, ABTS assay, DPPH assay and in-vitro lipid peroxidation inhibiting activity were determined along with the FT-IR (Fourier transform infrared spectroscopy) analysis of the ...

  8. Signal-to-noise ratio of FT-IR CO gas spectra

    DEFF Research Database (Denmark)

    Bak, J.; Clausen, Sønnik

    1999-01-01

    in emission and transmission spectrometry, an investigation of the SNR in CO gas spectra as a function of spectral resolution has been carried out. We present a method to (1) determine experimentally the SNR at constant throughput, (2) determine the SNR on the basis of measured noise levels and Hitran......The minimum amount of a gaseous compound which can be detected and quantified with Fourier transform infrared (FT-IR) spectrometers depends on the signal-to-noise ratio (SNR) of the measured gas spectra. In order to use low-resolution FT-IR spectrometers to measure combustion gases like CO and CO2...... simulated signals, and (3) determine the SNR of CO from high to low spectral resolutions related to the molecular linewidth and vibrational-rotational lines spacing. In addition, SNR values representing different spectral resolutions but scaled to equal measurement times were compared. It was found...

  9. Prediction of the lifetime of nitrile-butadiene rubber by FT-IR.

    Science.gov (United States)

    Kawashima, Tetsuya; Ogawa, Toshio

    2005-12-01

    A quantitative measurement method with FT-IR was proposed for a thermal degradation analysis of nitrile-butadiene rubber (NBR). An NBR film was prepared as a model sample on a barium fluoride (BaF2) crystal plate, which was subjected to a heat treatment. The absorbances of various functional groups were measured directly by FT-IR after thermal degradation at high temperatures. By measuring the absorbances, it was possible to readily determine quantitatively each of the functional groups after the degradation of NBR. By assuming that the NBR lifetime was the point at which the absorbance of a carbon-carbon double bond reaches 45% of that prior to thermal treatment, a method for predicting the lifetime of NBR heated below 150 degrees C was proposed, by using an Arrhenius plot of the heating time versus heating temperature.

  10. Preliminary study of corrosion mechanisms of actinides alloys: calibration of FT-IR spectroscopy

    International Nuclear Information System (INIS)

    Magnien, Veronique; Cadignan, Marx; Faivret, Olivier; Rosa, Gaelle

    2008-01-01

    In situ analyzes of gaseous atmospheres could be performed by FT-IR spectroscopy in order to study the corrosion reactions of actinides. Nevertheless experimental conditions and the nature of studied species have a strong effect on IR absorption laws. Thus a prior calibration of our set-up is required to obtain an accurate estimation of gas concentration. For this purpose, the behavior of several air pure gases has been investigated according to their concentration from IR spectra. Reproducible results revealed subsequent increases of the most significant peak areas with gas pressure and small deviations from Beer Lambert's law. This preliminary work allowed to determine precise absorption laws for each studied pure gas in our in situ experimental conditions. Besides our FT-IR set-up was well suitable to quantitative analysis of gaseous atmosphere during corrosion reactions. Finally the effect of foreign gas will be investigated through more complex air mixtures to obtain a complete calibration network. (authors)

  11. Molecular orientation in aligned electrospun polyimide nanofibers by polarized FT-IR spectroscopy.

    Science.gov (United States)

    Yang, Haoqi; Jiang, Shaohua; Fang, Hong; Hu, Xiaowu; Duan, Gaigai; Hou, Haoqing

    2018-07-05

    Quantitative explanation on the improved mechanical properties of aligned electrospun polyimide (PI) nanofibers as the increased imidization temperatures is highly required. In this work, polarized FT-IR spectroscopy is applied to solve this problem. Based on the polarized FT-IR spectroscopy and the molecular model in the fibers, the length of the repeat unit of PI molecule, the angle between the fiber axis and the symmetric stretching direction of carbonyl group on the imide ring, and the angle between the PI molecular axis and fiber axis are all investigated. The Mark-Howink equation is used to calculate the number-average molar mass of PI molecules. The orientation states of PI molecules in the electrospun nanofibers are studied from the number-average molar mass of PI molecules and the average fiber diameter. Quantitative analysis of the orientation factor of PI molecules in the electrospun nanofibers is performed by polarized FT-IR spectroscopy. Copyright © 2018 Elsevier B.V. All rights reserved.

  12. Drift and transmission FT-IR spectroscopy of forest soils: an approach to determine decomposition processes of forest litter

    International Nuclear Information System (INIS)

    Haberhauer, G.; Gerzabek, M.H.

    1999-06-01

    A method is described to characterize organic soil layers using Fourier transformed infrared spectroscopy. The applicability of FT-IR, either dispersive or transmission, to investigate decomposition processes of spruce litter in soil originating from three different forest sites in two climatic regions was studied. Spectral information of transmission and diffuse reflection FT-IR spectra was analyzed and compared. For data evaluation Kubelka Munk (KM) transformation was applied to the DRIFT spectra. Sample preparation for DRIFT is simpler and less time consuming in comparison to transmission FT-IR, which uses KBr pellets. A variety of bands characteristics of molecular structures and functional groups has been identified for these complex samples. Analysis of both transmission FT-IR and DRIFT, showed that the intensity of distinct bands is a measure of the decomposition of forest litter. Interferences due to water adsorption spectra were reduced by DRIFT measurement in comparison to transmission FT-IR spectroscopy. However, data analysis revealed that intensity changes of several bands of DRIFT and transmission FT-IR were significantly correlated with soil horizons. The application of regression models enables identification and differentiation of organic forest soil horizons and allows to determine the decomposition status of soil organic matter in distinct layers. On the basis of the data presented in this study, it may be concluded that FT-IR spectroscopy is a powerful tool for the investigation of decomposition dynamics in forest soils. (author)

  13. High-definition Fourier Transform Infrared (FT-IR) Spectroscopic Imaging of Human Tissue Sections towards Improving Pathology

    Science.gov (United States)

    Nguyen, Peter L.; Davidson, Bennett; Akkina, Sanjeev; Guzman, Grace; Setty, Suman; Kajdacsy-Balla, Andre; Walsh, Michael J.

    2015-01-01

    High-definition Fourier Transform Infrared (FT-IR) spectroscopic imaging is an emerging approach to obtain detailed images that have associated biochemical information. FT-IR imaging of tissue is based on the principle that different regions of the mid-infrared are absorbed by different chemical bonds (e.g., C=O, C-H, N-H) within cells or tissue that can then be related to the presence and composition of biomolecules (e.g., lipids, DNA, glycogen, protein, collagen). In an FT-IR image, every pixel within the image comprises an entire Infrared (IR) spectrum that can give information on the biochemical status of the cells that can then be exploited for cell-type or disease-type classification. In this paper, we show: how to obtain IR images from human tissues using an FT-IR system, how to modify existing instrumentation to allow for high-definition imaging capabilities, and how to visualize FT-IR images. We then present some applications of FT-IR for pathology using the liver and kidney as examples. FT-IR imaging holds exciting applications in providing a novel route to obtain biochemical information from cells and tissue in an entirely label-free non-perturbing route towards giving new insight into biomolecular changes as part of disease processes. Additionally, this biochemical information can potentially allow for objective and automated analysis of certain aspects of disease diagnosis. PMID:25650759

  14. Identification and characterization of salmonella serotypes using DNA spectral characteristics by fourier transform infrared (FT-IR) spectroscopy

    Science.gov (United States)

    Analysis of DNA samples of Salmonella serotypes (Salmonella Typhimurium, Salmonella Enteritidis, Salmonella Infantis, Salmonella Heidelberg and Salmonella Kentucky) were performed using Fourier transform infrared spectroscopy (FT-IR) spectrometer by placing directly in contact with a diamond attenua...

  15. FT-IR imaging for quantitative determination of liver fat content in non-alcoholic fatty liver.

    Science.gov (United States)

    Kochan, K; Maslak, E; Chlopicki, S; Baranska, M

    2015-08-07

    In this work we apply FT-IR imaging of large areas of liver tissue cross-section samples (∼5 cm × 5 cm) for quantitative assessment of steatosis in murine model of Non-Alcoholic Fatty Liver (NAFLD). We quantified the area of liver tissue occupied by lipid droplets (LDs) by FT-IR imaging and Oil Red O (ORO) staining for comparison. Two alternative FT-IR based approaches are presented. The first, straightforward method, was based on average spectra from tissues and provided values of the fat content by using a PLS regression model and the reference method. The second one – the chemometric-based method – enabled us to determine the values of the fat content, independently of the reference method by means of k-means cluster (KMC) analysis. In summary, FT-IR images of large size liver sections may prove to be useful for quantifying liver steatosis without the need of tissue staining.

  16. Application of FT-IR spectroscopy on breast cancer serum analysis

    Science.gov (United States)

    Elmi, Fatemeh; Movaghar, Afshin Fayyaz; Elmi, Maryam Mitra; Alinezhad, Heshmatollah; Nikbakhsh, Novin

    2017-12-01

    Breast cancer is regarded as the most malignant tumor among women throughout the world. Therefore, early detection and proper diagnostic methods have been known to help save women's lives. Fourier Transform Infrared (FT-IR) spectroscopy, coupled with PCA-LDA analysis, is a new technique to investigate the characteristics of serum in breast cancer. In this study, 43 breast cancer and 43 healthy serum samples were collected, and the FT-IR spectra were recorded for each one. Then, PCA analysis and linear discriminant analysis (LDA) were used to analyze the spectral data. The results showed that there were differences between the spectra of the two groups. Discriminating wavenumbers were associated with several spectral differences over the 950-1200 cm- 1(sugar), 1190-1350 cm- 1 (collagen), 1475-1710 cm- 1 (protein), 1710-1760 cm- 1 (ester), 2800-3000 cm- 1 (stretching motions of -CH2 & -CH3), and 3090-3700 cm- 1 (NH stretching) regions. PCA-LDA performance on serum IR could recognize changes between the control and the breast cancer cases. The diagnostic accuracy, sensitivity, and specificity of PCA-LDA analysis for 3000-3600 cm- 1 (NH stretching) were found to be 83%, 84%, 74% for the control and 80%, 76%, 72% for the breast cancer cases, respectively. The results showed that the major spectral differences between the two groups were related to the differences in protein conformation in serum samples. It can be concluded that FT-IR spectroscopy, together with multivariate data analysis, is able to discriminate between breast cancer and healthy serum samples.

  17. Fluorescence, aggregation properties and FT-IR microspectroscopy of elastin and collagen fibers.

    Science.gov (United States)

    Vidal, Benedicto de Campos

    2014-10-01

    Histological and histochemical observations support the hypothesis that collagen fibers can link to elastic fibers. However, the resulting organization of elastin and collagen type complexes and differences between these materials in terms of macromolecular orientation and frequencies of their chemical vibrational groups have not yet been solved. This study aimed to investigate the macromolecular organization of pure elastin, collagen type I and elastin-collagen complexes using polarized light DIC-microscopy. Additionally, differences and similarities between pure elastin and collagen bundles (CB) were investigated by Fourier transform-infrared (FT-IR) microspectroscopy. Although elastin exhibited a faint birefringence, the elastin-collagen complex aggregates formed in solution exhibited a deep birefringence and formation of an ordered-supramolecular complex typical of collagen chiral structure. The FT-IR study revealed elastin and CB peptide NH groups involved in different types of H-bonding. More energy is absorbed in the vibrational transitions corresponding to CH, CH2 and CH3 groups (probably associated with the hydrophobicity demonstrated by 8-anilino-1-naphtalene sulfonic acid sodium salt [ANS] fluorescence), and to νCN, δNH and ωCH2 groups of elastin compared to CB. It is assumed that the α-helix contribution to the pure elastin amide I profile is 46.8%, whereas that of the B-sheet is 20% and that unordered structures contribute to the remaining percentage. An FT-IR profile library reveals that the elastin signature within the 1360-1189cm(-1) spectral range resembles that of Conex-Toray aramid fibers. Copyright © 2014 Elsevier GmbH. All rights reserved.

  18. FT-IR spectroscopic studies of protein secondary structures for breast cancer diagnosis

    International Nuclear Information System (INIS)

    Karamancheva, I; Simonova, D.; Milev, A.

    2013-01-01

    Full text: Roughly 14 million new cancer cases and 8 million cancer deaths have occurred worldwide in 2012. At least 30 % of all cancer cases and 40 % of the cancer deaths should be avoided by improving the early detection. Fourier transform infrared (FT-IR) spectroscopy has shown many advantages as a tool for the detection of cancer over the traditional methods such as histopathological analysis, X-ray transmission, ultrasonic and computer tomography techniques. With the aim to establish the FT-IR spectroscopy as an alternative method for the diagnosis of human cancers, we have made several studies to examine in details the spectroscopic properties of normal and carcinomatous tissues. Human breast tissues were obtained immediately after surgical breast resection with the informed patient's consent. In our studies we made extensive use of Fourier self-deconvolution, second-order derivatization, difference spectra, curve-fitting procedures and quantitative determinations according to Beer's law. Cancer is a multi-step process. Characteristic differences in both the frequencies and the intensity ratios of several bands have been revealed. Considerable differences have been found in the spectral patterns. The most important and informative region in the mid-IR for determination of protein secondary structure is the amide I and amide II region. The bands between 1730 and 1600 cm -1 are highly sensitive to conformational changes. Considerable changes were observed in the A1735/A1652 absorbance ratio, which provides a measure for the content of a- helix and P-sheet domains. Our investigations have shown that the major biomarker peaks are in the amide I and amide II regions. In the so called 'fingerprint region' many molecular constituents such as lipids, phospholipids, proteins, DNA and RNA, carbohydrates and metabolites may overlap and the quantitative interpretation is impossible. The spectrum may therefore reflect only the average biochemical composition.; key words

  19. Evaluation of Polymerization Efficacy in Composite Resins via FT-IR Spectroscopy and Vickers Microhardness Test

    Directory of Open Access Journals (Sweden)

    Tahereh-Sadat Jafarzadeh

    2015-12-01

    Full Text Available Background and aims. Polymerization efficacy affects the properties and performance of composite resin restorations.The purpose of this study was to evaluate the effectiveness of polymerization of two micro-hybrid, two nano-hybrid and one nano-filled ormocer-based composite resins, cured by two different light-curing systems, using Fourier transformation infrared (FT-IR spectroscopy and Vickers microhardness testing at two different depths (top surface, 2 mm. Materials and methods. For FT-IR spectrometry, five cylindrical specimens (5mm in diameter × 2 mm in length were prepared from each composite resin using Teflon molds and polymerized for 20 seconds. Then, 70-μm wafers were sectioned at the top surface and at2mm from the top surface. The degree of conversion for each sample was calculated using FT-IR spectroscopy. For Vickers micro-hardness testing, three cylindrical specimens were prepared from each composite resin and polymerized for 20 seconds. The Vickers microhardness test (Shimadzu, Type M, Japan was performed at the top and bottom (depth=2 mm surfaces of each specimen. Three-way ANOVA with independent variables and Tukey tests were performed at 95% significance level. Results. No significant differences were detected in degree of conversion and microhardness between LED and QTH light-curing units except for the ormocer-based specimen, CeramX, which exhibited significantly higher DC by LED. All the composite resins showed a significantly higher degree of conversion at the surface. Microhardness was not significantly affected by depth, except for Herculite XRV Ultra and CeramX, which showed higher values at the surface. Conclusion. Composite resins containing nano-particles generally exhibited more variations in degree of conversion and microhardness.

  20. Evaluation of Polymerization Efficacy in Composite Resins via FT-IR Spectroscopy and Vickers Microhardness Test.

    Science.gov (United States)

    Jafarzadeh, Tahereh-Sadat; Erfan, Mohammad; Behroozibakhsh, Marjan; Fatemi, Mostafa; Masaeli, Reza; Rezaei, Yashar; Bagheri, Hossein; Erfan, Yasaman

    2015-01-01

    Background and aims. Polymerization efficacy affects the properties and performance of composite resin restorations.The purpose of this study was to evaluate the effectiveness of polymerization of two micro-hybrid, two nano-hybrid and one nano-filled ormocer-based composite resins, cured by two different light-curing systems, using Fourier transformation infrared (FT-IR) spectroscopy and Vickers microhardness testing at two different depths (top surface, 2 mm). Materials and methods. For FT-IR spectrometry, five cylindrical specimens (5mm in diameter × 2 mm in length) were prepared from each composite resin using Teflon molds and polymerized for 20 seconds. Then, 70-μm wafers were sectioned at the top surface and at2mm from the top surface. The degree of conversion for each sample was calculated using FT-IR spectroscopy. For Vickers micro-hardness testing, three cylindrical specimens were prepared from each composite resin and polymerized for 20 seconds. The Vickers microhardness test (Shimadzu, Type M, Japan) was performed at the top and bottom (depth=2 mm) surfaces of each specimen. Three-way ANOVA with independent variables and Tukey tests were performed at 95% significance level. Results. No significant differences were detected in degree of conversion and microhardness between LED and QTH light-curing units except for the ormocer-based specimen, CeramX, which exhibited significantly higher DC by LED. All the composite resins showed a significantly higher degree of conversion at the surface. Microhardness was not significantly affected by depth, except for Herculite XRV Ultra and CeramX, which showed higher values at the surface. Conclusion. Composite resins containing nano-particles generally exhibited more variations in degree of conversion and microhardness.

  1. 4-Mercaptophenylboronic acid: conformation, FT-IR, Raman, OH stretching and theoretical studies.

    Science.gov (United States)

    Parlak, Cemal; Ramasami, Ponnadurai; Tursun, Mahir; Rhyman, Lydia; Kaya, Mehmet Fatih; Atar, Necip; Alver, Özgür; Şenyel, Mustafa

    2015-06-05

    4-Mercaptophenylboronic acid (4-mpba, C6H7BO2S) was investigated experimentally by vibrational spectroscopy. The molecular structure and spectroscopic parameters were studied by computational methods. The molecular dimer was investigated for intermolecular hydrogen bonding. Potential energy distribution analysis of normal modes was performed to identify characteristic frequencies. The present work provides a simple physical picture of the OH stretch vibrational spectra of 4-mpba and analogues of the compound studied. When the different computational methods are compared, there is a strong evidence of the better performance of the BLYP functional than the popular B3LYP functional to describe hydrogen bonding in the dimer. The findings of this research work should be useful to experimentalists in their quests for functionalised 4-mpba derivatives. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. Typing some of lactic acid bacteria in Syria using PCR and FT-IR techniques

    International Nuclear Information System (INIS)

    Al-Mariri, A.; Sharabi, N. D.

    2008-11-01

    Lactic Acid Bacteria (LAB) are considered to be the most useful microorganisms. They are beneficial in flavoring foods, inhibiting pathogenic as well as spoilage bacteria in food products. The isolates of LAB were obtained from traditional Syrian dairy products (white cheese and curdled yogurt) obtained from different regions in Syria. The isolates were subjected to phenotypic characterization analyses. The PCR technique of bacterial DNA was evaluated as an advanced tool for the identification of LAB. It was found that strains: E. faecium, E. faecalis and S. thermophilus dominate in white cheese and in yogurt. Our results demonstrated that we could identify LAB using Fourier transform infrared spectroscopy (FT-IR) patterns. (Authors)

  3. Typing some of lactic acid bacteria in Syria using PCR and FT-IR techniques

    Energy Technology Data Exchange (ETDEWEB)

    Al-Mariri, A; Sharabi, N D [Atomic Energy Commission, Damascus (Syrian Arab Republic), Dept. of Molecular Biology and Biotechnology

    2008-11-15

    Lactic Acid Bacteria (LAB) are considered to be the most useful microorganisms. They are beneficial in flavoring foods, inhibiting pathogenic as well as spoilage bacteria in food products. The isolates of LAB were obtained from traditional Syrian dairy products (white cheese and curdled yogurt) obtained from different regions in Syria. The isolates were subjected to phenotypic characterization analyses. The PCR technique of bacterial DNA was evaluated as an advanced tool for the identification of LAB. It was found that strains: E. faecium, E. faecalis and S. thermophilus dominate in white cheese and in yogurt. Our results demonstrated that we could identify LAB using Fourier transform infrared spectroscopy (FT-IR) patterns. (Authors)

  4. FT-IR spectroscopic analysis for studying Clostridium cell response to conversion of enzymatically hydrolyzed hay

    Science.gov (United States)

    Grube, Mara; Gavare, Marita; Nescerecka, Alina; Tihomirova, Kristina; Mezule, Linda; Juhna, Talis

    2013-07-01

    Grass hay is one of assailable cellulose containing non-food agricultural wastes that can be used as a carbohydrate source by microorganisms producing biofuels. In this study three Clostridium strains Clostridium acetobutylicum, Clostridium beijerinckii and Clostridium tetanomorphum, capable of producing acetone, butanol and ethanol (ABE) were adapted to convert enzymatically hydrolyzed hay used as a growth media additive. The results of growth curves, substrate degradation kinetics and FT-IR analyses of bacterial biomass macromolecular composition showed diverse strain-specific cell response to the growth medium composition.

  5. Authenticity study of Phyllanthus species by NMR and FT-IR techniques coupled with chemometric methods

    International Nuclear Information System (INIS)

    Santos, Maiara S.; Pereira-Filho, Edenir R.; Ferreira, Antonio G.; Boffo, Elisangela F.; Figueira, Glyn M.

    2012-01-01

    The importance of medicinal plants and their use in industrial applications is increasing worldwide, especially in Brazil. Phyllanthus species, popularly known as 'quebra-pedras' in Brazil, are used in folk medicine for treating urinary infections and renal calculus. This paper reports an authenticity study, based on herbal drugs from Phyllanthus species, involving commercial and authentic samples using spectroscopic techniques: FT-IR, 1 H HR-MAS NMR and 1 H NMR in solution, combined with chemometric analysis. The spectroscopic techniques evaluated, coupled with chemometric methods, have great potential in the investigation of complex matrices. Furthermore, several metabolites were identified by the NMR techniques. (author)

  6. Authenticity study of Phyllanthus species by NMR and FT-IR Techniques coupled with chemometric methods

    Directory of Open Access Journals (Sweden)

    Maiara S. Santos

    2012-01-01

    Full Text Available The importance of medicinal plants and their use in industrial applications is increasing worldwide, especially in Brazil. Phyllanthus species, popularly known as "quebra-pedras" in Brazil, are used in folk medicine for treating urinary infections and renal calculus. This paper reports an authenticity study, based on herbal drugs from Phyllanthus species, involving commercial and authentic samples using spectroscopic techniques: FT-IR, ¹H HR-MAS NMR and ¹H NMR in solution, combined with chemometric analysis. The spectroscopic techniques evaluated, coupled with chemometric methods, have great potential in the investigation of complex matrices. Furthermore, several metabolites were identified by the NMR techniques.

  7. Matrix isolation FT-IR spectroscopy and molecular orbital study of sarcosine methyl ester

    OpenAIRE

    Gómez-Zavaglia, Andrea; Fausto, R.

    2004-01-01

    N-methylglycine methyl ester (sarcosine-Me) has been studied by matrix isolation FT-IR spectroscopy and molecular orbital calculations undertaken at the DFT/B3LYP and MP2 levels of theory with the 6-311++G(d,p) and 6-31++G(d,p) basis set, respectively. Twelve different conformers were located in the potential energy surface of the studied compound, with the ASC conformer being the ground conformational state. This form is analogous to the dimethylglycine methyl ester most stable conformer and...

  8. Authenticity study of Phyllanthus species by NMR and FT-IR techniques coupled with chemometric methods

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Maiara S.; Pereira-Filho, Edenir R.; Ferreira, Antonio G. [Universidade Federal de Sao Carlos (UFSCAR), SP (Brazil). Dept. de Quimica; Boffo, Elisangela F. [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Inst. de Quimica; Figueira, Glyn M., E-mail: maiarassantos@yahoo.com.br [Universidade Estadual de Campinas (UNICAMP), Campinas, SP (Brazil). Centro Pluridisciplinar de Pesquisas Quimicas, Biologicas e Agricolas

    2012-07-01

    The importance of medicinal plants and their use in industrial applications is increasing worldwide, especially in Brazil. Phyllanthus species, popularly known as 'quebra-pedras' in Brazil, are used in folk medicine for treating urinary infections and renal calculus. This paper reports an authenticity study, based on herbal drugs from Phyllanthus species, involving commercial and authentic samples using spectroscopic techniques: FT-IR, {sup 1}H HR-MAS NMR and {sup 1}H NMR in solution, combined with chemometric analysis. The spectroscopic techniques evaluated, coupled with chemometric methods, have great potential in the investigation of complex matrices. Furthermore, several metabolites were identified by the NMR techniques. (author)

  9. Typing some of lactic acid bacteria in Syria using PCR and FT-IR techniques

    International Nuclear Information System (INIS)

    Al-Mariri, A.; Sharabi, N. D.

    2010-01-01

    Lactic Acid Bacteria (LAB) are considered to be the most useful microorganisms. They are beneficial in flavoring foods, inhibiting pathogenic as well as spoilage bacteria in food products. The isolates of LAB were obtained from traditional Syrian dairy products (white cheese and curdled yogurt) obtained from different regions in Syria. The isolates were subjected to phenotypic characterization analyses. The PCR technique of bacterial DNA was evaluated as an advanced tool for the identification of LAB. It was found that strains: E. faecium, E. faecalis and S. thermophilus dominate in white cheese and in yogurt. Our results demonstrated that we could identify LAB using Fourier transform infrared spectroscopy (FT-IR) patterns. (author)

  10. [Application of FT-IR pattern recognition method for the quality control of pharmaceutical ingredients].

    Science.gov (United States)

    Horgos, József; Kóger, Péter; Zelkó, Romána

    2009-01-01

    Nowadays infrared spectroscopy and chemometrics have proven their effectiveness for both qualitative and quantitative analyses in different fields like agriculture, food, chemical and oil industry. Furier Transformation Infrared Spectroscopy (FT-IR) combined with Attenuated Total Reflectance (ATR) plate is a fast identification instrument. It is suitable for analysis of solid and liquid phase, too. Associated with chemometrics, it would be a powerful tool for the pharmaceutical wholesalers to detect the insufficient quality of pharmaceutical ingredients. In the present study beside the review of the infra red technology, pharmaceutical ingredients were examined with the help of our spectra library.

  11. Authenticity study of Phyllanthus species by NMR and FT-IR techniques coupled with chemometric methods

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Maiara S.; Pereira-Filho, Edenir R.; Ferreira, Antonio G. [Universidade Federal de Sao Carlos (UFSCAR), SP (Brazil). Dept. de Quimica; Boffo, Elisangela F. [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Inst. de Quimica; Figueira, Glyn M., E-mail: maiarassantos@yahoo.com.br [Universidade Estadual de Campinas (UNICAMP), Campinas, SP (Brazil). Centro Pluridisciplinar de Pesquisas Quimicas, Biologicas e Agricolas

    2012-07-01

    The importance of medicinal plants and their use in industrial applications is increasing worldwide, especially in Brazil. Phyllanthus species, popularly known as 'quebra-pedras' in Brazil, are used in folk medicine for treating urinary infections and renal calculus. This paper reports an authenticity study, based on herbal drugs from Phyllanthus species, involving commercial and authentic samples using spectroscopic techniques: FT-IR, {sup 1}H HR-MAS NMR and {sup 1}H NMR in solution, combined with chemometric analysis. The spectroscopic techniques evaluated, coupled with chemometric methods, have great potential in the investigation of complex matrices. Furthermore, several metabolites were identified by the NMR techniques. (author)

  12. Using FT-IR Spectroscopy to Elucidate the Structures of Ablative Polymers

    Science.gov (United States)

    Fan, Wendy

    2011-01-01

    The composition and structure of an ablative polymer has a multifaceted influence on its thermal, mechanical and ablative properties. Understanding the molecular level information is critical to the optimization of material performance because it helps to establish correlations with the macroscopic properties of the material, the so-called structure-property relationship. Moreover, accurate information of molecular structures is also essential to predict the thermal decomposition pathways as well as to identify decomposition species that are fundamentally important to modeling work. In this presentation, I will describe the use of infrared transmission spectroscopy (FT-IR) as a convenient tool to aid the discovery and development of thermal protection system materials.

  13. A Controlled-Environment Chamber for Atmospheric Chemistry Studies Using FT-IR Spectroscopy

    Science.gov (United States)

    1990-06-01

    necessary and identify by block number) FELD GROUP SUB-GROUP i >Chamber, controlled environment; long-path cell ; 07 04 FT-IR; Hydrazine decay...modification doubles the useable path length of the original multipass cell described by White (Reference 8). The pattern of images formed on the nesting...system is shown in Figure 13. 24 z C C02, Ibm, El4 944 C3 ta) caC E-4- 252 14 $4 41) 41) 0. 0 04 04 4 41) ~0 to 0.0 V-4 (A q14 0~ 1% 4-r4 $4 0 u P416 4 4

  14. Rapid identification of Chinese Sauce liquor from different fermentation positions with FT-IR spectroscopy

    Science.gov (United States)

    Li, Changwen; Wei, Jiping; Zhou, Qun; Sun, Suqin

    2008-07-01

    FT-IR and two-dimensional correlation spectroscopy (2D-IR) technology were applied to discriminate Chinese Sauce liquor from different fermentation positions (top, middle and bottom of fermentation cellar) for the first time. The liquors at top, middle and bottom of fermentation cellar, possessed the characteristic peaks at 1731 cm -1, 1733 cm -1 and 1602 cm -1, respectively. In the 2D correlation infrared spectra, the differences were amplified. A strong auto-peak at 1725 cm -1 showed in the 2D spectra of the Top Liquor, which indicated that the liquor might contain some ester compounds. Different from Top Liquor, three auto-peaks at 1695, 1590 and 1480 cm -1 were identified in 2D spectra of Middle Liquor, which were the characteristic absorption of acid, lactate. In 2D spectra of Bottom Liquor, two auto-peaks at 1570 and 1485 cm -1 indicated that lactate was the major component. As a result, FT-IR and 2D-IR correlation spectra technology provided a rapid and effective method for the quality analysis of the Sauce liquor.

  15. Chemical fingerprinting of Arabidopsis using Fourier transform infrared (FT-IR) spectroscopic approaches.

    Science.gov (United States)

    Gorzsás, András; Sundberg, Björn

    2014-01-01

    Fourier transform infrared (FT-IR) spectroscopy is a fast, sensitive, inexpensive, and nondestructive technique for chemical profiling of plant materials. In this chapter we discuss the instrumental setup, the basic principles of analysis, and the possibilities for and limitations of obtaining qualitative and semiquantitative information by FT-IR spectroscopy. We provide detailed protocols for four fully customizable techniques: (1) Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS): a sensitive and high-throughput technique for powders; (2) attenuated total reflectance (ATR) spectroscopy: a technique that requires no sample preparation and can be used for solid samples as well as for cell cultures; (3) microspectroscopy using a single element (SE) detector: a technique used for analyzing sections at low spatial resolution; and (4) microspectroscopy using a focal plane array (FPA) detector: a technique for rapid chemical profiling of plant sections at cellular resolution. Sample preparation, measurement, and data analysis steps are listed for each of the techniques to help the user collect the best quality spectra and prepare them for subsequent multivariate analysis.

  16. FT-IR and X-ray spectroscopic investigations of Na-diclofenac-cyclodextrins interactions

    Science.gov (United States)

    Bratu, I.; Astilean, S.; Ionesc, Corina; Indrea, E.; Huvenne, J. P.; Legrand, P.

    1998-01-01

    The association of DCF-Na (the salt of the 2-[(2,6-dichlorophenyl)amino]-phenyl-acetic acid) with β-CD (cyclodextrin) in some therapeutic formulas can contribute to the optimisation of the physico-chemical and pharmaceutical properties of the parent drug. The understanding of the interaction between DCF with β-CD represents the objective of this study. FT-IR spectroscopy is one of the methods which clarify the nature of these interactions in complexes of such type. Therefore the changes in FT-IR spectra of binary dispersed systems DCF/ β-CD in physical mixture and coprecipitate from methanol (molar ratios: 1/1, 1/2, 2/3, 3/4, 7/4) were analysed. The analysis of the broadening of the X-ray powder diffraction line has been applied to investigate the average effective crystallite size, the mean square of the microstrain caused by distortions within β-CD crystallite and the fault probability in the binary dispersed DCF/ β-CD coprecipitate system.

  17. Monitoring wine aging with Fourier transform infrared spectroscopy (FT-IR

    Directory of Open Access Journals (Sweden)

    Basalekou Marianthi

    2015-01-01

    Full Text Available Oak wood has commonly been used in wine aging but recently other wood types such as Acacia and Chestnut, have attracted the interest of the researchers due to their possible positive contribution to wine quality. However, only the use of oak and chestnut woods is approved by the International Enological Codex of the International Organisation of Vine and Wine. In this study Fourier Transform (FT-mid-infrared spectroscopy combined with Discriminant Analysis was used to differentiate wines aged in barrels made from French oak, American oak, Acacia and Chestnut and in tanks with oak chips, over a period of 12 months. Two red (Mandilaria, Kotsifali and two white (Vilana, Dafni native Greek grape varieties where used to produce four wines. The Fourier Transform Infrared (FT-IR spectra of the samples were recorded on a Zinc Selenide (ZnSe window after incubation at 40 °C for 30 min. A complete differentiation of the samples according to both the type of wood used and the contact time was achieved based on their FT-IR spectra.

  18. FT-IR emissivity measurements of Nb melt using an electrostatic levitation furnace

    International Nuclear Information System (INIS)

    Sakata, K.; Watanabe, Y.; Okada, J.T.; Kumar, M.V.; Paradis, P.-F.; Ishikawa, T.

    2015-01-01

    Highlights: • Since molten Nb has a high melting point, its thermal properties were measured using FT-IR combined with an electrostatic levitator. • The measured ε_T of molten Nb at the melting temperature in this study was 0.29, and the C_p was calculated as 41.9 J ⋅ mol"−"1 ⋅ K"−"1. - Abstract: Total hemispherical emissivity (ε_T) and constant pressure heat capacity (C_p) of molten Nb, which has a high melting point, was measured using FT-IR combined with an electrostatic levitator. In order to heat the sample to temperatures higher than 2000 °C and avoid chemical reactions between the sample and a crucible, a containerless method was needed. By applying these methods, the measured ε_T of molten Nb at the melting temperature was 0.29, and the C_p was calculated as 41.9 J ⋅ mol"−"1 ⋅ K"−"1. Both data showed good agreement with the literature values. In addition, the result was compared with the Drude model and the difference of emissivity between Zr and Nb was discussed.

  19. Development of a method for determination of fatty acid using FT-IR spectroscopy

    Directory of Open Access Journals (Sweden)

    Dimas Augusto Morozin Zaia

    2011-05-01

    Full Text Available In the present paper a new methodology has been developed for determination of fatty acids in biological systems using FT-IR spectroscopy. For this method is not necessary chromophore reagent or pre sample preparation. Palmitic acid was chosen as standard, because it is found in several biological systems. The FT-IR spectrum of palmitic acid showed two absorption bands in the region of 2852 and 2920 cm-1 attributed to CH stretching. The results for these bands showed that the Beer-Lambert Law was followed in wide range of concentration of palmitic acid (14 to 257 mmol L-1. Potassium ferricyanide (K3[Fe(CN6] was used as internal standard. Several interferents were tested and only cholesterol, ferric chloride (higher concentration, mixture of amino acids for the band at 2919 cm-1 (higher concentration and triglyceride could be interferent if they appear in high concentration. Thus, this new methodology has advantage to be not expensive and simple.

  20. FT-IR microspectroscopy characterization of supports for enzyme immobilization in biosensing applications

    Science.gov (United States)

    Portaccio, M.; Della Ventura, B.; Gabrovska, K.; Marinov, I.; Godjevargova, T.; Mita, D. G.; Lepore, M.

    2010-04-01

    The investigation of materials suitable for enzyme immobilization in biosensing applications has a widespread interest. There are many studies on physico-chemical properties of these materials at macroscopic level but few studies have been devoted to examine and correlate these properties at microscopic level. FT-IR spectroscopy with Micro-Attenuated Total Reflection (Micro-ATR) approach can be extremely useful for understanding a variety of aspects of materials which can be used for optimising immobilization procedures. Moreover, this experimental approach is particularly simple to use (no sample preparation is required) and minimally invasive. Using a Perkin Elmer Spectrum One FT-IR spectrometer equipped with a mercury-cadmium-telluride detector and a micro-ATR element we investigated different materials used for immobilization procedures with various enzymes widely used for biosensing in environmental and clinical applications. In particular, composite membranes constituted by a chemically modified poly-acrylonitrile (PAN) membrane plus layers of tethered chitosan of different molecular weight have been examined. Also silica gel matrices without and with glucose oxidase have been investigated. Spectra have been analysed and the contribution of principal functional groups has been evidenced.

  1. FT-IR microscopical analysis with synchrotron radiation: The microscope optics and system performance

    International Nuclear Information System (INIS)

    Reffner, J.A.; Martoglio, P.A.; Williams, G.P.

    1995-01-01

    When a Fourier transform infrared (FT-IR) microspectrometer was first interfaced with the National Synchrotron Light Source (NSLS) in September 1993, there was an instant realization that the performance at the diffraction limit had increased 40-100 times. The synchrotron source transformed the IR microspectrometer into a true IR microprobe, providing high-quality IR spectra for probe diameters at the diffraction limit. The combination of IR microspectroscopy and synchrotron radiation provides a powerful new tool for molecular spectroscopy. The ability to perform IR microspectroscopy with synchrotron radiation is still under development at Brookhaven National Laboratory, but several initial studies have been completed that demonstrate the broad-ranging applications of this technology and its potential for materials characterization

  2. FT-IR spectroscopic analyses of 2-(2-furanylmethylene) propanedinitrile

    Science.gov (United States)

    Soliman, H. S.; Eid, Kh. M.; Ali, H. A. M.; El-Mansy, M. A. M.; Atef, S. M.

    2013-03-01

    In the present work, a computational study for the optimized molecular structural parameters, thermo-chemical parameters, total dipole moment, HOMO-LUMO energy gap and a combined experimental and computational study for FT-IR spectra for 2-(2-furanylmethylene) propanedinitrile have been investigated using B3LYP utilizing 6-31G and 6-311G basis set. Our calculated results showed that the investigated compound possesses a dipole moment of 7.5 D and HOMO-LUMO energy gap of 3.92 eV using B3LYP/6-311G which indicates that our investigated compound is highly applicable for photovoltaic solar cell applications.

  3. Analysis of pure and malachite green doped polysulfone sample using FT-IR technique

    Science.gov (United States)

    Nayak, Rashmi J.; Khare, P. K.; Nayak, J. G.

    2018-05-01

    The sample of pure and malachite green doped Polysulfone in the form of foil was prepared by isothermal immersion technique. For the preparation of pure sample 4 gm of Polysulfone was dissolved in 50 ml of Dimethyl farmamide (DMF) solvent, while for the preparation of doped sample 10 mg, 50 mg and 100 mg Malachite Green was mixed with 4 gm of Polysulfone respectively. For the study of structural characterization of these pure and doped sample, Fourier Transform Infra-Red Spectroscopy (FT-IR) technique was used. This study shows that the intensity of transmittance decreases as the ratio of doping increases in pure polysulfone. The reduction in intensity of transmittance is clearly apparent in the present case more over the bands were broader which indicates towards charge transfer interaction between the donar and acceptor molecule.

  4. Spectroelectrochemical study of polyphenylene by in situ external reflection FT-IR spectroscopy. Pt. 2

    International Nuclear Information System (INIS)

    Kvarnstroem, C.; Ivaska, A.

    1994-01-01

    In situ external reflection FT-IR measurements are performed during cyclic voltammetric scans on electrochemically polymerized polyphenylene films. The films are polymerized either in 0.1 or 0.8 M biphenyl in 0.1 M TBABF 4 in acetonitrile. Changes in the IR spectrum of films of different thicknesses are studied when the films are potentially cycled from the neutral to the oxidized states of the polymer. No differences between films made in high or low dimer concentration can be observed in the spectra. The potential-dependent insertion and expulsion of solvent, residual water, anions and cations in and out of the film have different behaviour in films of different thicknesses. Changes in the structure of the segments in the film, from the benzenoid form into the quinoid form, can be followed. Differences between the first and subsequent cyclic potential scans are observed. (orig.)

  5. FT-IR microscopical analysis with synchrotron radiation: The microscope optics and system performance

    Energy Technology Data Exchange (ETDEWEB)

    Reffner, J.A.; Martoglio, P.A. [Spectra-Tech, Inc., Shelton, CT (United States); Williams, G.P. [Brookhaven National Lab., Upton, NY (United States)

    1995-01-01

    When a Fourier transform infrared (FT-IR) microspectrometer was first interfaced with the National Synchrotron Light Source (NSLS) in September 1993, there was an instant realization that the performance at the diffraction limit had increased 40-100 times. The synchrotron source transformed the IR microspectrometer into a true IR microprobe, providing high-quality IR spectra for probe diameters at the diffraction limit. The combination of IR microspectroscopy and synchrotron radiation provides a powerful new tool for molecular spectroscopy. The ability to perform IR microspectroscopy with synchrotron radiation is still under development at Brookhaven National Laboratory, but several initial studies have been completed that demonstrate the broad-ranging applications of this technology and its potential for materials characterization.

  6. Investigation of UV curing reaction of dicyclopentadienyl acrylate by FT-IR

    International Nuclear Information System (INIS)

    Lu Qiting; Hou Yibin

    1999-01-01

    Dicyclopentadienyl acrylate (DCPA) is characterized by low odor, low volatility, high flash point, low toxicity and low shrinkage on cure. Another advantage of DCPA is its insensitiveness to the inhibiting effect of oxygen. DCPA have wide industrial applications. It was used for the preparation of adhesives, UV-curable coatings and polymer concreted). The advantages of DCPA result from its particular structure. There are two unsaturated bonds, one acrylic double bond and one cyclic double bond, in each DCPA molecule. But, few reports on reaction behavior of the two type double bonds were issued up to date. In this paper, reaction behavior of the acrylic and the cyclic double bond of DCPA during and after LTV-curing were investigated by Fourier Transform-Infrared(FT-IR)

  7. Analysis of cosmetic residues on a single human hair by ATR FT-IR microspectroscopy

    Science.gov (United States)

    Pienpinijtham, Prompong; Thammacharoen, Chuchaat; Naranitad, Suwimol; Ekgasit, Sanong

    2018-05-01

    In this work, ATR FT-IR spectra of single human hair and cosmetic residues on hair surface are successfully collected using a homemade dome-shaped Ge μIRE accessary installed on an infrared microscope. By collecting ATR spectra of hairs from the same person, the spectral patterns are identical and superimposed while different spectral features are observed from ATR spectra of hairs collected from different persons. The spectral differences depend on individual hair characteristics, chemical treatments, and cosmetics on hair surface. The "Contact-and-Collect" technique that transfers remarkable materials on the hair surface to the tip of the Ge μIRE enables an identification of cosmetics on a single hair. Moreover, the differences between un-split and split hairs are also studied in this report. These highly specific spectral features can be employed for unique identification or for differentiation of hairs based on the molecular structures of hairs and cosmetics on hairs.

  8. Characterization of Paracoccidioides brasiliensis by FT-IR spectroscopy and nanotechnology

    Science.gov (United States)

    Ferreira, Isabelle; Ferreira-Strixino, Juliana; Castilho, Maiara L.; Campos, Claudia B. L.; Tellez, Claudio; Raniero, Leandro

    2016-01-01

    Paracoccidioides brasiliensis, the etiological agent of paracoccidioidomycosis, is a dimorphic fungus existing as mycelia in the environment (or at 25 °C in vitro) and as yeast cells in the human host (or at 37 °C in vitro). Because mycological examination of lesions in patients frequently is unable to show the presence of the fungus and serological tests can misdiagnose the disease with other mycosis, the development of new approach's for molecular identification of P. brasiliensis spurges is needed. This study describes the use of a gold nanoprobe of a known gene sequence of P. brasiliensis as a molecular tool to identify P. brasiliensis by regular polymerase chain reaction (PCR) associated with a colorimetric methods. This approach is suitable for testing in remote areas because it does not require any further step than gene amplification, being safer and cheaper than electrophoresis methods. The proposed test showed a color change of the PCR reaction mixture from red to blue in negative samples, whereas the solution remains red in positive samples. We also performed a Fourier Transform Infrared (FT-IR) Spectroscopy analysis to characterize and compare the chemical composition between yeast and mycelia forms, which revealed biochemical differences between these two forms. The analysis of the spectra showed that differences were distributed in chemical bonds of proteins, lipids and carbohydrates. The most prominent difference between both forms was vibration modes related to 1,3-β-glucan usually found in mycelia and 1,3-α-glucan found in yeasts and also chitin forms. In this work, we introduce FT-IR as a new method suitable to reveal overall differences that biochemically distinguish each form of P. brasiliensis that could be additionally used to discriminate biochemical differences among a single form under distinct environmental conditions.

  9. Effect of Water on HEMA Conversion by FT-IR Spectroscopy

    Directory of Open Access Journals (Sweden)

    TS. Jafarzadeh Kashi

    2007-09-01

    Full Text Available Objective: The use of HEMA as a biocompatible material in dentin bonding systems and its potential for clinical applications has been well established. Excess water can affect conversion of bonding resins. The aim of this study was to survey the effect of water on the degree of conversion of HEMA by Fourier Transform Infra-red Spectroscopy (FT-IR.Materials and Methods: In this experimental study, distilled water was added in amounts of 0, 0.05, 0.1, 0.2, and 0.4 ml to 1 ml of curable HEMA solution. Six repetitions per wa-ter ratio were made and investigated. Each sample was polymerized for 60 seconds. De-gree of conversion was obtained from the absorbance IR-Spectrum of the materials before and after polymerization by FT-IR spectroscopy. One way ANOVA and Tukey-HSD were carried out to compare and detect any differences among groups.Results: Statistical analysis indicates highly significant difference between pairs of groups at level (P<0.001. The results showed a trend of decreasing in HEMA conversion with increasing water. Degree of conversion changes significantly within the 0.05 ml to 0.2 ml water range. However, degree of conversion did not change after reaching 0.02 ml and before 0.05.Conclusion: Degree of conversion of HEMA decreased by increasing water. The most dramatic effect of water on the polymerization process occurs within a range which exists under clinical conditions. The reason that the degree of conversion did not show signifi-cant result before 0.05 ml may be related to the hydrophilic nature of HEMA.

  10. FT-IR study of gamma-radiation induced degradation of polyvinyl alcohol (PVA) and PVA/humic acids blends

    International Nuclear Information System (INIS)

    Ilcin, M.; Hola, O.; Bakajova, B.; Kucerik, J.

    2010-01-01

    Samples of pure polyvinyl alcohol (PVA) and PVA doped with humic acids were exposed to gamma radiation. Gamma rays induced the degradation of the pure polymer. Degradation changes were observed using ATR FT-IR equipment. Dehydration, double bond creation, and their subsequent oxidation (surrounding atmosphere was air) were found out. Also, other degradation reactions (e.g. chain scission, cyclization) occur simultaneously. Formation of C=C and C=O bonds is apparent from FT-IR spectra. In contrast the presence of humic acids in the PVA sample showed stabilizing effect on PVA structure within the concentration range 0.5-10%. (author)

  11. A novel synthesis of octahydropyrido[3,2-c]carbazole framework of aspidospermidine alkaloids and a combined computational, FT-IR, NMR, NBO, NLO, FMO, MEP study of the cis-4a-Ethyl-1-(2hydroxyethyl)-2,3,4,4a,5,6,7,11c-octahydro-1H-pyrido[3,2-c]carbazole

    Science.gov (United States)

    Uludağ, Nesimi; Serdaroğlu, Goncagul; Yinanc, Abdullah

    2018-06-01

    In this study, we performed a novel synthesis of the octahydropyrido[3,2-c]carbazole derivative 6 from 1 in five steps with a 34% overall yield. We also developed a unique compound 2 by a cyclization reaction from the cyanoethylation of compound 1, which is an intermediate step in the synthesis of Aspidospermidine. The parent compound of Aspidospermidine alkaloids, comprise a large family of diverse structures. As a result, we obtained octahydropyrido[3,2-c]carbazole (6)and the proposed method may be applicable to other alkaloids. All quantum chemical calculations of the cis-4a-Ethyl-1-(2-hydroxyethyl)-2,3,4,4a,5,6,7,11c-octahydro-1H-pyrido[3,2-c]carbazole have been performed with the DFT/B3LYP and HF methods by using the Gaussian 09W software package. The most stable conformer obtained from the Potential Energy Surface (PES) scan analysis at the B3LYP/6-31G** level of theory in the gas phase was used as the starting structure of the title compound to further computational analysis. The Natural Bond Orbital (NBO) and NLO analyses were performed to evaluate the intra-molecular interactions contributing to the molecular stability and to predict the optical properties of the title compound, respectively. Gauge-Independent Atomic Orbital (GIAO) approach was used to determine the 1H and 1C NMR chemical shifts of the title compound by subtracting the shielding constants of TMS at both methods. The calculated vibrational frequencies of the title compound were assigned by using the VEDA program and were scaled down by using the scaling factor 0.9668 for B3LYP/6-311++G(d, p) and 0.9050 for HF/6-311++G(d, p) to improve the calculated vibrational frequencies. The FMO (frontier molecular orbital) analysis was evaluated to predict the chemical and physical properties of the title compound and the HOMO, LUMO, and MEP diagrams were visualized by GaussView 4.1 program to present the reactive site of the title compound.

  12. Matrix isolation FT-IR spectroscopy and molecular orbital study of sarcosine methyl ester

    Science.gov (United States)

    Gómez-Zavaglia, A.; Fausto, R.

    2004-02-01

    N-methylglycine methyl ester (sarcosine-Me) has been studied by matrix isolation FT-IR spectroscopy and molecular orbital calculations undertaken at the DFT/B3LYP and MP2 levels of theory with the 6-311++G(d,p) and 6-31++G(d,p) basis set, respectively. Twelve different conformers were located in the potential energy surface of the studied compound, with the ASC conformer being the ground conformational state. This form is analogous to the dimethylglycine methyl ester most stable conformer and is characterized by a NH⋯O intramolecular hydrogen bond; in this form, the ester group assumes the cis configuration and the OC-C-N and Lp-N-C-C (where Lp is the nitrogen lone electron pair) dihedral angles are ca. -17.8 and 171.3°, respectively. The second most stable conformer ( GSC) differs from the ASC conformer essentially in the conformation assumed by the methylamino group, which in this case is gauche ( Lp-N-C-C dihedral angle equal to 79.4°). On the other hand, the third most stable conformer ( AAC) differs from the most stable form in the conformation of the OC-C-N axis (151.4°). These three forms were predicted to differ in energy by less than ca. 5 kJ mol -1 and represent ≈95% of the total conformational population at room temperature. FT-IR spectra were obtained for sarcosine-Me isolated in argon matrices (T=9 K) revealing the presence in the matrices of the three lowest energy conformers predicted by the calculations. The matrices were prepared by deposition of the vapour of the compound using two different nozzle temperatures, 25 and 60 °C. The relative populations of the three conformers trapped in the matrices were found to be consistent with occurrence of conformational cooling during matrix deposition and with a stabilization of the most polar GSC and AAC conformers in the matrices compared to the gas phase. Indeed, like it was previously observed for the methyl ester of dimethylglycine [Phys. Chem. Chem. Phys. 5 (2003) 52] the different

  13. Sugar and acid content of Citrus prediction modeling using FT-IR fingerprinting in combination with multivariate statistical analysis.

    Science.gov (United States)

    Song, Seung Yeob; Lee, Young Koung; Kim, In-Jung

    2016-01-01

    A high-throughput screening system for Citrus lines were established with higher sugar and acid contents using Fourier transform infrared (FT-IR) spectroscopy in combination with multivariate analysis. FT-IR spectra confirmed typical spectral differences between the frequency regions of 950-1100 cm(-1), 1300-1500 cm(-1), and 1500-1700 cm(-1). Principal component analysis (PCA) and subsequent partial least square-discriminant analysis (PLS-DA) were able to discriminate five Citrus lines into three separate clusters corresponding to their taxonomic relationships. The quantitative predictive modeling of sugar and acid contents from Citrus fruits was established using partial least square regression algorithms from FT-IR spectra. The regression coefficients (R(2)) between predicted values and estimated sugar and acid content values were 0.99. These results demonstrate that by using FT-IR spectra and applying quantitative prediction modeling to Citrus sugar and acid contents, excellent Citrus lines can be early detected with greater accuracy. Copyright © 2015 Elsevier Ltd. All rights reserved.

  14. Detection and classification of salmonella serotypes using spectral signatures collected by fourier transform infrared (FT-IR) spectroscopy

    Science.gov (United States)

    Spectral signatures of Salmonella serotypes namely Salmonella Typhimurium, Salmonella Enteritidis, Salmonella Infantis, Salmonella Heidelberg and Salmonella Kentucky were collected using Fourier transform infrared spectroscopy (FT-IR). About 5-10 µL of Salmonella suspensions with concentrations of 1...

  15. Matrix-isolation FT-IR spectra and theoretical study of dimethyl sulfate

    Science.gov (United States)

    Borba, Ana; Gómez-Zavaglia, Andrea; Simões, Pedro N. N. L.; Fausto, Rui

    2005-05-01

    The preferred conformations of dimethyl sulfate and their vibrational spectra were studied by matrix-isolation FT-IR spectroscopy and theoretical methods (DFT and MP2, with basis sets of different sizes, including the quadruple-zeta, aug-cc-pVQZ basis). Conformer GG (of C 2 symmetry and exhibiting O sbnd S sbnd O sbnd C dihedral angles of 74.3°) was found to be the most stable conformer in both the gaseous phase and isolated in argon. Upon annealing of the matrix, the less stable observed conformer (GT; with C 1 symmetry) quickly converts to the GG conformer, with the resulting species being embedded in a matrix-cage which corresponds to the most stable matrix-site for GG form. The highest energy TT conformer, which was assumed to be the most stable conformer in previous studies, is predicted by the calculations to have a relative energy of ca. 10 kJ mol -1 and was not observed in the spectra of the matrix-isolated compound.

  16. FT-IR, NMR spectroscopic and quantum mechanical investigations of two ferrocene derivatives

    Directory of Open Access Journals (Sweden)

    Ö. Alver

    2017-07-01

    Full Text Available New ferrocene derivatives as N-(3-piperidin-1-ylpropylferrocenamide (Fc-3ppa and N-(pyridine-3-ylmethylferrocenamide (Fc-3pica and structural investigations were carried out with 1H, 13C, DEPT 45 or 135, HETCOR, COSY NMR and FT-IR spectroscopic techniques. Characterization of Fc-3ppa (FeC19H26N2O and Fc-3pica (FeC17H16N2O was also supported by density functional theory (DFT used by B3LYP functional and 6-31G(d or 6-311++G(d,p basis sets. From the combination of all the results, it can be clearly seen that syntheses of Fc-3ppa and Fc-3pica have been successfully achieved. Theoretical values are successfully compared against experimental data and B3LYP method is able to provide satisfactory results for predicting NMR properties and vibrational frequencies of the synthesized ferrocene based systems.

  17. FT-IR studies on interactions among components in hexanoyl chitosan-based polymer electrolytes

    Science.gov (United States)

    Winie, Tan; Arof, A. K.

    2006-03-01

    Fourier transform infrared (FT-IR) spectroscopic studies have been undertaken to investigate the interactions among components in a system of hexanoyl chitosan-lithium trifluoromethanesulfonate (LiCF 3SO 3)-diethyl carbonate (DEC)/ethylene carbonate (EC). LiCF 3SO 3 interacts with the hexanoyl chitosan to form a hexanoyl chitosan-salt complex that results in the shifting of the N(COR) 2, C dbnd O sbnd NHR and OCOR bands to lower wavenumbers. Interactions between EC and DEC with LiCF 3SO 3 has been noted and discussed. Evidence of interaction between EC and DEC has been obtained experimentally. Studies on polymer-plasticizer spectra suggested that there is no interaction between the polymer host and plasticizers. Competition between plasticizer and polymer on associating with Li + ions was observed from the spectral data for gel polymer electrolytes. The obtained spectroscopic data has been correlated with the conductivity performance of hexanoyl chitosan-based polymer electrolytes.

  18. FT-IR spectroscopic imaging of reactions in multiphase flow in microfluidic channels.

    Science.gov (United States)

    Chan, K L Andrew; Kazarian, Sergei G

    2012-05-01

    Rapid, in situ, and label-free chemical analysis in microfluidic devices is highly desirable. FT-IR spectroscopic imaging has previously been shown to be a powerful tool to visualize the distribution of different chemicals in flows in a microfluidic device at near video rate imaging speed without tracers or dyes. This paper demonstrates the possibility of using this imaging technology to capture the chemical information of all reactants and products at different points in time and space in a two-phase system. Differences in the rates of chemical reactions in laminar flow and segmented flow systems are also compared. Neutralization of benzoic acid in decanol with disodium phosphate in water has been used as the model reaction. Quantitative information, such as concentration profiles of reactant and products, can be extracted from the imaging data. The same feed flow rate was used in both the laminar flow and segmented flow systems. The laminar flow pattern was achieved using a plain wide T-junction, whereas the segmented flow was achieved by introducing a narrowed section and a nozzle at the T-junction. The results show that the reaction rate is limited by diffusion and is much slower with the laminar flow pattern, whereas the reaction is completed more quickly in the segmented flow due to better mixing.

  19. Spectroelectrochemical study of polyphenylene by in situ external reflection FT-IR spectroscopy. Pt. 1

    International Nuclear Information System (INIS)

    Kvarnstroem, C.; Ivaska, A.

    1994-01-01

    In situ spectroelectrochemical measurements with external reflection FT-IR are performed at different stages of polymerization of 0.05, 0.1 and 0.8 M biphenyl in 0.1 M TBABF 4 in acetonitrile. The biphenyl concentration is not found to have any effect on the structure of the polymer formed. Formation of oligomers and the ratio of ortho/para-substituted polymer chains during film growth are studied. The first coupling of dimers to oligomers is found to take place in the vicinity of the electrode surface and at a later stage of polymerization the oligomers start to form polymer film on the electrode. A mixed para and ortho coupling resulting in crosslinking between chains is observed already at the early stage of polymerization. However, when a lower current density is used a more ordered polymer structure is obtained. A breakdown of the polymer film due to overoxidation can be seen when the potential is increased to 2.0 V. (orig.)

  20. Analysis of cosmetic residues on a single human hair by ATR FT-IR microspectroscopy.

    Science.gov (United States)

    Pienpinijtham, Prompong; Thammacharoen, Chuchaat; Naranitad, Suwimol; Ekgasit, Sanong

    2018-05-15

    In this work, ATR FT-IR spectra of single human hair and cosmetic residues on hair surface are successfully collected using a homemade dome-shaped Ge μIRE accessary installed on an infrared microscope. By collecting ATR spectra of hairs from the same person, the spectral patterns are identical and superimposed while different spectral features are observed from ATR spectra of hairs collected from different persons. The spectral differences depend on individual hair characteristics, chemical treatments, and cosmetics on hair surface. The "Contact-and-Collect" technique that transfers remarkable materials on the hair surface to the tip of the Ge μIRE enables an identification of cosmetics on a single hair. Moreover, the differences between un-split and split hairs are also studied in this report. These highly specific spectral features can be employed for unique identification or for differentiation of hairs based on the molecular structures of hairs and cosmetics on hairs. Copyright © 2018 Elsevier B.V. All rights reserved.

  1. Similarity maps and hierarchical clustering for annotating FT-IR spectral images.

    Science.gov (United States)

    Zhong, Qiaoyong; Yang, Chen; Großerüschkamp, Frederik; Kallenbach-Thieltges, Angela; Serocka, Peter; Gerwert, Klaus; Mosig, Axel

    2013-11-20

    Unsupervised segmentation of multi-spectral images plays an important role in annotating infrared microscopic images and is an essential step in label-free spectral histopathology. In this context, diverse clustering approaches have been utilized and evaluated in order to achieve segmentations of Fourier Transform Infrared (FT-IR) microscopic images that agree with histopathological characterization. We introduce so-called interactive similarity maps as an alternative annotation strategy for annotating infrared microscopic images. We demonstrate that segmentations obtained from interactive similarity maps lead to similarly accurate segmentations as segmentations obtained from conventionally used hierarchical clustering approaches. In order to perform this comparison on quantitative grounds, we provide a scheme that allows to identify non-horizontal cuts in dendrograms. This yields a validation scheme for hierarchical clustering approaches commonly used in infrared microscopy. We demonstrate that interactive similarity maps may identify more accurate segmentations than hierarchical clustering based approaches, and thus are a viable and due to their interactive nature attractive alternative to hierarchical clustering. Our validation scheme furthermore shows that performance of hierarchical two-means is comparable to the traditionally used Ward's clustering. As the former is much more efficient in time and memory, our results suggest another less resource demanding alternative for annotating large spectral images.

  2. Pressure-modulation dynamic attenuated-total-reflectance (ATR) FT-IR spectroscopy

    Science.gov (United States)

    Marcott, C.; Story, G. M.; Noda, I.; Bibby, A.; Manning, C. J.

    1998-06-01

    A single-reflectance attenuated-total-reflectance (ATR) accessory with a diamond internal-reflection element was modified by the addition of a piezoelectric transducer. Initial dynamic pressure-modulation experiments have been performed in the sample compartment of a step-scanning FT-IR spectrometer. A sinusoidal pressure modulation applied to samples of isotactic polypropylene and linear low density polyethylene resulted in dynamic responses which appear to be similar to those observed in previous dynamic 2D IR experiments. Preliminary pressure-modulation dynamic ATR results are also reported for a styrene-butadiene-styrene triblock copolymer. The new method has the advantages that a much wider variety of sample types and geometries can be studied and less sample preparation is required. Dynamic 2D IR experiments carried out by ATR no longer require thin films of large area and sufficient strength to withstand the dynamic strain applied by a rheometer. The ability to obtain dynamic IR spectroscopic information from a wider variety of sample types and thicknesses would greatly expand the amount of useful information that could be extracted from normally complicated, highly overlapped IR spectra.

  3. Forensic Hair Differentiation Using Attenuated Total Reflection Fourier Transform Infrared (ATR FT-IR) Spectroscopy.

    Science.gov (United States)

    Manheim, Jeremy; Doty, Kyle C; McLaughlin, Gregory; Lednev, Igor K

    2016-07-01

    Hair and fibers are common forms of trace evidence found at crime scenes. The current methodology of microscopic examination of potential hair evidence is absent of statistical measures of performance, and examiner results for identification can be subjective. Here, attenuated total reflection (ATR) Fourier transform-infrared (FT-IR) spectroscopy was used to analyze synthetic fibers and natural hairs of human, cat, and dog origin. Chemometric analysis was used to differentiate hair spectra from the three different species, and to predict unknown hairs to their proper species class, with a high degree of certainty. A species-specific partial least squares discriminant analysis (PLSDA) model was constructed to discriminate human hair from cat and dog hairs. This model was successful in distinguishing between the three classes and, more importantly, all human samples were correctly predicted as human. An external validation resulted in zero false positive and false negative assignments for the human class. From a forensic perspective, this technique would be complementary to microscopic hair examination, and in no way replace it. As such, this methodology is able to provide a statistical measure of confidence to the identification of a sample of human, cat, and dog hair, which was called for in the 2009 National Academy of Sciences report. More importantly, this approach is non-destructive, rapid, can provide reliable results, and requires no sample preparation, making it of ample importance to the field of forensic science. © The Author(s) 2016.

  4. 3D FT-IR imaging spectroscopy of phase-separation in a poly(3-hydroxybutyrate)/poly(L-lactic acid) blend

    Science.gov (United States)

    Miriam Unger; Julia Sedlmair; Heinz W. Siesler; Carol Hirschmugl; Barbara Illman

    2014-01-01

    In the present study, 3D FT-IR spectroscopic imaging measurements were applied to study the phase separation of a poly(3-hydroxybutyrate) (PHB)/poly(L-lactic acid) (PLA) (50:50 wt.%) polymer blend film. While in 2D projection imaging the z-dependent information is overlapped, thereby complicating the analysis, FT-IR spectro-micro-tomography,...

  5. Characterization of soil organic matter by FT-IR spectroscopy and its relationship with chlorpyrifos sorption.

    Science.gov (United States)

    Parolo, María Eugenia; Savini, Mónica Claudia; Loewy, Ruth Miriam

    2017-07-01

    Sorption of non-ionic organic compounds to soil is usually expressed as the carbon-normalized partition coefficient (K OC ) assuming that the main factor that influences the amount sorbed is the organic carbon content (OC) of the soil. However, K OC can vary across a range of soils. The influence of certain soil characteristics on the chlorpyrifos K OC values variation for 12 representative soils of the Northpatagonian Argentinian region with different physicochemical properties was investigated for this study. The chlorpyrifos sorption coefficients normalized by the OC content were experimentally obtained using the batch equilibrium method; the K OC values ranged between 9000-20,000 L kg -1 . The soil characteristics assessed were pH, clay content and spectral data indicative of soil organic matter (SOM) quality measured by FT-IR on the whole soil. The bands considered in the spectroscopic analyses were those corresponding to the aliphatic components, 2947-2858 cm -1 (band A) and the hydrophilic components, 1647-1633 cm -1 (band B). A significant relationship was found (R 2  = 0.66) between chlorpyrifos sorption (K OC ) and the variables pH and A/B height band ratio. The correlation between the values predicted by the derived model and the experimental data was significant (r = 0.89 p chlorpyrifos sorption coefficient through the use of a simple, rapid, and environmentally-friendly measurement. K OC analysis in relation to soil properties represents a valuable contribution to the understanding of the attenuation phenomena of the organic contaminants off-site migration in the environment. Copyright © 2017 Elsevier Ltd. All rights reserved.

  6. Kinetics and evolved gas analysis for pyrolysis of food processing wastes using TGA/MS/FT-IR.

    Science.gov (United States)

    Özsin, Gamzenur; Pütün, Ayşe Eren

    2017-06-01

    The objective of this study was to identify the pyrolysis of different bio-waste produced by food processing industry in a comprehensible manner. For this purpose, pyrolysis behaviors of chestnut shells (CNS), cherry stones (CS) and grape seeds (GS) were investigated by thermogravimetric analysis (TGA) combined with a Fourier-transform infrared (FT-IR) spectrometer and a mass spectrometer (MS). In order to make available theoretical groundwork for biomass pyrolysis, activation energies were calculated with the help of four different model-free kinetic methods. The results are attributed to the complex reaction schemes which imply parallel, competitive and complex reactions during pyrolysis. During pyrolysis, the evolution of volatiles was also characterized by FT-IR and MS. The main evolved gases were determined as H 2 O, CO 2 and hydrocarbons such as CH 4 and temperature dependent profiles of the species were obtained. Copyright © 2017 Elsevier Ltd. All rights reserved.

  7. Some critical aspects of FT-IR, TGA, powder XRD, EDAX and SEM studies of calcium oxalate urinary calculi.

    Science.gov (United States)

    Joshi, Vimal S; Vasant, Sonal R; Bhatt, J G; Joshi, Mihir J

    2014-06-01

    Urinary calculi constitute one of the oldest afflictions of humans as well as animals, which are occurring globally. The calculi vary in shape, size and composition, which influence their clinical course. They are usually of the mixed-type with varying percentages of the ingredients. In medical management of urinary calculi, either the nature of calculi is to be known or the exact composition of calculi is required. In the present study, two selected calculi were recovered after surgery from two different patients for detailed examination and investigated by using Fourier-Transform infrared spectroscopy (FT-IR), thermo-gravimetric analysis (TGA), powder X-ray diffraction (XRD), scanning electron microscopy and energy dispersive analysis of X-rays (EDAX) techniques. The study demonstrated that the nature of urinary calculi and presence of major phase in mixed calculi could be identified by FT-IR, TGA and powder XRD, however, the exact content of various elements could be found by EDAX only.

  8. Identification of urushi coated films taken from ancient Buddha images by using PIXE, FT-IR, and organic elemental analysis

    International Nuclear Information System (INIS)

    Kagemori, N.; Umemura, K.; Yoshimura, T.; Inoue, M.; Kawai, S.; Yano, K.; Sera, K.; Futatsugawa, S.; Nakamura, Y.

    1999-01-01

    Six types of samples including urushi, urushi tree and black coating films taken from ancient Buddha images were examined by analyses of PIXE, organic element and FT-IR to identify with urushi or another material. Based on the results of three analytical experiments above mentioned, the coating materials aging over hundreds of years were identified with weathered urushi films mixed with other material. Further investigation may reveal the urushi coating techniques used in the past. (author)

  9. Geographic identification of Boletus mushrooms by data fusion of FT-IR and UV spectroscopies combined with multivariate statistical analysis

    Science.gov (United States)

    Yao, Sen; Li, Tao; Li, JieQing; Liu, HongGao; Wang, YuanZhong

    2018-06-01

    Boletus griseus and Boletus edulis are two well-known wild-grown edible mushrooms which have high nutrition, delicious flavor and high economic value distributing in Yunnan Province. In this study, a rapid method using Fourier transform infrared (FT-IR) and ultraviolet (UV) spectroscopies coupled with data fusion was established for the discrimination of Boletus mushrooms from seven different geographical origins with pattern recognition method. Initially, the spectra of 332 mushroom samples obtained from the two spectroscopic techniques were analyzed individually and then the classification performance based on data fusion strategy was investigated. Meanwhile, the latent variables (LVs) of FT-IR and UV spectra were extracted by partial least square discriminant analysis (PLS-DA) and two datasets were concatenated into a new matrix for data fusion. Then, the fusion matrix was further analyzed by support vector machine (SVM). Compared with single spectroscopic technique, data fusion strategy can improve the classification performance effectively. In particular, the accuracy of correct classification of SVM model in training and test sets were 99.10% and 100.00%, respectively. The results demonstrated that data fusion of FT-IR and UV spectra can provide higher synergic effect for the discrimination of different geographical origins of Boletus mushrooms, which may be benefit for further authentication and quality assessment of edible mushrooms.

  10. Validation of ATR FT-IR to identify polymers of plastic marine debris, including those ingested by marine organisms

    Science.gov (United States)

    Jung, Melissa R.; Horgen, F. David; Orski, Sara V.; Rodriguez, Viviana; Beers, Kathryn L.; Balazs, George H.; Jones, T. Todd; Work, Thierry M.; Brignac, Kayla C.; Royer, Sarah-Jeanne; Hyrenbach, David K.; Jensen, Brenda A.; Lynch, Jennifer M.

    2018-01-01

    Polymer identification of plastic marine debris can help identify its sources, degradation, and fate. We optimized and validated a fast, simple, and accessible technique, attenuated total reflectance Fourier transform infrared spectroscopy (ATR FT-IR), to identify polymers contained in plastic ingested by sea turtles. Spectra of consumer good items with known resin identification codes #1–6 and several #7 plastics were compared to standard and raw manufactured polymers. High temperature size exclusion chromatography measurements confirmed ATR FT-IR could differentiate these polymers. High-density (HDPE) and low-density polyethylene (LDPE) discrimination is challenging but a clear step-by-step guide is provided that identified 78% of ingested PE samples. The optimal cleaning methods consisted of wiping ingested pieces with water or cutting. Of 828 ingested plastics pieces from 50 Pacific sea turtles, 96% were identified by ATR FT-IR as HDPE, LDPE, unknown PE, polypropylene (PP), PE and PP mixtures, polystyrene, polyvinyl chloride, and nylon.

  11. Application of fourier-transform infrared (ft-ir) spectroscopy for determination of total phenolics of freeze dried lemon juices

    International Nuclear Information System (INIS)

    Sherazi, S.T.H.; Bhutto, A.A.; Mehesar, S.A.

    2017-01-01

    A cost effective and environmentally safe analytical method for rapid assessment of total phenolic content (TPC) in freeze dried lemon juice samples was developed using transmission Fourier-transform infrared spectroscopy (FT-IR) in conjunction with chemometric techniques. Two types of calibrations i.e. simple Beer's law and partial least square (PLS) were applied to investigate most accurate calibration model based on region from1420 to 1330 cm-1. The better analytical performance was obtained by PLS technique coefficient of determination (R2), root mean square error of calibration (RMSEC) with the value of 0.999 and 0.00864, respectively. The results of TPC in freeze dried lemon juice samples obtained by transmission FT-IR were compared with TPC observed by Folin-Ciocalteu (FC) assay and found to be comparable. Outcomes of the present study indicate that transmission FT-IR spectroscopic approach could be used as an alternative approach in place of Folin-Ciocalteu (FC) assay which is expensive and time-consuming conventional chemical methods for determination of the total phenolic content of lemon fruits. (author)

  12. The characterization of natural gemstones using non-invasive FT-IR spectroscopy: New data on tourmalines.

    Science.gov (United States)

    Mercurio, Mariano; Rossi, Manuela; Izzo, Francesco; Cappelletti, Piergiulio; Germinario, Chiara; Grifa, Celestino; Petrelli, Maurizio; Vergara, Alessandro; Langella, Alessio

    2018-02-01

    Fourteen samples of tourmaline from the Real Museo Mineralogico of Federico II University (Naples) have been characterized through multi-methodological investigations (EMPA-WDS, SEM-EDS, LA-ICP-MS, and FT-IR spectroscopy). The samples show different size, morphology and color, and are often associated with other minerals. Data on major and minor elements allowed to identify and classify tourmalines as follows: elbaites, tsilaisite, schorl, dravites, uvites and rossmanite. Non-invasive, non-destructive FT-IR and in-situ analyses were carried out on the same samples to validate this chemically-based identification and classification. The results of this research show that a complete characterization of this mineral species, usually time-consuming and expensive, can be successfully achieved through non-destructive FT-IR technique, thus representing a reliable tool for a fast classification extremely useful to plan further analytical strategies, as well as to support gemological appraisals. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Biochemical Monitoring of Spinal Cord Injury by FT-IR Spectroscopy—Effects of Therapeutic Alginate Implant in Rat Models

    Science.gov (United States)

    Uckermann, Ortrud; Sitoci-Ficici, Kerim H.; Later, Robert; Beiermeister, Rudolf; Doberenz, Falko; Gelinsky, Michael; Leipnitz, Elke; Schackert, Gabriele; Koch, Edmund; Sablinskas, Valdas; Steiner, Gerald; Kirsch, Matthias

    2015-01-01

    Spinal cord injury (SCI) induces complex biochemical changes, which result in inhibition of nervous tissue regeneration abilities. In this study, Fourier-transform infrared (FT-IR) spectroscopy was applied to assess the outcomes of implants made of a novel type of non-functionalized soft calcium alginate hydrogel in a rat model of spinal cord hemisection (n = 28). Using FT-IR spectroscopic imaging, we evaluated the stability of the implants and the effects on morphology and biochemistry of the injured tissue one and six months after injury. A semi-quantitative evaluation of the distribution of lipids and collagen showed that alginate significantly reduced injury-induced demyelination of the contralateral white matter and fibrotic scarring in the chronic state after SCI. The spectral information enabled to detect and localize the alginate hydrogel at the lesion site and proved its long-term persistence in vivo. These findings demonstrate a positive impact of alginate hydrogel on recovery after SCI and prove FT-IR spectroscopic imaging as alternative method to evaluate and optimize future SCI repair strategies. PMID:26559822

  14. Biochemical Monitoring of Spinal Cord Injury by FT-IR Spectroscopy--Effects of Therapeutic Alginate Implant in Rat Models.

    Directory of Open Access Journals (Sweden)

    Sandra Tamosaityte

    Full Text Available Spinal cord injury (SCI induces complex biochemical changes, which result in inhibition of nervous tissue regeneration abilities. In this study, Fourier-transform infrared (FT-IR spectroscopy was applied to assess the outcomes of implants made of a novel type of non-functionalized soft calcium alginate hydrogel in a rat model of spinal cord hemisection (n = 28. Using FT-IR spectroscopic imaging, we evaluated the stability of the implants and the effects on morphology and biochemistry of the injured tissue one and six months after injury. A semi-quantitative evaluation of the distribution of lipids and collagen showed that alginate significantly reduced injury-induced demyelination of the contralateral white matter and fibrotic scarring in the chronic state after SCI. The spectral information enabled to detect and localize the alginate hydrogel at the lesion site and proved its long-term persistence in vivo. These findings demonstrate a positive impact of alginate hydrogel on recovery after SCI and prove FT-IR spectroscopic imaging as alternative method to evaluate and optimize future SCI repair strategies.

  15. Forensic Drug Identification, Confirmation, and Quantification Using Fully Integrated Gas Chromatography with Fourier Transform Infrared and Mass Spectrometric Detection (GC-FT-IR-MS).

    Science.gov (United States)

    Lanzarotta, Adam; Lorenz, Lisa; Voelker, Sarah; Falconer, Travis M; Batson, JaCinta S

    2018-05-01

    This manuscript is a continuation of a recent study that described the use of fully integrated gas chromatography with direct deposition Fourier transform infrared detection and mass spectrometric detection (GC-FT-IR-MS) to identify and confirm the presence of sibutramine and AB-FUBINACA. The purpose of the current study was to employ the GC-FT-IR portion of the same instrument to quantify these compounds, thereby demonstrating the ability to identify, confirm, and quantify drug substances using a single GC-FT-IR-MS unit. The performance of the instrument was evaluated by comparing quantitative analytical figures of merit to those measured using an established, widely employed method for quantifying drug substances, high performance liquid chromatography with ultraviolet detection (HPLC-UV). The results demonstrated that GC-FT-IR was outperformed by HPLC-UV with regard to sensitivity, precision, and linear dynamic range (LDR). However, sibutramine and AB-FUBINACA concentrations measured using GC-FT-IR were not significantly different at the 95% confidence interval compared to those measured using HPLC-UV, which demonstrates promise for using GC-FT-IR as a semi-quantitative tool at the very least. The most significant advantage of GC-FT-IR compared to HPLC-UV is selectivity; a higher level of confidence regarding the identity of the analyte being quantified is achieved using GC-FT-IR. Additional advantages of using a single GC-FT-IR-MS instrument for identification, confirmation, and quantification are efficiency, increased sample throughput, decreased consumption of laboratory resources (solvents, chemicals, consumables, etc.), and thus cost.

  16. Caracterização por FT-IR da superfície de borracha EPDM tratada via plasma por micro-ondas FT-IR characterization of EPDM rubber surface treated by microwave plasma

    Directory of Open Access Journals (Sweden)

    Renata P. dos Santos

    2012-01-01

    Full Text Available A superfície de uma borracha de etileno-propileno-dieno (EPDM vulcanizada foi modificada via plasma por microondas, com gases Ar, Ar/O2, N2/O2 e N2/H2, tendo como objetivo melhorar as propriedades adesivas da superfície. A técnica FT-IR/UATR foi escolhida para caracterizar as superfícies após tratamento, pois apresentou menor interferência dos ingredientes da formulação da EPDM, dentre as técnicas analisadas (ATR/KRS-5 e Ge. Grupos oxigenados foram inseridos na superfície da amostra tratada, mesmo quando não foi utilizado o oxigênio, pois estes grupos foram formados quando a superfície ativada foi exposta à atmosfera. Já em tratamentos contendo N2, grupos oxigenados e possíveis grupos nitrogenados foram identificados por FT-IR. Redução nos valores do ângulo de contato, aumento no trabalho de adesão e aumento no ensaio de resistência ao descascamento (EPDM × Poliuretano foram observados após tratamento com Ar e N2/H2, resultando em melhora nas propriedades adesivas da superfície tratada.The surface of a vulcanized ethylene propylene diene monomer (EPDM rubber was modified by microwave plasma in Ar, Ar/O2, N2/O2 and N2/H2 in order to improve the adhesion properties. Surface modification was characterized by FT-IR/UATR, because this technique showed smaller interference of ingredients of EPDM formulation in comparison with other techniques used (ATR KRS-5 and Ge. Oxygenated groups were introduced in the EPDM surface after treatment, even in treatments without oxygen. Theses groups were formed when the activated surface was exposed to the atmosphere. In treatments with nitrogen, oxygenated and possible nitrogenated groups were identified by FT-IR. Reduction in the contact angle, increase in the work of adhesion and increase in the peel strength (EPDM × Polyurethane were observed after treatment with Ar and N2/H2, resulting in improved adhesion properties of the modified surface.

  17. Differentiation of Candida albicans, Candida glabrata, and Candida krusei by FT-IR and chemometrics by CHROMagar™ Candida.

    Science.gov (United States)

    Wohlmeister, Denise; Vianna, Débora Renz Barreto; Helfer, Virginia Etges; Calil, Luciane Noal; Buffon, Andréia; Fuentefria, Alexandre Meneghello; Corbellini, Valeriano Antonio; Pilger, Diogo André

    2017-10-01

    Pathogenic Candida species are detected in clinical infections. CHROMagar™ is a phenotypical method used to identify Candida species, although it has limitations, which indicates the need for more sensitive and specific techniques. Infrared Spectroscopy (FT-IR) is an analytical vibrational technique used to identify patterns of metabolic fingerprint of biological matrixes, particularly whole microbial cell systems as Candida sp. in association of classificatory chemometrics algorithms. On the other hand, Soft Independent Modeling by Class Analogy (SIMCA) is one of the typical algorithms still little employed in microbiological classification. This study demonstrates the applicability of the FT-IR-technique by specular reflectance associated with SIMCA to discriminate Candida species isolated from vaginal discharges and grown on CHROMagar™. The differences in spectra of C. albicans, C. glabrata and C. krusei were suitable for use in the discrimination of these species, which was observed by PCA. Then, a SIMCA model was constructed with standard samples of three species and using the spectral region of 1792-1561cm -1 . All samples (n=48) were properly classified based on the chromogenic method using CHROMagar™ Candida. In total, 93.4% (n=45) of the samples were correctly and unambiguously classified (Class I). Two samples of C. albicans were classified correctly, though these could have been C. glabrata (Class II). Also, one C. glabrata sample could have been classified as C. krusei (Class II). Concerning these three samples, one triplicate of each was included in Class II and two in Class I. Therefore, FT-IR associated with SIMCA can be used to identify samples of C. albicans, C. glabrata, and C. krusei grown in CHROMagar™ Candida aiming to improve clinical applications of this technique. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. FT-IR spectroscopy: A powerful tool for studying the inter- and intraspecific biodiversity of cultivable non-Saccharomyces yeasts isolated from grape must.

    Science.gov (United States)

    Grangeteau, Cédric; Gerhards, Daniel; Terrat, Sebastien; Dequiedt, Samuel; Alexandre, Hervé; Guilloux-Benatier, Michèle; von Wallbrunn, Christian; Rousseaux, Sandrine

    2016-02-01

    The efficiency of the FT-IR technique for studying the inter- and intra biodiversity of cultivable non-Saccharomyces yeasts (NS) present in different must samples was examined. In first, the capacity of the technique FT-IR to study the global diversity of a given sample was compared to the pyrosequencing method, used as a reference technique. Seven different genera (Aureobasidium, Candida, Cryptococcus, Hanseniaspora, Issatchenkia, Metschnikowia and Pichia) were identified by FT-IR and also by pyrosequencing. Thirty-eight other genera were identified by pyrosequencing, but together they represented less than 6% of the average total population of 6 musts. Among the species identified, some of them present organoleptic potentials in winemaking, particularly Starmerella bacillaris (synonym Candidazemplinina). So in a second time, we evaluated the capacity of the FT-IR technique to discriminate the isolates of this species because few techniques were able to study intraspecific NS yeast biodiversity. The results obtained were validated by using a classic method as ITS sequencing. Biodiversity at strain level was high: 19 different strains were identified from 58 isolates. So, FT-IR spectroscopy seems to be an accurate and reliable method for identifying major genera present in the musts. The two biggest advantages of the FT-IR are the capacity to characterize intraspecific biodiversity of non-Saccharomyces yeasts and the possibility to discriminate a lot of strains. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Matrix-isolation and solid state low temperature FT-IR study of 2,3-butanedione (diacetyl)

    OpenAIRE

    Gómez-Zavaglia, Andrea; Fausto, R.

    2003-01-01

    2,3-Butanedione (diacetyl) was studied by matrix-isolation and low temperature solid state FT-IR spectroscopy, supported by molecular orbital calculations undertaken at the DFT(B3LYP) and MP2 levels of theory with the 6-311++G(d,p) basis set. Both in the crystalline phase and in the matrices, the compound exists in the C2h symmetry trans conformation (O=C-C=O dihedral angle of 180°). This form corresponds to the single conformational state predicted by the theoretical calculations for the com...

  20. Conformational study of sarcosine as probed by matrix-isolation FT-IR spectroscopy and molecular orbital calculations

    OpenAIRE

    Gómez-Zavaglia, Andrea; Fausto, R.

    2003-01-01

    Sarcosine (N-methylglycine) has been studied by matrix-isolation FT-IR spectroscopy and molecular orbital calculations undertaken at the DFT/B3LYP and MP2 levels of theory with the 6-311++G(d, p) and 6-31++G(d, p) basis set, respectively. Eleven different conformers were located in the potential energy surface (PES) of sarcosine, with the ASC conformer being the ground conformational state. This form is analogous to the glycine most stable conformer and is characterized by a NH...O= intramole...

  1. Avaliação do uso de técnicas PIR-G/FT-IR para caracterização de elastômeros Evaluation of PIR-G/FT-IR techniques for characterization of elastomers

    Directory of Open Access Journals (Sweden)

    Natália B. Sanches

    2006-01-01

    Full Text Available A técnica de pirólise gasosa, em bico de Bunsen, para análise por espectroscopia no infravermelho com transformada de Fourier (PIR-G/FT-IR foi aplicada a diferentes borrachas, incluindo algumas misturas. Foi observado que é possível diferenciar os tipos de elastômeros por meio de análise de produtos gasosos de pirólise, inclusive aqueles que apresentam espectros IR de pirolisados líquidos similares, como é o caso de CIIR e BIIR, NR/SBR e EPDM/SBR, SBR/BR e SBR.Pyrolysis and infrared spectroscopy (PIR-G/FT-IR were used for investigating gaseous products of rubber. The results show that this method was suitable to identify different elastomers and elastomer blends, including rubbers that present similar IR spectra of pyrolysed liquid products such as CIIR and BIIR, NR/SBR and EPDM/SBR, SBR/BR and SBR.

  2. Synchrotron FT-IR analyses of microstructured biomineral domains: Hints to the biomineralization processes in freshwater cultured pearls.

    Science.gov (United States)

    Soldati, A. L.; Vicente-Vilas, V.; Gasharova, B.; Jacob, D. E.

    2009-04-01

    Recent investigations in freshwater cultured pearls (bio-carbonate) by micro-Raman spectroscopy (Wehrmeister et al., 2008; Soldati et al., 2008), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) imaging (Jacob et al., 2008) show that the pearl biomineralisation starts with a self assembling process in which an existing gel matrix of amorphous calcium carbonate (ACC) and organic substances reorganizes and conglomerates in small domains; these conglomerates then form prisms and mature nacreous tablets of aragonite or vaterite. Raman spectroscopy shows that the calcium carbonate polymorphs have decreasing luminescence in the order ACC>Vaterite>Aragonite, coinciding with decreasing quantities of S and P (related to the organic matrix) measured by Laser Ablation Inductively Coupled Plasma Mass Spectroscopy (LA-ICP-MS) and Electron Probe Micro Analyzer (EPMA). Although little is known about the process of transformation of the ACC gel into vaterite and aragonite, it is speculated that this probably involves dehydration and change of the accompanying organic matrix. This is also supported by our laboratory FT-IR analysis. However, due to the small size of the areas of ACC (about 10 ?m) and the biogenic crystals an in-situ high spatially resolved IR-method is needed to record how the water content and organic matrix change in the biomineralisation sequence, to understand which processes take place in the self-organization. The beamline IR-1 at the ANKA synchrotron source (Karlsruhe, Germany) was used for this experiment. Freshwater cultured pearls from China cultured in Hyriopsis cumingii mussels by tissue nucleation methods (so-called beadless pearls) as well as by bead implantation methods (aragonite nucleus) were studied. The pearls were cut in half with a diamond-plated saw and polished with diamond paste on a copper plate. Micro-Raman spectroscopy maps (Department of Geosciences, at the Johannes Gutenberg-University, Mainz) were generated

  3. Activation and thermodynamic parameter study of the heteronuclear C=O···H-N hydrogen bonding of diphenylurethane isomeric structures by FT-IR spectroscopy using the regularized inversion of an eigenvalue problem.

    Science.gov (United States)

    Spegazzini, Nicolas; Siesler, Heinz W; Ozaki, Yukihiro

    2012-08-02

    The doublet of the ν(C=O) carbonyl band in isomeric urethane systems has been extensively discussed in qualitative terms on the basis of FT-IR spectroscopy of the macromolecular structures. Recently, a reaction extent model was proposed as an inverse kinetic problem for the synthesis of diphenylurethane for which hydrogen-bonded and non-hydrogen-bonded C=O functionalities were identified. In this article, the heteronuclear C=O···H-N hydrogen bonding in the isomeric structure of diphenylurethane synthesized from phenylisocyanate and phenol was investigated via FT-IR spectroscopy, using a methodology of regularization for the inverse reaction extent model through an eigenvalue problem. The kinetic and thermodynamic parameters of this system were derived directly from the spectroscopic data. The activation and thermodynamic parameters of the isomeric structures of diphenylurethane linked through a hydrogen bonding equilibrium were studied. The study determined the enthalpy (ΔH = 15.25 kJ/mol), entropy (TΔS = 14.61 kJ/mol), and free energy (ΔG = 0.6 kJ/mol) of heteronuclear C=O···H-N hydrogen bonding by FT-IR spectroscopy through direct calculation from the differences in the kinetic parameters (δΔ(‡)H, -TδΔ(‡)S, and δΔ(‡)G) at equilibrium in the chemical reaction system. The parameters obtained in this study may contribute toward a better understanding of the properties of, and interactions in, supramolecular systems, such as the switching behavior of hydrogen bonding.

  4. Identification and Quantification of Microplastics in Wastewater Using Focal Plane Array-Based Reflectance Micro-FT-IR Imaging.

    Science.gov (United States)

    Tagg, Alexander S; Sapp, Melanie; Harrison, Jesse P; Ojeda, Jesús J

    2015-06-16

    Microplastics (microplastics in these matrices has not been investigated. Although efficient methods for the analysis of microplastics in sediment samples and marine organisms have been published, no methods have been developed for detecting these pollutants within organic-rich wastewater samples. In addition, there is no standardized method for analyzing microplastics isolated from environmental samples. In many cases, part of the identification protocol relies on visual selection before analysis, which is open to bias. In order to address this, a new method for the analysis of microplastics in wastewater was developed. A pretreatment step using 30% hydrogen peroxide (H2O2) was employed to remove biogenic material, and focal plane array (FPA)-based reflectance micro-Fourier-transform (FT-IR) imaging was shown to successfully image and identify different microplastic types (polyethylene, polypropylene, nylon-6, polyvinyl chloride, polystyrene). Microplastic-spiked wastewater samples were used to validate the methodology, resulting in a robust protocol which was nonselective and reproducible (the overall success identification rate was 98.33%). The use of FPA-based micro-FT-IR spectroscopy also provides a considerable reduction in analysis time compared with previous methods, since samples that could take several days to be mapped using a single-element detector can now be imaged in less than 9 h (circular filter with a diameter of 47 mm). This method for identifying and quantifying microplastics in wastewater is likely to provide an essential tool for further research into the pathways by which microplastics enter the environment.

  5. FT-IR and thermoluminescence investigation of P2O5-BaO-K2O glass system

    Science.gov (United States)

    Ivascu, C.; Timar-Gabor, A.; Cozar, O.

    2013-11-01

    The 0.5P2O5ṡxBaOṡ(0.5-x)K2O glass system (0≤x≤0.5mol%) is investigated by FT-IR and thermoluminescence as a possible dosimetic material. FT-IR spectra show structural network modifications with the composition variations of the studied glasses. The predominant absorption bands are characterized by two broad peaks near 500 cm-1, two weak peaks around 740 cm-1 and three peaks in the 900-1270 cm-1 region. The shift in the position of the band assigned to asymmetric stretching of PO2- group, υas(PO2-) modes from ˜1100 cm-1 to 1085 cm-1 and the decrease in its relative intensity with the increasing of K2O content shows a network modifier role of this oxide.. Luminescence investigations show that by adding modifier oxides in the phosphate glass a dose dependent TL signals result upon irradiation. Thus P2O5-BaO-K2O glass system is a possible candidate material for dosimetry in the dose 0 - 50 Gy range.

  6. Quantum-chemical, NMR, FT IR, and ESI MS studies of complexes of colchicine with Zn(II).

    Science.gov (United States)

    Jankowski, Wojciech; Kurek, Joanna; Barczyński, Piotr; Hoffmann, Marcin

    2017-04-01

    Colchicine is a tropolone alkaloid from Colchicinum autumnale. It shows antifibrotic, antimitotic, and anti-inflammatory activities, and is used to treat gout and Mediterranean fever. In this work, complexes of colchicine with zinc(II) nitrate were synthesized and investigated using DFT, 1 H and 13 C NMR, FT IR, and ESI MS. The counterpoise-corrected and uncorrected interaction energies of these complexes were calculated. We also calculated their 1 H, 13 C NMR, and IR spectra and compared them with the corresponding experimentally obtained data. According to the ESI MS mass spectra, colchicine forms stable complexes with zinc(II) nitrate that have various stoichiometries: 2:1, 1:1:1, and 2:1:1 with respect to colchichine, Zn(II), and nitrate ion. All of the complexes were investigated using the quantum theory of atoms in molecules (QTAIM). The calculated and the measured spectra showed differences before and after the complexation process. Calculated electron densities and bond critical points indicated the presence of bonds between the ligands and the central cation in the investigated complexes that satisfied the quantum theory of atoms in molecules. Graphical Abstract DFT, NMR, FT IR, ESI MS, QTAIM and puckering studies of complexes of colchicine with Zn(II).

  7. FT-IR X-ray diffraction and porosimetry studies of archaeologic artifacts recently excavated from Rajakkamangalam in Tamilnadu

    International Nuclear Information System (INIS)

    Babu Suresh; Velraj, Gothandapani

    2011-01-01

    In the present study, fragmented pottery sample were collected from the recently excavated archaeologic site named Rajakkamangalam, India. The samples were collected at different depths. The samples were subjected to FT-IR, X-ray diffraction and also porosimetry study was done, The spectroscopic method Fourier Transform Infrared Spectroscopy (FT-IR) has been employed to find the mineralogical composition of the potteries. And the complementary technique to find the clay minerals present using XRD. The major primary minerals present in the samples are Kaolinite and the secondary mineral present is quartz and the accessory minerals present in the sample are hematite and magnetite. In addition to the used mineral the orthoclase and orthopyroxene are present in the sample of interest. The firing temperature of the samples at the time of manufacturing is also estimated from apparent porosity of the samples. The percentage of the potteries lies in the range of porosity is 17-42 percentages. The results obtained from Porosimetry techniques on pottery shreds provide information of the firing temperature might have been fired below 1000 deg C at the time of manufacturing the potteries. (author)

  8. Effects of curing conditions on the structure of sodium carboxymethyl starch/mineral matrix system: FT-IR investigation.

    Science.gov (United States)

    Kaczmarska, Karolina; Grabowska, Beata; Bobrowski, Artur; Cukrowicz, Sylwia

    2018-04-24

    Strength properties of the microwave cured molding sands containing binders in a form of the aqueous solution of sodium carboxymethyl starch (CMS-Na) are higher than the same molding composition cured by conventional heating. Finding the reason of this effect was the main purpose in this study. Structural changes caused by both physical curing methods of molding sands systems containing mineral matrix (silica sand) and polymer water-soluble binder (CMS-Na) were compared. It was shown, by means of the FT-IR spectroscopic studies, that the activation of the polar groups in the polymer macromolecules structure as well as silanol groups on the mineral matrix surfaces was occurred in the microwave radiation. Binding process in microwave-cured samples was an effect of formation the hydrogen bonds network between hydroxyl and/or carbonyl groups present in polymer and silanol groups present in mineral matrix. FT-IR studies of structural changes in conventional and microwave cured samples confirm that participation of hydrogen bonds is greater after microwave curing than conventional heating. Copyright © 2018 Elsevier B.V. All rights reserved.

  9. ATR FT-IR spectroscopy on Vmh2 hydrophobin self-assembled layers for Teflon membrane bio-functionalization

    International Nuclear Information System (INIS)

    Portaccio, M.; Gravagnuolo, A.M.; Longobardi, S.; Giardina, P.; Rea, I.; De Stefano, L.; Cammarota, M.; Lepore, M.

    2015-01-01

    Graphical abstract: - Highlights: • Hydrophobin self-assembled layers on Teflon in different preparation conditions were investigated. • ATR collection data geometry allowed samples examination without any particular preparation. • Amide content, lipid/amide and carbohydrate/amide ratios of the protein layer were estimated. • Secondary structure of protein was determined for the examined samples. • FT-IR demonstrated to be of extreme relevance in monitoring hydrophobin self-assembled layers preparation. - Abstract: Surface functionalization by layers of hydrophobins, amphiphilic proteins produced by fungi offers a promising and green strategy for fabrication of biomedical and bioanalytical devices. The layering process of the Vmh2 hydrophobin from Pleurotus ostreatus on Teflon membrane has been investigated by Attenuated Total Reflection Fourier Transform Infrared (ATR FT-IR) spectroscopy. In particular, protein layers obtained with hydrophobin purified with two different procedures and in various coating conditions have been examined. The layers have been characterized by quantifying the amide I and amide II band area together with the lipid/amide ratio and carbohydrate/amide ratio. This characterization can be very useful in evaluating the best purification strategy and coating conditions. Moreover the analysis of the secondary structure of the layered protein using the deconvolution procedure of amide I band indicate the prevalent contribution from β-sheet state. The results inferred by infrared spectroscopy have been also confirmed by scanning electron microscopy imaging

  10. Structural investigations on some cadmium-borotellurate glasses using ultrasonic, FT-IR and X-ray techniques

    Energy Technology Data Exchange (ETDEWEB)

    Gaafar, M.S., E-mail: m.gaafar@mu.edu.sa [Physics Department, College of Sciences, Majmaah University (Saudi Arabia); Ultrasonic Laboratory, National Institute for Standards, Tersa Str., P.O. Box 136, El-Haram, El-Giza 12211 (Egypt); Shaarany, I. [Physics Department, College of Sciences, Majmaah University (Saudi Arabia); Physics Department, Faculty of Science, Suez Canal University, Ismailia (Egypt); Alharbi, T. [Physics Department, College of Sciences, Majmaah University (Saudi Arabia)

    2014-12-15

    Highlights: • 50B{sub 2}O{sub 3}–(50 – x)TeO{sub 2}–xCdO glass system has been prepared by melt quenching technique. • Both sound velocities decrease with increase in x. • Studies on the structure of these glasses, have revealed that Cd{sup 2+} ions are incorporated in the form of CdO{sub 6}. - Abstract: Glasses in the system 50B{sub 2}O{sub 3}–(50 − x)TeO{sub 2}–xCdO with different CdO contents (0, 10, 20, 30, 40 and 50 mol%), have been prepared by melt quenching technique. Elastic properties, X-ray and FT-IR spectroscopic studies have been employed to study the role of CdO on the structure of the investigated glass system. Elastic properties and Debye temperature have been investigated using sound wave velocity measurements at 4 MHz at room temperature. The results showed that the density increase and the molar volume decrease while both sound velocities decrease with increase in x. Elastic properties, FT-IR and X-ray diffraction studies on the network structure of these glass structures, have revealed that Cd{sup 2+} ions are incorporated in the form of CdO{sub 6}, decreasing the molar volume and compensate for the decrease in the average coordination number of tellurium atoms which was the reason for the increase in elastic moduli.

  11. ATR FT-IR spectroscopy on Vmh2 hydrophobin self-assembled layers for Teflon membrane bio-functionalization

    Energy Technology Data Exchange (ETDEWEB)

    Portaccio, M., E-mail: marianna.portaccio@unina2.it [Dipartimento di Medicina Sperimentale – Seconda Università di Napoli, Via S.M. di Costantinopoli, 16-80134 Napoli (Italy); Gravagnuolo, A.M., E-mail: alfredomaria.gravagnuolo@unina.it [Dipartimento di Scienze Chimiche, Università “Federico II”, Via Cintia, 21- 80126 Napoli (Italy); Longobardi, S., E-mail: sara.longobardi@unina.it [Dipartimento di Scienze Chimiche, Università “Federico II”, Via Cintia, 21- 80126 Napoli (Italy); Giardina, P., E-mail: paola.giardina@unina.it [Dipartimento di Scienze Chimiche, Università “Federico II”, Via Cintia, 21- 80126 Napoli (Italy); Rea, I., E-mail: ilaria.rea@na.imm.cnr.it [Institute for Microelectronics and Microsystems, CNR, Via P. Castellino, 111-80131 Napoli (Italy); De Stefano, L., E-mail: luca.destefano@na.imm.cnr.it [Institute for Microelectronics and Microsystems, CNR, Via P. Castellino, 111-80131 Napoli (Italy); Cammarota, M., E-mail: marcella.cammarota@unina2.it [Dipartimento di Medicina Sperimentale – Seconda Università di Napoli, Via S.M. di Costantinopoli, 16-80134 Napoli (Italy); Lepore, M., E-mail: maria.lepore@unina2.it [Dipartimento di Medicina Sperimentale – Seconda Università di Napoli, Via S.M. di Costantinopoli, 16-80134 Napoli (Italy)

    2015-10-01

    Graphical abstract: - Highlights: • Hydrophobin self-assembled layers on Teflon in different preparation conditions were investigated. • ATR collection data geometry allowed samples examination without any particular preparation. • Amide content, lipid/amide and carbohydrate/amide ratios of the protein layer were estimated. • Secondary structure of protein was determined for the examined samples. • FT-IR demonstrated to be of extreme relevance in monitoring hydrophobin self-assembled layers preparation. - Abstract: Surface functionalization by layers of hydrophobins, amphiphilic proteins produced by fungi offers a promising and green strategy for fabrication of biomedical and bioanalytical devices. The layering process of the Vmh2 hydrophobin from Pleurotus ostreatus on Teflon membrane has been investigated by Attenuated Total Reflection Fourier Transform Infrared (ATR FT-IR) spectroscopy. In particular, protein layers obtained with hydrophobin purified with two different procedures and in various coating conditions have been examined. The layers have been characterized by quantifying the amide I and amide II band area together with the lipid/amide ratio and carbohydrate/amide ratio. This characterization can be very useful in evaluating the best purification strategy and coating conditions. Moreover the analysis of the secondary structure of the layered protein using the deconvolution procedure of amide I band indicate the prevalent contribution from β-sheet state. The results inferred by infrared spectroscopy have been also confirmed by scanning electron microscopy imaging.

  12. Evaluation of turmeric powder adulterated with metanil yellow using FT-Raman and FT-IR spectroscopy

    Science.gov (United States)

    Turmeric powder (Curcuma longa L.) is valued both for its medicinal properties and for its popular culinary use such as being a component in curry powder. Due to its high demand in international trade, turmeric powder has been subject to economically driven, hazardous chemical adulteration. This stu...

  13. Structure and vibrational spectra of melaminium bis(trifluoroacetate) trihydrate: FT-IR, FT-Raman and quantum chemical calculations

    Science.gov (United States)

    Sangeetha, V.; Govindarajan, M.; Kanagathara, N.; Marchewka, M. K.; Gunasekaran, S.; Anbalagan, G.

    Melaminium bis(trifluoroacetate) trihydrate (MTFA), an organic material has been synthesized and single crystals of MTFA have been grown by the slow solvent evaporation method at room temperature. X-ray powder diffraction analysis confirms that MTFA crystal belongs to the monoclinic system with space group P2/c. The molecular geometry, vibrational frequencies and intensity of the vibrational bands have been interpreted with the aid of structure optimization based on density functional theory (DFT) B3LYP method with 6-311G(d,p) and 6-311++G(d,p) basis sets. The X-ray diffraction data have been compared with the data of optimized molecular structure. The theoretical results show that the crystal structure can be reproduced by optimized geometry and the vibrational frequencies show good agreement with the experimental values. The nuclear magnetic resonance (NMR) chemical shift of the molecule has been calculated by the gauge independent atomic orbital (GIAO) method and compared with experimental results. HOMO-LUMO, and other related molecular and electronic properties are calculated. The Mulliken and NBO charges have also been calculated and interpreted.

  14. Application of Fourier-transform infrared (FT-IR) spectroscopy for simple and easy determination of chylomicron-triglyceride and very low density lipoprotein-triglyceride.

    Science.gov (United States)

    Sato, Kenichi; Seimiya, Masanori; Kodera, Yoshio; Kitamura, Akihide; Nomura, Fumio

    2010-02-01

    Fourier-transform infrared (FT-IR) spectroscopy is a simple and reagent-free physicochemical analysis method, and is a potential alternative to more time-consuming and labor-intensive procedures. In this study, we aimed to use FT-IR spectroscopy to determine serum concentrations of chylomicron-triglyceride (TG) and very low density lipoprotein (VLDL)-TG. We analyzed a chylomicron fraction and VLDL fraction, which had been obtained by ultracentrifugation, to search for wavelengths to designate to each fraction. Then, partial least square (PLS) calibrations were developed using a training set of samples, for which TG concentrations had been determined by conventional procedures. Validation was conducted with another set of samples using the PLS model to predict serum TG concentrations on the basis of the samples' IR spectra. We analyzed a total of 150 samples. Serum concentrations of chylomicron-TG and VLDL-TG estimated by FT-IR spectroscopy agreed well with those obtained by the reference method (r=0.97 for both lipoprotein fractions). FT-IR spectrometric analysis required 15mul of serum and was completed within 1min. Serum chylomicron-TG and VLDL-TG concentrations can be determined with FT-IR spectroscopy. This rapid and simple test may have a great impact on the management of patients with dyslipidemia. Copyright 2009. Published by Elsevier B.V.

  15. Using synchrotron-based FT-IR microspectroscopy to study erucamide migration in 50-micron-thick bilayer linear low-density polyethylene and polyolefin plastomer films.

    Science.gov (United States)

    Sankhe, Shilpa Y; Hirt, Douglas E

    2003-01-01

    The diffusion of additives in thick (approximately 500 microns) single layer and multilayer films has been characterized using FT-IR microspectroscopy. The objective of this research was to investigate additive migration and concentration profiles in coextruded multilayer films of industrially relevant thicknesses. In particular, the investigation focused on the migration of an erucamide slip agent in 50-micron-thick coextruded bilayer films of linear low-density polyethylene (LLDPE) and a polyolefin plastomer (POP). Erucamide concentration profiles were successfully mapped using synchrotron-based FT-IR microspectroscopy. The synchrotron radiation helped to achieve a higher spatial resolution for the thin films. Meticulous sample preparation was needed to map the thin film samples. Results with FT-IR microspectroscopy showed that the additive-concentration profiles were relatively uniform across the multilayer-film thickness irrespective of the intended initial additive distribution. For example, a bilayer planned for 1 wt % erucamide in an LLDPE layer and no erucamide in a POP layer showed significant additive migration into the POP layer at the extrusion rates used. FT-IR microspectroscopy results also showed that more erucamide migrated to the surface of a POP layer than an LLDPE layer. Attenuated total reflectance (ATR) FT-IR spectroscopy was used to confirm the time-dependent increase of erucamide surface concentration and that the increase was more pronounced at the surface of the POP layers.

  16. THE SULFONATION STUDY OF REACTION MECHANISM ON PAPAVERINE ALKALOID BY GC-MS AND FT-IR

    Directory of Open Access Journals (Sweden)

    I Made Sudarma

    2010-06-01

    Full Text Available The aim of this research was to prove theoretical mechanism reaction on the sulfonation of papaverine alkaloid and the result could be used as a reference on the transformation of these alkaloid to the other derivatives. Theoriticaly sulfonation of papaverine (1 by HO-SO2Cl could produced papaverine sulfonyl chloride (1a. The formation of this product was analyzed by analytical thin layer chromatography GC-MS, and FT-IR. These analysis showed the formation of product (1a more favorable than the other. Tlc showed product (1a less polar than papaverine, and supported by GC-MS and infrared which showed molecular ion at m/z 412 due to the presence of -SO2Cl and vibration at 1153,4 dan 1265,2 Cm-1 due to absorption of sulfonyl group.   Keywords: reaction mechanism, sulfonation, papaverine alkaloid.

  17. Differentiation of Body Fluid Stains on Fabrics Using External Reflection Fourier Transform Infrared Spectroscopy (FT-IR) and Chemometrics.

    Science.gov (United States)

    Zapata, Félix; de la Ossa, Ma Ángeles Fernández; García-Ruiz, Carmen

    2016-04-01

    Body fluids are evidence of great forensic interest due to the DNA extracted from them, which allows genetic identification of people. This study focuses on the discrimination among semen, vaginal fluid, and urine stains (main fluids in sexual crimes) placed on different colored cotton fabrics by external reflection Fourier transform infrared spectroscopy (FT-IR) combined with chemometrics. Semen-vaginal fluid mixtures and potential false positive substances commonly found in daily life such as soaps, milk, juices, and lotions were also studied. Results demonstrated that the IR spectral signature obtained for each body fluid allowed its identification and the correct classification of unknown stains by means of principal component analysis (PCA) and soft independent modeling of class analogy (SIMCA). Interestingly, results proved that these IR spectra did not show any bands due to the color of the fabric and no substance of those present in daily life which were analyzed, provided a false positive. © The Author(s) 2016.

  18. Lead (II) biosorption equilibrium and characterization through FT-IR and SEM-EDAX crosslinked pectin from orange peels

    International Nuclear Information System (INIS)

    Garcia Villegas, Victor R.; Ale Borja, Neptali; Guzman Lezama, Enrique G.; Maldonado Garcia, Holger J.; Yipmantin Ojeda, Andrea G.

    2013-01-01

    Pectic material extracted from orange peels was previously cross-linked to diminish hydration and swelling capacity when pectin is found in aqueous solution medium. Degree of metoxilation (DM), galacturonic acid anhydrous (% AGA) and pKa determination allowed characterizing biosorbent. Maximum sorption capacity was obtained at pH between 4.5 and 5.5. For data processing and statistical treatment informatics Orign 6.0 version program was used. Data from biosorption equilibrium had a better fit on Langmuir sorption equation model, obtaining q max = 186 mg/g as a maximum adsorption capacity. Fourier transform infrared spectroscopy analysis (FT-IR) allowed recognizing characteristic functional groups presents as well as biomass modifications. Biosorbent surface morphologic was studied by scanning electron microscope (SEM) and elemental composition biomass before biosorption process was obtained through Energy-dispersive X-ray spectroscopy (EDAX). (author)

  19. A Simple Approach to Distinguish Classic and Formaldehyde-Free Tannin Based Rigid Foams by ATR FT-IR

    Directory of Open Access Journals (Sweden)

    Gianluca Tondi

    2015-01-01

    Full Text Available Tannin based rigid foams (TBRFs have been produced with formaldehyde since 1994. Only recently several methods have been developed in order to produce these foams without using formaldehyde. TBRFs with and without formaldehyde are visually indistinguishable; therefore a method for determining the differences between these foams had to be found. The attenuated total reflectance infrared spectroscopy (ATR FT-IR investigation of the TBRFs presented in this paper allowed discrimination between the formaldehyde-containing (classic and formaldehyde-free TBRFs. The spectra of the formaldehyde-free TBRFs, indeed, present decreased band intensity related to the C–O stretching vibration of (i the methylol groups and (ii the furanic rings. This evidence served to prove the chemical difference between the two TBRFs and explained the slightly higher mechanical properties measured for the classic TBRFs.

  20. In vivo skin leptin modulation after 14 MeV neutron irradiation: a molecular and FT-IR spectroscopic study

    Energy Technology Data Exchange (ETDEWEB)

    Cestelli Guidi, M.; Mirri, C.; Marcelli, A. [Laboratori Nazionali di Frascati - INFN, Frascati, Rome (Italy); Fratini, E.; Amendola, R. [ENEA, UT BIORAD-RAB, Rome (Italy); Licursi, V.; Negri, R. [Universita La Sapienza, Dip. Biologia e Biotecnologie ' ' Charles Darwin' ' , Rome (Italy)

    2012-09-15

    This paper discusses gene expression changes in the skin of mice treated by monoenergetic 14 MeV neutron irradiation and the possibility of monitoring the resultant lipid depletion (cross-validated by functional genomic analysis) as a marker of radiation exposure by high-resolution FT-IR (Fourier transform infrared) imaging spectroscopy. The irradiation was performed at the ENEA Frascati Neutron Generator (FNG), which is specifically dedicated to biological samples. FNG is a linear electrostatic accelerator that produces up to 1.0 x 10{sup 11} 14-MeV neutrons per second via the D-T nuclear reaction. The functional genomic approach was applied to four animals for each experimental condition (unirradiated, 0.2 Gy irradiation, or 1 Gy irradiation) 6 hours or 24 hours after exposure. Coregulation of a subclass of keratin and keratin-associated protein genes that are physically clustered in the mouse genome and functionally related to skin and hair follicle proliferation and differentiation was observed. Most of these genes are transiently upregulated at 6 h after the delivery of the lower dose delivered, and drastically downregulated at 24 h after the delivery of the dose of 1 Gy. In contrast, the gene coding for the leptin protein was consistently upregulated upon irradiation with both doses. Leptin is a key protein that regulates lipid accumulation in tissues, and its absence provokes obesity. The tissue analysis was performed by monitoring the accumulation and the distribution of skin lipids using FT-IR imaging spectroscopy. The overall picture indicates the differential modulation of key genes during epidermis homeostasis that leads to the activation of a self-renewal process at low doses of irradiation. (orig.)

  1. Modeling Microalgal Biosediment Formation Based on Attenuated Total Reflection Fourier Transform Infrared (ATR FT-IR) Monitoring.

    Science.gov (United States)

    Ogburn, Zachary L; Vogt, Frank

    2018-03-01

    With increasing amounts of anthropogenic pollutants being released into ecosystems, it becomes ever more important to understand their fate and interactions with living organisms. Microalgae play an important ecological role as they are ubiquitous in marine environments and sequester inorganic pollutants which they transform into organic biomass. Of particular interest in this study is their role as a sink for atmospheric CO 2 , a greenhouse gas, and nitrate, one cause of harmful algal blooms. Novel chemometric hard-modeling methodologies have been developed for interpreting phytoplankton's chemical and physiological adaptations to changes in their growing environment. These methodologies will facilitate investigations of environmental impacts of anthropogenic pollutants on chemical and physiological properties of marine microalgae (here: Nannochloropsis oculata). It has been demonstrated that attenuated total reflection Fourier transform infrared (ATR FT-IR) spectroscopy can gain insights into both and this study only focuses on the latter. From time-series of spectra, the rate of microalgal biomass settling on top of a horizontal ATR element is derived which reflects several of phytoplankton's physiological parameters such as growth rate, cell concentrations, cell size, and buoyancy. In order to assess environmental impacts on such parameters, microalgae cultures were grown under 25 different chemical scenarios covering 200-600 ppm atmospheric CO 2 and 0.35-0.75 mM dissolved NO 3 - . After recording time-series of ATR FT-IR spectra, a multivariate curve resolution-alternating least squares (MCR-ALS) algorithm extracted spectroscopic and time profiles from each data set. From the time profiles, it was found that in the considered concentration ranges only NO 3 - has an impact on the cells' physiological properties. In particular, the cultures' growth rate has been influenced by the ambient chemical conditions. Thus, the presented spectroscopic

  2. The use of combined synchrotron radiation micro FT-IR and XRD for the characterization of Romanesque wall paintings

    International Nuclear Information System (INIS)

    Salvado, N.; Buti, S.; Pantos, E.; Bahrami, F.; Labrador, A.; Pradell, T.

    2008-01-01

    The high analytical sensitivity and high spatial resolution of synchrotron radiation-based techniques, in particular SR-XRD and SR-FT-IR, allows the identification of complex micrometric mixtures of compounds that constitute the different layers of ancient paintings. The reliability of the measurements even with an extremely small amount of sampled material is very high, and this is particularly important when analyzing art works. Furthermore, the micro size (10 x 10μm for FT-IR and 30 to 50 μm squared spot size for XRD) of the beam enables one to obtain detailed compositional profiles from the different chromatic and preparation layers. The sensitivity of the techniques is high enough for the determination of minor and trace compounds, such as reaction and weathering compounds. We report here the identification of pigments in the Romanesque wall paintings found in situ in the church of Saint Eulalia of Unha place in the Aran valley (central Pyrenees). During the first centuries of the second millennium numerous religious buildings were built in Western Europe in the Romanesque style. In particular, a great number of churches were built in the Pyrenees, most of which were decorated with wall paintings. Although only a few of these paintings have survived, they represent one of the most important collections of Romanesque art, both for their quantity and quality. A full identification of the pigments, binder, supports, and reaction and weathering compounds has been obtained. The results obtained, in particular aerinite as a pigment, indicate a clear connection between the paintings found in this Occitanian church and the Catalan Romanesque paintings from the south bound of the Pyrenees. (orig.)

  3. In vivo skin leptin modulation after 14 MeV neutron irradiation: a molecular and FT-IR spectroscopic study.

    Science.gov (United States)

    Cestelli Guidi, M; Mirri, C; Fratini, E; Licursi, V; Negri, R; Marcelli, A; Amendola, R

    2012-09-01

    This paper discusses gene expression changes in the skin of mice treated by monoenergetic 14 MeV neutron irradiation and the possibility of monitoring the resultant lipid depletion (cross-validated by functional genomic analysis) as a marker of radiation exposure by high-resolution FT-IR (Fourier transform infrared) imaging spectroscopy. The irradiation was performed at the ENEA Frascati Neutron Generator (FNG), which is specifically dedicated to biological samples. FNG is a linear electrostatic accelerator that produces up to 1.0 × 10(11) 14-MeV neutrons per second via the D-T nuclear reaction. The functional genomic approach was applied to four animals for each experimental condition (unirradiated, 0.2 Gy irradiation, or 1 Gy irradiation) 6 hours or 24 hours after exposure. Coregulation of a subclass of keratin and keratin-associated protein genes that are physically clustered in the mouse genome and functionally related to skin and hair follicle proliferation and differentiation was observed. Most of these genes are transiently upregulated at 6 h after the delivery of the lower dose delivered, and drastically downregulated at 24 h after the delivery of the dose of 1 Gy. In contrast, the gene coding for the leptin protein was consistently upregulated upon irradiation with both doses. Leptin is a key protein that regulates lipid accumulation in tissues, and its absence provokes obesity. The tissue analysis was performed by monitoring the accumulation and the distribution of skin lipids using FT-IR imaging spectroscopy. The overall picture indicates the differential modulation of key genes during epidermis homeostasis that leads to the activation of a self-renewal process at low doses of irradiation.

  4. The use of combined synchrotron radiation micro FT-IR and XRD for the characterization of Romanesque wall paintings

    Energy Technology Data Exchange (ETDEWEB)

    Salvado, N.; Buti, S. [Universitat Politecnica de Catalunya, Dpt. d' Enginyeria Quimica, EPSEVG, Vilanova i la Geltru, Barcelona (Spain); Pantos, E.; Bahrami, F. [CCLRC, Daresbury Laboratory, Warrington (United Kingdom); Labrador, A. [LLS, BM16-ESRF, BP 220, Grenoble Cedex (France); Pradell, T. [Universitat Politecnica de Catalunya, Dpt. Fisica i Enginyeria Nuclear, ESAB, Castelldefels, Barcelona (Spain)

    2008-01-15

    The high analytical sensitivity and high spatial resolution of synchrotron radiation-based techniques, in particular SR-XRD and SR-FT-IR, allows the identification of complex micrometric mixtures of compounds that constitute the different layers of ancient paintings. The reliability of the measurements even with an extremely small amount of sampled material is very high, and this is particularly important when analyzing art works. Furthermore, the micro size (10 x 10{mu}m for FT-IR and 30 to 50 {mu}m squared spot size for XRD) of the beam enables one to obtain detailed compositional profiles from the different chromatic and preparation layers. The sensitivity of the techniques is high enough for the determination of minor and trace compounds, such as reaction and weathering compounds. We report here the identification of pigments in the Romanesque wall paintings found in situ in the church of Saint Eulalia of Unha place in the Aran valley (central Pyrenees). During the first centuries of the second millennium numerous religious buildings were built in Western Europe in the Romanesque style. In particular, a great number of churches were built in the Pyrenees, most of which were decorated with wall paintings. Although only a few of these paintings have survived, they represent one of the most important collections of Romanesque art, both for their quantity and quality. A full identification of the pigments, binder, supports, and reaction and weathering compounds has been obtained. The results obtained, in particular aerinite as a pigment, indicate a clear connection between the paintings found in this Occitanian church and the Catalan Romanesque paintings from the south bound of the Pyrenees. (orig.)

  5. Study of micro-phase separation of two polystyrene-based copolymer mixture using the combination of PALS and FT-IR

    International Nuclear Information System (INIS)

    Jiang, Z.Y.; Jiang, X.Q.; Yang, Y.X.; Huang, Y.J.; Huang, H.B.; Hsia, Y.F.

    2005-01-01

    Positron annihilation lifetime (PAL) spectroscopy, Fourier transform infrared (FT-IR) and differential scanning calorimetry (DSC) have been applied to study the micro-phase separation in the blends of poly(styrene-co-methylmethacrylate) (SMMA) copolymer and poly(styrene-co-maleic anhydride) (SMA) copolymer. The DSC results indicate that the SMA/SMMA blends are miscible and weak intermolecular interactions exist between SMA and SMMA. The strength of intermolecular interactions to some degree exhibits somewhat non-monotonic variation with increasing of SMA component in the blends. The results of PAL measurement present the blend containing 20 wt% SMA is phase-separated in molecular level, which is interpreted by the results of FT-IR analysis. It was concluded that it is helpful to study the miscibility of polymer blends in molecular level by means of PAL method, accompanied with the requisite measurement of DSC and FT-IR

  6. Development of C-lignin with G/S-lignin and lipids in orchid seed coats – an unexpected diversity exposed by ATR-FT-IR spectroscopy

    DEFF Research Database (Denmark)

    Barsberg, Søren Talbro; Lee, Y.-I.; Rasmussen, Hanne Nina

    2018-01-01

    Cite this article: Barsberg ST, Lee Y-I, Rasmussen HN. Development of C-lignin with G/S-lignin and lipids in orchid seed coats – an unexpected diversity exposed by ATR-FT-IR spectroscopy. Seed Science Research https:// doi.org/10.1017/S0960258517000344......Cite this article: Barsberg ST, Lee Y-I, Rasmussen HN. Development of C-lignin with G/S-lignin and lipids in orchid seed coats – an unexpected diversity exposed by ATR-FT-IR spectroscopy. Seed Science Research https:// doi.org/10.1017/S0960258517000344...

  7. A new Density Functional Theory (DFT) based method for supporting the assignment of vibrational signatures of mannan and cellulose—Analysis of palm kernel cake hydrolysis by ATR-FT-IR spectroscopy as a case study

    DEFF Research Database (Denmark)

    Barsberg, Søren Talbro; Sanadi, Anand Ramesh; Jørgensen, Henning

    2011-01-01

    Attenuated Total Reflectance (ATR) FT-IR spectroscopy gives in situ information on molecular concentration, organization and interactions in plant cell walls. We demonstrate its potential for further developments by a case study which combines ATR-FT-IR spectroscopy with a recently published DFT...... a decreasing degree of polymerization to be a plausible cause, although others may interfere. Keywords: Cellulose; Mannan; FT-IR; DFT; Molecular modelling; Palm kernel...

  8. FT-IR studies on the acidity of gallium-substituted mesoporous MCM-41 silica

    International Nuclear Information System (INIS)

    Turnes Palomino, Gemma; Jose Cuart Pascual, Juan; Rodriguez Delgado, Montserrat; Bernardo Parra, Jose; Otero Arean, Carlos

    2004-01-01

    Gallium-containing mesoporous MCM-41 silica was synthesized at a nominal Si:Ga ratio of 16:1. Synthesis was carried out from a parent gel containing no cations other than NH 4 + and cetyltrimethylammonium (template), so that following thermolysis of the template agent and ammonium ions the protonic form, H-GaMCM-41, was obtained. Powder X-ray diffraction showed the characteristic pattern of MCM-41-type materials, and nitrogen adsorption at 77 K lead to a value of 535 m 2 g -1 for the specific (BET) surface area. Infrared spectroscopy of carbon monoxide adsorbed at 77 K, and of pyridine and lutidine adsorbed at room temperature, showed the presence in H-GaMCM-41 of both Broensted and Lewis acid sites. Broensted acidity, assigned to structural Si(OH)Ga groups, was most distinctively proved by protonation of both pyridine and lutidine. Lewis acidity (coordinatively unsaturated Ga 3+ ions) showed up by formation of the characteristic Lewis-type adducts with both CO and pyridine

  9. A novel FT-IR spectroscopic method based on lipid characteristics for qualitative and quantitative analysis of animal-derived feedstuff adulterated with ruminant ingredients.

    Science.gov (United States)

    Gao, Fei; Zhou, Simiao; Han, Lujia; Yang, Zengling; Liu, Xian

    2017-12-15

    The objective of this study was to explore the ability of Fourier transform infrared (FT-IR) spectroscopy to authenticate adulterated animal-derived feedstuff. A total of 18 raw meat and bone meals (MBMs), including 9 non-ruminant MBMs and 9 ruminant MBMs, were mixed to obtain 81 binary mixtures with specific proportions (1-35%). Lipid spectral characteristics were analyzed by FT-IR spectroscopy combined with chemometrics. Changes in FT-IR spectra were observed as adulterant concentration was varied. The results illustrate ruminant adulteration can be successfully distinguished based on lipid characteristics. PLS model was established to quantify ruminant adulteration, which was shown to be valid (R 2 P >0.90). Furthermore, the ratios of CC/CO and CC/CH(CH 2 ), as well as the number of CH(CH 2 ) in the fatty acids of adulterated lipids, were calculated, which showed that differences in the trans fatty acid content and the degree of unsaturation were the main contributors to determination of adulteration based on FT-IR spectroscopy. Copyright © 2017. Published by Elsevier Ltd.

  10. Classification and structural analysis of live and dead salmonella cells using fourier transform infrared (FT-IR) spectroscopy and principle component analysis (PCA)

    Science.gov (United States)

    Fourier Transform Infrared Spectroscopy (FT-IR) was used to detect Salmonella typhimurium and Salmonella enteritidis foodborne bacteria and distinguish between live and dead cells of both serotypes. Bacteria were loaded individually on the ZnSe Attenuated Total Reflection (ATR) crystal surface and s...

  11. Combining FT-IR spectroscopy and multivariate analysis for qualitative and quantitative analysis of the cell wall composition changes during apples development.

    Science.gov (United States)

    Szymanska-Chargot, M; Chylinska, M; Kruk, B; Zdunek, A

    2015-01-22

    The aim of this work was to quantitatively and qualitatively determine the composition of the cell wall material from apples during development by means of Fourier transform infrared (FT-IR) spectroscopy. The FT-IR region of 1500-800 cm(-1), containing characteristic bands for galacturonic acid, hemicellulose and cellulose, was examined using principal component analysis (PCA), k-means clustering and partial least squares (PLS). The samples were differentiated by development stage and cultivar using PCA and k-means clustering. PLS calibration models for galacturonic acid, hemicellulose and cellulose content from FT-IR spectra were developed and validated with the reference data. PLS models were tested using the root-mean-square errors of cross-validation for contents of galacturonic acid, hemicellulose and cellulose which was 8.30 mg/g, 4.08% and 1.74%, respectively. It was proven that FT-IR spectroscopy combined with chemometric methods has potential for fast and reliable determination of the main constituents of fruit cell walls. Copyright © 2014 Elsevier Ltd. All rights reserved.

  12. Rapid, nondestructive estimation of surface polymer layer thickness using attenuated total reflection fourier transform infrared (ATR FT-IR) spectroscopy and synthetic spectra derived from optical principles.

    Science.gov (United States)

    Weinstock, B André; Guiney, Linda M; Loose, Christopher

    2012-11-01

    We have developed a rapid, nondestructive analytical method that estimates the thickness of a surface polymer layer with high precision but unknown accuracy using a single attenuated total reflection Fourier transform infrared (ATR FT-IR) measurement. Because the method is rapid, nondestructive, and requires no sample preparation, it is ideal as a process analytical technique. Prior to implementation, the ATR FT-IR spectrum of the substrate layer pure component and the ATR FT-IR and real refractive index spectra of the surface layer pure component must be known. From these three input spectra a synthetic mid-infrared spectral matrix of surface layers 0 nm to 10,000 nm thick on substrate is created de novo. A minimum statistical distance match between a process sample's ATR FT-IR spectrum and the synthetic spectral matrix provides the thickness of that sample. We show that this method can be used to successfully estimate the thickness of polysulfobetaine surface modification, a hydrated polymeric surface layer covalently bonded onto a polyetherurethane substrate. A database of 1850 sample spectra was examined. Spectrochemical matrix-effect unknowns, such as the nonuniform and molecularly novel polysulfobetaine-polyetherurethane interface, were found to be minimal. A partial least squares regression analysis of the database spectra versus their thicknesses as calculated by the method described yielded an estimate of precision of ±52 nm.

  13. Single Cell Synchrotron FT-IR Microspectroscopy Reveals a Link between Neutral Lipid and Storage Carbohydrate Fluxes in S. cerevisiae

    Science.gov (United States)

    Jamme, Frédéric; Vindigni, Jean-David; Méchin, Valérie; Cherifi, Tamazight; Chardot, Thierry; Froissard, Marine

    2013-01-01

    In most organisms, storage lipids are packaged into specialized structures called lipid droplets. These contain a core of neutral lipids surrounded by a monolayer of phospholipids, and various proteins which vary depending on the species. Hydrophobic structural proteins stabilize the interface between the lipid core and aqueous cellular environment (perilipin family of proteins, apolipoproteins, oleosins). We developed a genetic approach using heterologous expression in Saccharomyces cerevisiae of the Arabidopsis thaliana lipid droplet oleosin and caleosin proteins AtOle1 and AtClo1. These transformed yeasts overaccumulate lipid droplets, leading to a specific increase in storage lipids. The phenotype of these cells was explored using synchrotron FT-IR microspectroscopy to investigate the dynamics of lipid storage and cellular carbon fluxes reflected as changes in spectral fingerprints. Multivariate statistical analysis of the data showed a clear effect on storage carbohydrates and more specifically, a decrease in glycogen in our modified strains. These observations were confirmed by biochemical quantification of the storage carbohydrates glycogen and trehalose. Our results demonstrate that neutral lipid and storage carbohydrate fluxes are tightly connected and co-regulated. PMID:24040242

  14. Single cell synchrotron FT-IR microspectroscopy reveals a link between neutral lipid and storage carbohydrate fluxes in S. cerevisiae.

    Directory of Open Access Journals (Sweden)

    Frédéric Jamme

    Full Text Available In most organisms, storage lipids are packaged into specialized structures called lipid droplets. These contain a core of neutral lipids surrounded by a monolayer of phospholipids, and various proteins which vary depending on the species. Hydrophobic structural proteins stabilize the interface between the lipid core and aqueous cellular environment (perilipin family of proteins, apolipoproteins, oleosins. We developed a genetic approach using heterologous expression in Saccharomyces cerevisiae of the Arabidopsis thaliana lipid droplet oleosin and caleosin proteins AtOle1 and AtClo1. These transformed yeasts overaccumulate lipid droplets, leading to a specific increase in storage lipids. The phenotype of these cells was explored using synchrotron FT-IR microspectroscopy to investigate the dynamics of lipid storage and cellular carbon fluxes reflected as changes in spectral fingerprints. Multivariate statistical analysis of the data showed a clear effect on storage carbohydrates and more specifically, a decrease in glycogen in our modified strains. These observations were confirmed by biochemical quantification of the storage carbohydrates glycogen and trehalose. Our results demonstrate that neutral lipid and storage carbohydrate fluxes are tightly connected and co-regulated.

  15. Matrix-isolation and solid state low temperature FT-IR study of 2,3-butanedione (diacetyl)

    Science.gov (United States)

    Gómez-Zavaglia, A.; Fausto, R.

    2003-12-01

    2,3-Butanedione (diacetyl) was studied by matrix-isolation and low temperature solid state FT-IR spectroscopy, supported by molecular orbital calculations undertaken at the DFT(B3LYP) and MP2 levels of theory with the 6-311++G(d,p) basis set. Both in the crystalline phase and in the matrices, the compound exists in the C 2h symmetry trans conformation (OC-CO dihedral angle of 180°). This form corresponds to the single conformational state predicted by the theoretical calculations for the compound in vacuum. However, in the low temperature amorphous state, obtained by fast deposition of the vapour of the compound onto a suitable cold (9 K) substrate, as well as in the liquid and gaseous phases, spectroscopic features are observed that can only be explained by assuming that conformations without an inversion centre ( C 2 symmetry) do also contribute to the spectra. These results are in agreement with the experimental evidence that diacetyl has a permanent dipole moment (ca.1 Debye) in the vapour phase at room temperature and are here explained taking into consideration the influence of the low frequency large amplitude torsional vibration around the central C-C bond on the molecular properties.

  16. Detection of tautomer proportions of dimedone in solution: a new approach based on theoretical and FT-IR viewpoint

    Science.gov (United States)

    Karabulut, Sedat; Namli, Hilmi; Leszczynski, Jerzy

    2013-08-01

    Molecular structures of stable tautomers of dimedone [5,5-dimethyl-cyclohexane-1,3-dione ( 1) and 3-hydroxy-5,5-dimethylcyclohex-2-enone ( 2)] were optimized and vibrational frequencies were calculated in five different organic solvents (dimethylsulfoxide, methanol, acetonitrile, dichloromethane and chloroform). Geometry optimizations and harmonic vibrational frequency calculations were performed at DFT 6-31+G(d,p), DFT 6-311++G(2d,2p), MP2 6-311++G (2d,2p) and MP2 aug-cc-pVDZ levels for both stable forms of dimedone. Experimental FT-IR spectra of dimedone have also been recorded in the same solvents. A new approach was developed in order to determine tautomers' ratio using both experimental and theoretical data in Lambert-Beer equation. Obtained results were compared with experimental results published in literature. It has been concluded that while DFT 6-31+G(d,p) method provides accurate enol ratio in DMSO, MeOH, and DCM, in order to obtain accurate results for the other solvents the MP2 aug-cc-pVDZ level calculations should be used for CH3CN and CHCl3 solutions.

  17. Ft-Ir Spectroscopic Analysis of Potsherds Excavated from the First Settlement Layer of Kuriki Mound, Turkey

    Science.gov (United States)

    Bayazit, Murat; Isik, Iskender; Cereci, Sedat; Issi, Ali; Genc, Elif

    The region covering Southeastern Anatolia takes place in upper Mesopotamia, so it has numerous cultural heritages due to its witness to various social movements of different civilizations in ancient times. Kuruki Mound is located on the junction point of Tigris River and Batman Creek, near Oymatas village which is almost 15 km to Batman, Turkey. The mound is dated back to Late Chalcolithic. Archaeological excavations are carried out on two hills named as “Kuriki Mound-1” and “Kuriki Mound-2” in which 4-layer and 2-layer settlements have been revealed, respectively. This region will be left under the water by the reservoir lake of Ilısu Dam when its construction is completed. Thus, characterization of ancient materials such as potsherds, metals and skeleton ruins should be rapidly done. In this study, 12 potsherds excavated from Layer-1 (the first settlement layer after the surface) in Kuriki Mound-2 were investigated by FT-IR spectrometry. Energy dispersive X-ray fluorescence (EDXRF) and X-ray diffraction (XRD) analyses were used as complementary techniques in order to expose chemical and mineralogical/phase contents, respectively. Obtained results showed that the potteries have been produced with calcareous clays and they include moderate amounts of MgO, K2O, Na2O and Fe2O3 in this context. Additionally, high temperature phases have also been detected with XRD analyses in some samples.

  18. Total sulfur determination in residues of crude oil distillation using FT-IR/ATR and variable selection methods

    Science.gov (United States)

    Müller, Aline Lima Hermes; Picoloto, Rochele Sogari; Mello, Paola de Azevedo; Ferrão, Marco Flores; dos Santos, Maria de Fátima Pereira; Guimarães, Regina Célia Lourenço; Müller, Edson Irineu; Flores, Erico Marlon Moraes

    2012-04-01

    Total sulfur concentration was determined in atmospheric residue (AR) and vacuum residue (VR) samples obtained from petroleum distillation process by Fourier transform infrared spectroscopy with attenuated total reflectance (FT-IR/ATR) in association with chemometric methods. Calibration and prediction set consisted of 40 and 20 samples, respectively. Calibration models were developed using two variable selection models: interval partial least squares (iPLS) and synergy interval partial least squares (siPLS). Different treatments and pre-processing steps were also evaluated for the development of models. The pre-treatment based on multiplicative scatter correction (MSC) and the mean centered data were selected for models construction. The use of siPLS as variable selection method provided a model with root mean square error of prediction (RMSEP) values significantly better than those obtained by PLS model using all variables. The best model was obtained using siPLS algorithm with spectra divided in 20 intervals and combinations of 3 intervals (911-824, 823-736 and 737-650 cm-1). This model produced a RMSECV of 400 mg kg-1 S and RMSEP of 420 mg kg-1 S, showing a correlation coefficient of 0.990.

  19. Midinfrared FT-IR as a Tool for Monitoring Herbaceous Biomass Composition and Its Conversion to Furfural

    Directory of Open Access Journals (Sweden)

    Anna Maria Raspolli Galletti

    2015-01-01

    Full Text Available A semiquantitative analysis by means of midinfrared FT-IR spectroscopy was tuned for the simultaneous determination of cellulose, hemicellulose, and lignin in industrial crops such as giant reed (Arundo donax L. and switchgrass (Panicum virgatum L.. Ternary mixtures of pure cellulose, hemicellulose, and lignin were prepared and a direct correlation area/concentration was achieved for cellulose and lignin, whereas indirect correlations were found for hemicellulose quantification. Good correspondences between the values derived from our model and those reported in the literature or obtained according to the official Van Soest method were ascertained. Average contents of 40–45% of cellulose, 20–25% of hemicellulose, and 20–25% of lignin were obtained for different samples of giant reed species. In the case of switchgrass, a content of 36% of cellulose, 28% of hemicellulose, and 26% of lignin was achieved. This analysis was also carried out on giant reed and switchgrass residues after a mild hydrolysis step carried out with dilute hydrochloric acid for the production of furfural with good yield. Reasonable compositional data were obtained, thus allowing an indirect monitoring which helps the optimization of the hydrothermal pretreatment for furfural production from hemicellulose fractions.

  20. FT-IR reflection spectra of single crystals: resolving phonons of different symmetry without using polarised radiation

    Directory of Open Access Journals (Sweden)

    METODIJA NAJDOSKI

    2000-07-01

    Full Text Available Fourier-transform infrared (FT-IR reflection spectra, asquired at nearnormal incidence, were recorded from single crystals belonging to six crystal systems: CsCr(SO42.12H2O (alum, cubic, K2CuCl2·2H2O (Mitscherlichite, tetragonal, CaCO3 (calcite, hexagonal, KHSO4 (mercallite, orthorhombic, CaSO4·2H2O (gypsum, monoclinic and CuSO4·5H2O (chalcantite, triclinic. The acquired IR reflection spectra were further transformed into absorption spectra, employing the Kramers-Kronig transformation. Except for the cubic alums, the spectra strongly depend on the crystal face from which they were recorded; this is a consequence of anisotropy. Phonons of a given symmetry (E-species, in tetragonal/hexagonal and B-species, in monoclinic crystals may be resolved without using a polariser. The spectrum may be simplified in the case of an orthorhombic crystal, as well. The longitudinal-optical (LO and transversal-optical (TO mode frequencies were calculated in the case of optically isotropic and the simplified spectra of optically uniaxial crystals.

  1. A simplification of the deuterium oxide dilution technique using FT-IR analysis of plasma, for estimating piglet milk intake

    International Nuclear Information System (INIS)

    Glencross, B.D.; Tuckey, R.C.; Hartmann, P.E.; Mullan, B.P.

    1997-01-01

    Previous studies estimating milk intake using deuterium oxide (D 2 O) as a tracer have required sublimation of the sample fluid (usually plasma) to remove solids and retrieve total water. This procedure has been simplified by directly measuring the D 2 O content of plasma with a Fourier transform-infrared (FT-IR) spectrometer, removing the requirement for sample sublimation. Comparisons of samples that were split and then analysed as water of sublimation and as total plasma were performed. It was found that the direct analysis of the plasma could be achieved without a loss in fidelity of the results (sublimated v. plasma, r 2 = 0.976; n = 26). Linearity of assay standards was very high (r 2 > 0.997). The modified technique was used to determine the milk intake by piglets from litters of 7 sows during established lactation (Days 10-15). Water turnover (WTO) was shown to be the primary point by which differences in the piglet milk intakes were influenced. Differences in the milk composition had minimal effect on the milk intake determinations. Milk intake by each piglet was shown to be strongly correlated to piglet growth (r 2 = 0.59, P 2 = 0.84, P < 0.01). Copyright (1997) CSIRO Australia

  2. On the Traceability of Commercial Saffron Samples Using 1H-NMR and FT-IR Metabolomics

    Directory of Open Access Journals (Sweden)

    Roberto Consonni

    2016-02-01

    Full Text Available In previous works on authentic samples of saffron of known history (harvest and processing year, storage conditions, and length of time some biomarkers were proposed using both FT-IR and NMR metabolomics regarding the shelf life of the product. This work addresses the difficulties to trace back the “age” of commercial saffron samples of unknown history, sets a limit value above which these products can be considered substandard, and offers a useful tool to combat saffron mislabeling and fraud with low-quality saffron material. Investigations of authentic and commercial saffron samples of different origin and harvest year, which had been stored under controlled conditions for different lengths of time, allowed a clear-cut clustering of samples in two groups according to the storage period irrespectively of the provenience. In this respect, the four-year cut off point proposed in our previous work assisted to trace back the “age” of unknown samples and to check for possible mislabeling practices.

  3. Matrix-isolation FT-IR and DFT theoretical studies of the intramolecular hydrogen bonding in Mannich bases

    International Nuclear Information System (INIS)

    Pajak, J.; Rospenk, M.; Maes, G.; Sobczyk, L.

    2006-01-01

    FT-IR Ar-matrix isolated spectra were studied for dichloro- (Cl 2 -MB) and tetrachloroderivatives (Cl 4 -MB) of the ortho Mannich base. The spectra were analyzed based on the DFT calculated frequencies and intensities and compared with those recorded in CCl 4 solution in the region of the ν(OH) and ν(OD) vibrations. The matrix-isolated spectra are characterized by narrower ν(OH) and ν(OD) bands with much better resolved fine structure than in solution. The fine structure originates from the anharmonic coupling with the low frequency modes as well as from Fermi resonance. The ν(OD) band shapes can be reproduced exclusively by assuming the Fermi resonance with overtones and summation of the frequencies of modes into which the bridge atoms are involved. The frequency isotopic ratio (ISR) is for both compounds 1.33 while the half-width ratios are equal to 1.82 and 1.94, for Cl 2 -MB and Cl 4 -MB, respectively

  4. Optical Determination of Lead Chrome Green in Green Tea by Fourier Transform Infrared (FT-IR Transmission Spectroscopy.

    Directory of Open Access Journals (Sweden)

    Xiaoli Li

    Full Text Available The potential of Fourier transform infrared (FT-IR transmission spectroscopy for determination of lead chrome green in green tea was investigated based on chemometric methods. Firstly, the qualitative analysis of lead chrome green in tea was performed based on partial least squares discriminant analysis (PLS-DA, and the correct rate of classification was 100%. And then, a hybrid method of interval partial least squares (iPLS regression and successive projections algorithm (SPA was proposed to select characteristic wavenumbers for the quantitative analysis of lead chrome green in green tea, and 19 wavenumbers were obtained finally. Among these wavenumbers, 1384 (C = C, 1456, 1438, 1419(C = N, and 1506 (CNH cm-1 were the characteristic wavenumbers of lead chrome green. Then, these 19 wavenumbers were used to build determination models. The best model was achieved by least squares support vector machine (LS-SVMalgorithm with high coefficient of determination and low root-mean square error of prediction set (R2p = 0.864 and RMSEP = 0.291. All these results indicated the feasibility of IR spectra for detecting lead chrome green in green tea.

  5. Rapid authentication and identification of different types of A. roxburghii by Tri-step FT-IR spectroscopy

    Science.gov (United States)

    Chen, Ying; Huang, Jinfang; Yeap, Zhao Qin; Zhang, Xue; Wu, Shuisheng; Ng, Chiew Hoong; Yam, Mun Fei

    2018-06-01

    Anoectochilus roxburghii (Wall.) Lindl. (Orchidaceae) is a precious traditional Chinese medicinal herb and has been perennially used to treat various illness. However, there were unethical sellers who adulterated wild A. roxburghii with tissue cultured and cultivated ones. Therefore, there is an urgent need for an effective authentication method to differentiate between these different types of A. roxburghii. In this research, the infrared spectroscopic tri-step identification approach including Fourier transform infrared spectroscopy (FT-IR), Second derivative infrared spectra (SD-IR) and two-dimensional correlation infrared spectra (2D-IR) was used to develop a simple and rapid method to discriminate between wild, cultivated and tissue cultivated A. roxburghii plant. Through this study, all three types of A. roxburghii plant were successfully identified and discriminated through the infrared spectroscopic tri-step identification method. Besides that, all the samples of wild, cultivated and tissue cultivated A. roxburghii plant were analysed with the Soft Independent Modelling of Class Analogy (SIMCA) pattern recognition technique to test and verify the experimental results. The results showed that the three types of A. roxburghii can be discriminated clearly as the recognition rate was 100% for all three types and the rejection rate was more than 60%. 70% of the validated samples were also identified correctly by the SIMCA model. The SIMCA model was also validated by comparing 70 standard herbs to the model. As a result, it was demonstrated that the macroscopic IR fingerprint method and the classification analysis could discriminate not only between the A. roxburghi samples and the standard herbs, it could also distinguish between the three different types of A. roxburghi plant in a direct, rapid and holistic manner.

  6. Characterization of banana peel by scanning electron microscopy and FT-IR spectroscopy and its use for cadmium removal.

    Science.gov (United States)

    Memon, Jamil R; Memon, Saima Q; Bhanger, M I; Memon, G Zuhra; El-Turki, A; Allen, Geoffrey C

    2008-10-15

    This study describes the use of banana peel, a commonly produced fruit waste, for the removal of Cd(II) from environmental and industrial wastewater. The banana peel was characterized by FT-IR and scanning electron microscopy (SEM) coupled with energy dispersive X-ray (EDX) analysis. The parameters pH, contact time, initial metal ion concentration and temperature were investigated and found to be rapid ( approximately 97% within 10 min). The Langmuir adsorption isotherm was used to describe partitioning behavior for the system at room temperature. The value of Q(L) was found to be (35.52 mg g(-1)) higher than the previously reported materials. The binding of metal ions was found to be pH-dependent with the optimal sorption occurring at pH 8. The retained species were eluted with 5 mL of 5 x 10(-3)M HNO(3) with the detection limit of 1.7 x 10(-3)mg L(-1). Kinetics of sorption followed the pseudo-first-order rate equation with the rate constant k, equal to 0.13+/-0.01 min(-1). Thermodynamic parameters such as Gibbs free energy at 303K (-7.41+/-0.13 kJ mol(-1)) and enthalpy (40.56+/-2.34 kJ mol(-1)) indicated the spontaneous and endothermic nature of the sorption process. The developed method was utilized for the removal of Cd(II) ions from environmental and industrial wastewater samples using flame atomic absorption spectrophotometer (FAAS).

  7. Quantification of plaque area and characterization of plaque biochemical composition with atherosclerosis progression in ApoE/LDLR(-/-) mice by FT-IR imaging.

    Science.gov (United States)

    Wrobel, Tomasz P; Mateuszuk, Lukasz; Kostogrys, Renata B; Chlopicki, Stefan; Baranska, Malgorzata

    2013-11-07

    In this work the quantitative determination of atherosclerotic lesion area (ApoE/LDLR(-/-) mice) by FT-IR imaging is presented and validated by comparison with atherosclerotic lesion area determination by classic Oil Red O staining. Cluster analysis of FT-IR-based measurements in the 2800-3025 cm(-1) range allowed for quantitative analysis of the atherosclerosis plaque area, the results of which were highly correlated with those of Oil Red O histological staining (R(2) = 0.935). Moreover, a specific class obtained from a second cluster analysis of the aortic cross-section samples at different stages of disease progression (3, 4 and 6 months old) seemed to represent the macrophages (CD68) area within the atherosclerotic plaque.

  8. Simultaneous formation and detection of the reaction product of solid-state aspartame sweetener by FT-IR/DSC microscopic system.

    Science.gov (United States)

    Lin, S Y; Cheng, Y D

    2000-10-01

    The solid-state stability of aspartame hemihydrate (APM) sweetener during thermal treatment is important information for the food industry. The present study uses the novel technique of Fourier transform infrared microspectroscopy equipped with differential scanning calorimetry (FT-IR/DSC microscopic system) to accelerate and determine simultaneously the thermal-dependent impurity formation of solid-state APM. The results indicate a dramatic change in IR spectra from 50, 110 or 153 degrees C, which was respectively attributed to the onset temperature of water evaporation, dehydration and cyclization processes. It is suggested that the processes of dehydration and intramolecular cyclization occurred in the solid-state APM during the heating process. As an impurity, 3-carboxymethyl-6-benzyl-2,5-diketopiperazine (DKP) degraded from solid state APM via intramolecular cyclization and liberation of methanol. This was evidenced by this novel FT-IR/DSC microscopic system in a one-step procedure.

  9. Application of Fourier transform infrared (FT-IR) spectroscopy to the study of the modification of epoxidized sunflower oil by acrylation.

    Science.gov (United States)

    Irinislimane, Ratiba; Belhaneche-Bensemra, Naima

    2012-12-01

    Commercial sunflower oil was epoxidized at the laboratory-scale. The epoxidized sunflower oil (ESFO) was modified following the acrylation reaction. Modification was carried out simultaneously using acrylic acid (AA) and triethylamine (TEA). To optimize the reaction conditions, the effects of four temperatures (40, 60, 80, and 100 °C), the ESFO:AA (100:100) ratio, and 0.2% TEA were investigated. The rate of conversion was analyzed with both FT-IR and titration of the oxirane ring. After that, the temperature with the highest conversion was selected and used throughout for all modification reactions. Then, four ratios (100:100, 100:90, 100:80, and 100:75) of ESFO:AA were analyzed at four different concentrations of TEA (0.2, 0.3, 0.4, and 0.5%) to determine the best estimate for both the ESFO:AA ratio and the catalyst concentration. Conversion rate was analyzed using FT-IR spectroscopy by measuring the concentrations of ester, carbonyl, and alcohol groups. Moreover, oxirane-ring concentration was estimated using the titration method (with gentian violet as indicator) and FT-IR spectroscopy (epoxy ring absorptions at 1270 cm(-1) and 877 cm(-1)). Based on conversion yield, the optimum ESFO:AA ratio corresponds to 100:80; the best temperature reaction was at 60 °C, and the best TEA concentration was 0.2%. The critical amounts of reactants needed to reach maximum conversion were established. The final acid value of the acrylated ESFO after washing (pH = 7) was 2.1 mg potassium hydroxide (KOH)·g(-1). All results show that FT-IR spectroscopy is a simple, low-cost, rapid method for investigating the kinetics of a reaction.

  10. Técnicas FT-IR (PAS, UATR e Objetiva ATR Aplicadas à Caracterização de EPDM Modificada com Plasma

    Directory of Open Access Journals (Sweden)

    Renata Patrícia dos Santos

    2014-06-01

    Full Text Available Técnicas FT-IR (UATR, PAS e MIC, com objetiva ATR foram escolhidas para a caracterização da superfície da borracha de EPDM vulcanizada, após tratamento em plasma de Ar/O2 e N2/H2/Ar gerado em micro-ondas. Após tratamento, grupos oxigenados foram detectados por UATR e MIC/FT-IR, com objetiva ATR para as duas misturas gasosas, e possíveis grupos nitrogenados foram inseridos na superfície das amostras tratadas com plasma de N2/H2/Ar. A análise MIC/FT-IR sugeriu a formação de grupos em uma camada mais externa, para as amostras tratadas com plasma de N2/H2/Ar, sendo possível observar a redução na intensidade das bandas da absorção do CH2 e CH3, o que pode estar relacionado ao fato de o nitrogênio ser um gás menos permeável que o oxigênio. Diferentes velocidades, 0,05 cm.s-1 e 0,2 cm.s-1, foram utilizadas na análise PAS para avaliar a superfície após tratamento, e apenas para a velocidade 0,05 cm.s-1 com plasma de Ar/O2 alterações espectroscópicas foram detectadas. A redução na medida de ângulo de contato e o aumento na resistência ao descascamento da colagem indicaram melhoras nas propriedades adesivas da superfície. Falhas de adesão foram observadas entre a interface do filme de adesivo de PU e da borracha de EPDM, e confirmados por UATR/FT-IR.

  11. Analysis of clay smoking pipes from archeological sites in the region of the Guanabara Bay (Rio de Janeiro, Brazil) by FT-IR

    Science.gov (United States)

    Freitas, Renato P.; Ribeiro, Iohanna M.; Calza, Cristiane; Oliveira, Ana L.; Silva, Mariane L.; Felix, Valter S.; Ferreira, Douglas S.; Coelho, Felipe A.; Gaspar, Maria D.; Pimenta, André R.; Medeiros, Elanio A.; Lopes, Ricardo T.

    2016-06-01

    In this study, twenty samples of clay smoking pipes excavated in an 18 km2 area between the Macacu and Caceribu rivers, in the municipality of Itaboraí, Rio de Janeiro, Brazil were analyzed by FT-IR technique. The samples, excavated in different archeological sites of the region, are dated between the seventeenth and the nineteenth centuries and are part of the material culture left by Africans and African descendants that lived in the complex. FT-IR analyses and complementary SEM-EDS studies showed that the clay paste used in the manufacture of smoking pipes, mostly handcrafted, is composed of quartz, feldspar, phyllosilicates and iron oxides. Multivariate statistical tests (PCA) were applied to FT-IR data to assess the interactions between the archeological sites. The results indicated that one archeological site - Macacu IV - is greatly related to the other sites. The results obtained have helped archeologists and anthropologists in better understanding the manufacturing process employed in ancient ceramic artifacts produced during the period of colonial Brazil.

  12. Differentiation between probiotic and wild-type Bacillus cereus isolates by antibiotic susceptibility test and Fourier transform infrared spectroscopy (FT-IR).

    Science.gov (United States)

    Mietke, Henriette; Beer, W; Schleif, Julia; Schabert, G; Reissbrodt, R

    2010-05-30

    Animal feed often contains probiotic Bacillus strains used as feed additives. Spores of the non-pathogenic B. cereus var. toyoi (product name Toyocerin) are used. Distinguishing between toxic wild-type Bacillus cereus strains and this probiotic strain is essential for evaluating the quality and risk of feed. Bacillus cereus CIP 5832 (product name Paciflor was used as probiotic strain until 2001. The properties of the two probiotic strains are quite similar. Differentiating between probiotic strains and wild-type B. cereus strains is not easy. ss-lactam antibiotics such as penicillin and cefamandole exhibit an inhibition zone in the agar diffusion test of probiotic B. cereus strains which are not seen for wild-type strains. Therefore, performing the agar diffusion test first may make sense before FT-IR testing. When randomly checking these strains by Fourier transform infrared spectroscopy (FT-IR), the probiotic B. cereus strains were separated from wild-type B. cereus/B. thuringiensis/B. mycoides/B. weihenstephanensis strains by means of hierarchical cluster analysis. The discriminatory information was contained in the spectral windows 3000-2800 cm(-1) ("fatty acid region"), 1200-900 cm(-1) ("carbohydrate region") and 900-700 cm(-1) ("fingerprint region"). It is concluded that FT-IR spectroscopy can be used for the rapid quality control and risk analysis of animal feed containing probiotic B. cereus strains. (c) 2010 Elsevier B.V. All rights reserved.

  13. Honey bee odorant-binding protein 14: effects on thermal stability upon odorant binding revealed by FT-IR spectroscopy and CD measurements.

    Science.gov (United States)

    Schwaighofer, Andreas; Kotlowski, Caroline; Araman, Can; Chu, Nam; Mastrogiacomo, Rosa; Becker, Christian; Pelosi, Paolo; Knoll, Wolfgang; Larisika, Melanie; Nowak, Christoph

    2014-03-01

    In the present work, we study the effect of odorant binding on the thermal stability of honey bee (Apis mellifera L.) odorant-binding protein 14. Thermal denaturation of the protein in the absence and presence of different odorant molecules was monitored by Fourier transform infrared spectroscopy (FT-IR) and circular dichroism (CD). FT-IR spectra show characteristic bands for intermolecular aggregation through the formation of intermolecular β-sheets during the heating process. Transition temperatures in the FT-IR spectra were evaluated using moving-window 2D correlation maps and confirmed by CD measurements. The obtained results reveal an increase of the denaturation temperature of the protein when bound to an odorant molecule. We could also discriminate between high- and low-affinity odorants by determining transition temperatures, as demonstrated independently by the two applied methodologies. The increased thermal stability in the presence of ligands is attributed to a stabilizing effect of non-covalent interactions between odorant-binding protein 14 and the odorant molecule.

  14. Fourier Transform Infrared Spectroscopy (FT-IR) and Simple Algorithm Analysis for Rapid and Non-Destructive Assessment of Developmental Cotton Fibers.

    Science.gov (United States)

    Liu, Yongliang; Kim, Hee-Jin

    2017-06-22

    With cotton fiber growth or maturation, cellulose content in cotton fibers markedly increases. Traditional chemical methods have been developed to determine cellulose content, but it is time-consuming and labor-intensive, mostly owing to the slow hydrolysis process of fiber cellulose components. As one approach, the attenuated total reflection Fourier transform infrared (ATR FT-IR) spectroscopy technique has also been utilized to monitor cotton cellulose formation, by implementing various spectral interpretation strategies of both multivariate principal component analysis (PCA) and 1-, 2- or 3-band/-variable intensity or intensity ratios. The main objective of this study was to compare the correlations between cellulose content determined by chemical analysis and ATR FT-IR spectral indices acquired by the reported procedures, among developmental Texas Marker-1 (TM-1) and immature fiber ( im ) mutant cotton fibers. It was observed that the R value, CI IR , and the integrated intensity of the 895 cm -1 band exhibited strong and linear relationships with cellulose content. The results have demonstrated the suitability and utility of ATR FT-IR spectroscopy, combined with a simple algorithm analysis, in assessing cotton fiber cellulose content, maturity, and crystallinity in a manner which is rapid, routine, and non-destructive.

  15. Chemical profiling and adulteration screening of Aquilariae Lignum Resinatum by Fourier transform infrared (FT-IR) spectroscopy and two-dimensional correlation infrared (2D-IR) spectroscopy

    Science.gov (United States)

    Qu, Lei; Chen, Jian-bo; Zhang, Gui-Jun; Sun, Su-qin; Zheng, Jing

    2017-03-01

    As a kind of expensive perfume and valuable herb, Aquilariae Lignum Resinatum (ALR) is often adulterated for economic motivations. In this research, Fourier transform infrared (FT-IR) spectroscopy is employed to establish a simple and quick method for the adulteration screening of ALR. First, the principal chemical constituents of ALR are characterized by FT-IR spectroscopy at room temperature and two-dimensional correlation infrared (2D-IR) spectroscopy with thermal perturbation. Besides the common cellulose and lignin compounds, a certain amount of resin is the characteristic constituent of ALR. Synchronous and asynchronous 2D-IR spectra indicate that the resin (an unstable secondary metabolite) is more sensitive than cellulose and lignin (stable structural constituents) to the thermal perturbation. Using a certified ALR sample as the reference, the infrared spectral correlation threshold is determined by 30 authentic samples and 6 adulterated samples. The spectral correlation coefficient of an authentic ALR sample to the standard reference should be not less than 0.9886 (p = 0.01). Three commercial adulterated ALR samples are identified by the correlation threshold. Further interpretation of the infrared spectra of the adulterated samples indicates the common adulterating methods - counterfeiting with other kind of wood, adding ingredient such as sand to increase the weight, and adding the cheap resin such as rosin to increase the content of resin compounds. Results of this research prove that FT-IR spectroscopy can be used as a simple and accurate quality control method of ALR.

  16. Complementary online aerosol mass spectrometry and offline FT-IR spectroscopy measurements: Prospects and challenges for the analysis of anthropogenic aerosol particle emissions

    Science.gov (United States)

    Faber, Peter; Drewnick, Frank; Bierl, Reinhard; Borrmann, Stephan

    2017-10-01

    The aerosol mass spectrometer (AMS) is well established in investigating highly time-resolved dynamics of submicron aerosol chemical composition including organic aerosol (OA). However, interpretation of mass spectra on molecular level is limited due to strong fragmentation of organic substances and potential reactions inside the AMS ion chamber. Results from complementary filter-based FT-IR absorption measurements were used to explain features in high-resolution AMS mass spectra of different types of OA (e.g. cooking OA, cigarette smoking OA, wood burning OA). Using this approach some AMS fragment ions were validated in this study as appropriate and rather specific markers for a certain class of organic compounds for all particle types under investigation. These markers can therefore be used to get deeper insights in the chemical composition of OA based on AMS mass spectra in upcoming studies. However, the specificity of other fragment ions such as C2H4O2+ (m/z 60.02114) remains ambiguous. In such cases, complementary FT-IR measurements allow the interpretation of highly time-resolved AMS mass spectra at the level of molecular functional groups. Furthermore, this study discusses the challenges in reducing inorganic interferences (e.g. from water and ammonium salts) in FT-IR spectra of atmospheric aerosols to decrease spectral uncertainties for better comparisons and, thus, to get more robust results.

  17. Discrimination of edible oils and fats by combination of multivariate pattern recognition and FT-IR spectroscopy: A comparative study between different modeling methods

    Science.gov (United States)

    Javidnia, Katayoun; Parish, Maryam; Karimi, Sadegh; Hemmateenejad, Bahram

    2013-03-01

    By using FT-IR spectroscopy, many researchers from different disciplines enrich the experimental complexity of their research for obtaining more precise information. Moreover chemometrics techniques have boosted the use of IR instruments. In the present study we aimed to emphasize on the power of FT-IR spectroscopy for discrimination between different oil samples (especially fat from vegetable oils). Also our data were used to compare the performance of different classification methods. FT-IR transmittance spectra of oil samples (Corn, Colona, Sunflower, Soya, Olive, and Butter) were measured in the wave-number interval of 450-4000 cm-1. Classification analysis was performed utilizing PLS-DA, interval PLS-DA, extended canonical variate analysis (ECVA) and interval ECVA methods. The effect of data preprocessing by extended multiplicative signal correction was investigated. Whilst all employed method could distinguish butter from vegetable oils, iECVA resulted in the best performances for calibration and external test set with 100% sensitivity and specificity.

  18. FT-IR-cPAS—New Photoacoustic Measurement Technique for Analysis of Hot Gases: A Case Study on VOCs

    Science.gov (United States)

    Hirschmann, Christian Bernd; Koivikko, Niina Susanna; Raittila, Jussi; Tenhunen, Jussi; Ojala, Satu; Rahkamaa-Tolonen, Katariina; Marbach, Ralf; Hirschmann, Sarah; Keiski, Riitta Liisa

    2011-01-01

    This article describes a new photoacoustic FT-IR system capable of operating at elevated temperatures. The key hardware component is an optical-readout cantilever microphone that can work up to 200 °C. All parts in contact with the sample gas were put into a heated oven, incl. the photoacoustic cell. The sensitivity of the built photoacoustic system was tested by measuring 18 different VOCs. At 100 ppm gas concentration, the univariate signal to noise ratios (1σ, measurement time 25.5 min, at highest peak, optical resolution 8 cm−1) of the spectra varied from minimally 19 for o-xylene up to 329 for butyl acetate. The sensitivity can be improved by multivariate analyses over broad wavelength ranges, which effectively co-adds the univariate sensitivities achievable at individual wavelengths. The multivariate limit of detection (3σ, 8.5 min, full useful wavelength range), i.e., the best possible inverse analytical sensitivity achievable at optimum calibration, was calculated using the SBC method and varied from 2.60 ppm for dichloromethane to 0.33 ppm for butyl acetate. Depending on the shape of the spectra, which often only contain a few sharp peaks, the multivariate analysis improved the analytical sensitivity by 2.2 to 9.2 times compared to the univariate case. Selectivity and multi component ability were tested by a SBC calibration including 5 VOCs and water. The average cross selectivities turned out to be less than 2% and the resulting inverse analytical sensitivities of the 5 interfering VOCs was increased by maximum factor of 2.2 compared to the single component sensitivities. Water subtraction using SBC gave the true analyte concentration with a variation coefficient of 3%, although the sample spectra (methyl ethyl ketone, 200 ppm) contained water from 1,400 to 100k ppm and for subtraction only one water spectra (10k ppm) was used. The developed device shows significant improvement to the current state-of-the-art measurement methods used in industrial

  19. Imaging of lipids in atherosclerotic lesion in aorta from ApoE/LDLR-/- mice by FT-IR spectroscopy and Hierarchical Cluster Analysis.

    Science.gov (United States)

    P Wrobel, Tomasz; Mateuszuk, Lukasz; Chlopicki, Stefan; Malek, Kamilla; Baranska, Malgorzata

    2011-12-21

    Spectroscopy-based approaches can provide an insight into the biochemical composition of a tissue sample. In the present work Fourier transform infrared (FT-IR) spectroscopy was used to develop a reliable methodology to study the content of free fatty acids, triglycerides, cholesteryl esters as well as cholesterol in aorta from mice with atherosclerosis (ApoE/LDLR(-/-) mice). In particular, distribution and concentration of palmitic, oleic and linoleic acid derivatives were analyzed. Spectral analysis of pure compounds allowed for clear discrimination between free fatty acids and other similar moieties based on the carbonyl band position (1699-1710 cm(-1) range). In order to distinguish cholesteryl esters from triglycerides a ratio of carbonyl band to signal at 1010 cm(-1) was used. Imaging of lipids in atherosclerotic aortic lesions in ApoE/LDLR(-/-) mice was followed by Hierarchical Cluster Analysis (HCA). The aorta from C57Bl/6J control mice (fed with chow diet) was used for comparison. The measurements were completed with an FT-IR spectrometer equipped with a 128 × 128 FPA detector. In cross-section of aorta from ApoE/LDLR(-/-) mice a region of atherosclerotic plaque was clearly identified by HCA, which was later divided into 2 sub-regions, one characterized by the higher content of cholesterol, while the other by higher contents of cholesteryl esters. HCA of tissues deposited on normal microscopic glass, hence limited to the 2200-3800 cm(-1) spectral range, also identified a region of atherosclerotic plaque. Importantly, this region correlates with the area stained by standard histological staining for atherosclerotic plaque (Oil Red O). In conclusion, the use of FT-IR and HCA may provide a novel tool for qualitative and quantitative analysis of contents and distribution of lipids in atherosclerotic plaque.

  20. Chemical profiling and adulteration screening of Aquilariae Lignum Resinatum by Fourier transform infrared (FT-IR) spectroscopy and two-dimensional correlation infrared (2D-IR) spectroscopy.

    Science.gov (United States)

    Qu, Lei; Chen, Jian-Bo; Zhang, Gui-Jun; Sun, Su-Qin; Zheng, Jing

    2017-03-05

    As a kind of expensive perfume and valuable herb, Aquilariae Lignum Resinatum (ALR) is often adulterated for economic motivations. In this research, Fourier transform infrared (FT-IR) spectroscopy is employed to establish a simple and quick method for the adulteration screening of ALR. First, the principal chemical constituents of ALR are characterized by FT-IR spectroscopy at room temperature and two-dimensional correlation infrared (2D-IR) spectroscopy with thermal perturbation. Besides the common cellulose and lignin compounds, a certain amount of resin is the characteristic constituent of ALR. Synchronous and asynchronous 2D-IR spectra indicate that the resin (an unstable secondary metabolite) is more sensitive than cellulose and lignin (stable structural constituents) to the thermal perturbation. Using a certified ALR sample as the reference, the infrared spectral correlation threshold is determined by 30 authentic samples and 6 adulterated samples. The spectral correlation coefficient of an authentic ALR sample to the standard reference should be not less than 0.9886 (p=0.01). Three commercial adulterated ALR samples are identified by the correlation threshold. Further interpretation of the infrared spectra of the adulterated samples indicates the common adulterating methods - counterfeiting with other kind of wood, adding ingredient such as sand to increase the weight, and adding the cheap resin such as rosin to increase the content of resin compounds. Results of this research prove that FT-IR spectroscopy can be used as a simple and accurate quality control method of ALR. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Myowater dynamics and protein secondary structural changes as affected by heating rate in three pork qualities: a combined FT-IR microspectroscopic and 1H NMR relaxometry study.

    Science.gov (United States)

    Wu, Zhiyun; Bertram, Hanne Christine; Böcker, Ulrike; Ofstad, Ragni; Kohler, Achim

    2007-05-16

    The objective of this study was to investigate the influence of heating rate on myowater dynamics and protein secondary structures in three pork qualities by proton NMR T2 relaxation and Fourier transform infrared (FT-IR) microspectroscopy measurements. Two oven temperatures at 100 degrees C and 200 degrees C corresponding to slow and fast heating rates were applied on three pork qualities (DFD, PSE, and normal) to an internal center temperature of 65 degrees C. The fast heating induced a higher cooking loss, particularly for PSE meat. The water proton T21 distribution representing water entrapped within the myofibrillar network was influenced by heating rate and meat quality. Fast heating broadened the T21 distribution and decreased the relaxation times of the T21 peak position for three meat qualities. The changes in T21 relaxation times in meat can be interpreted in terms of chemical and diffusive exchange. FT-IR showed that fast heating caused a higher gain of random structures and aggregated beta-sheets at the expense of native alpha-helixes, and these changes dominate the fast-heating-induced broadening of T21 distribution and reduction in T21 times. Furthermore, of the three meat qualities, PSE meat had the broadest T21 distribution and the lowest T21 times for both heating rates, reflecting that the protein aggregation of PSE caused by heating is more extensive than those of DFD and normal, which is consistent with the IR data. The present study demonstrated that the changes in T2 relaxation times of water protons affected by heating rate and raw meat quality are well related to the protein secondary structural changes as probed by FT-IR microspectroscopy.

  2. DETERMINATION OF CRYSTALLINITY INDEX OF CARBOHYDRATE COMPONENTS IN HEMP (CANNABIS SATIVA L. WOODY CORE BY MEANS OF FT-IR SPECTROSCOPY

    Directory of Open Access Journals (Sweden)

    Esat Gümüşkaya

    2005-04-01

    Full Text Available In this study; it was investigated chemical compositions of hemp woody core and changes in crystallinity index of its carbohydrate components by using FT-IR spectroscopy was investigated. It was determined that carbohyrate components ratio in hemp woody core were similar to that in hard wood, but lignin content in hemp woody core was higher than in hard wood. Crystallinity index of carbohydrate components in hemp woody core increased by removing amorphous components. It was designated that monoclinic structure in hemp woody core and its carbohydrate components was dominant, but triclinic ratio increased by treated chemical isolation of carbohydrate from hemp woody core.

  3. Observations of surface-mediated reduction of Pu(VI) to Pu(IV) on hematite nanoparticles by ATR FT-IR

    Energy Technology Data Exchange (ETDEWEB)

    Emerson, Hilary P. [Florida International Univ., Applied Research Center, Miami, FL (United States); Powell, Brian A. [Clemson Univ., Dept. of Enviromental Engineering and Earth Sciences, Anderson, SC (United States)

    2015-07-01

    Previous studies have shown that mineral surfaces may facilitate the reduction of plutonium though the mechanisms of the reduction are still unknown. The objective of this study is to use batch sorption and attenuated total reflectance Fourier transform infrared spectroscopy experiments to observe the surface-mediated reduction of plutonium on hematite nanoparticles. These techniques allow for in situ measurement of reduction of plutonium with time and may lead to a better understanding of the mechanisms of surface mediated reduction of plutonium. For the first time, ATR FT-IR peaks for Pu(VI) sorbed to hematite are measured at ∝ 916 cm{sup -1}, respectively. The decrease in peak intensity with time provides a real-time, direct measurement of Pu(VI) reduction on the hematite surface. In this work pseudo first order rate constants estimated at the high loadings (22 mg{sub Pu}/g{sub hematite}, 1.34 x 10{sup -6} M{sub Pu}/m{sup 2}) for ATR FT-IR are approximately 10 x slower than at trace concentrations based on previous work. It is proposed that the reduced rate constant at higher Pu loadings occurs after the reduction capacity due to trace Fe(II) has been exhausted and is dependent on the oxidation of water and possibly electron shuttling based on the semiconducting nature of hematite. Therefore, the reduction rate at higher loadings is possibly due to the thermodynamic favorability of Pu(IV)-hydroxide complexes.

  4. Comparative investigation of Fourier transform infrared (FT-IR) spectroscopy and X-ray diffraction (XRD) in the determination of cotton fiber crystallinity.

    Science.gov (United States)

    Liu, Yongliang; Thibodeaux, Devron; Gamble, Gary; Bauer, Philip; VanDerveer, Don

    2012-08-01

    Despite considerable efforts in developing curve-fitting protocols to evaluate the crystallinity index (CI) from X-ray diffraction (XRD) measurements, in its present state XRD can only provide a qualitative or semi-quantitative assessment of the amounts of crystalline or amorphous fraction in a sample. The greatest barrier to establishing quantitative XRD is the lack of appropriate cellulose standards, which are needed to calibrate the XRD measurements. In practice, samples with known CI are very difficult to prepare or determine. In a previous study, we reported the development of a simple algorithm for determining fiber crystallinity information from Fourier transform infrared (FT-IR) spectroscopy. Hence, in this study we not only compared the fiber crystallinity information between FT-IR and XRD measurements, by developing a simple XRD algorithm in place of a time-consuming and subjective curve-fitting process, but we also suggested a direct way of determining cotton cellulose CI by calibrating XRD with the use of CI(IR) as references.

  5. Identification of Quercus agrifolia (coast live oak resistant to the invasive pathogen Phytophthora ramorum in native stands using Fourier-transform infrared (FT-IR spectroscopy

    Directory of Open Access Journals (Sweden)

    Anna Olivia Conrad

    2014-10-01

    Full Text Available Over the last two decades coast live oak (CLO dominance in many California coastal ecosystems has been threatened by the alien invasive pathogen Phytophthora ramorum, the causal agent of sudden oak death. In spite of high infection and mortality rates in some areas, the presence of apparently resistant trees has been observed, including trees that become infected but recover over time. However, identifying resistant trees based on recovery alone can take many years. The objective of this study was to determine if Fourier-transform infrared (FT-IR spectroscopy, a chemical fingerprinting technique, can be used to identify CLO resistant to P. ramorum prior to infection. Soft independent modeling of class analogy identified spectral regions that differed between resistant and susceptible trees. Regions most useful for discrimination were associated with carbonyl group vibrations. Additionally, concentrations of two putative phenolic biomarkers of resistance were predicted using partial least squares regression; > 99% of the variation was explained by this analysis. This study demonstrates that chemical fingerprinting can be used to identify resistance in a natural population of forest trees prior to infection with a pathogen. FT-IR spectroscopy may be a useful approach for managing forests impacted by sudden oak death, as well as in other situations where emerging or existing forest pests and diseases are of concern.

  6. On the Use of Fourier Transform Infrared (FT-IR) Spectroscopy and Synthetic Calibration Spectra to Quantify Gas Concentrations in a Fischer-Tropsch Catalyst System

    Science.gov (United States)

    Ferguson, Frank T.; Johnson, Natasha M.; Nuth, Joseph A., III

    2015-01-01

    One possible origin of prebiotic organic material is that these compounds were formed via Fischer-Tropsch-type (FTT) reactions of carbon monoxide and hydrogen on silicate and oxide grains in the warm, inner-solar nebula. To investigate this possibility, an experimental system has been built in which the catalytic efficiency of different grain-analog materials can be tested. During such runs, the gas phase above these grain analogs is sampled using Fourier transform infrared (FT-IR) spectroscopy. To provide quantitative estimates of the concentration of these gases, a technique in which high-resolution spectra of the gases are calculated using the high-resolution transmission molecular absorption (HITRAN) database is used. Next, these spectra are processed via a method that mimics the processes giving rise to the instrumental line shape of the FT-IR spectrometer, including apodization, self-apodization, and broadening due to the finite resolution. The result is a very close match between the measured and computed spectra. This technique was tested using four major gases found in the FTT reactions: carbon monoxide, methane, carbon dioxide, and water. For the ranges typical of the FTT reactions, the carbon monoxide results were found to be accurate to within 5% and the remaining gases accurate to within 10%. These spectra can then be used to generate synthetic calibration data, allowing the rapid computation of the gas concentrations in the FTT experiments.

  7. Caracterização por FT-IR da superfície de borracha EPDM tratada via plasma por micro-ondas

    Directory of Open Access Journals (Sweden)

    Renata P. dos Santos

    2012-01-01

    Full Text Available A superfície de uma borracha de etileno-propileno-dieno (EPDM vulcanizada foi modificada via plasma por microondas, com gases Ar, Ar/O2, N2/O2 e N2/H2, tendo como objetivo melhorar as propriedades adesivas da superfície. A técnica FT-IR/UATR foi escolhida para caracterizar as superfícies após tratamento, pois apresentou menor interferência dos ingredientes da formulação da EPDM, dentre as técnicas analisadas (ATR/KRS-5 e Ge. Grupos oxigenados foram inseridos na superfície da amostra tratada, mesmo quando não foi utilizado o oxigênio, pois estes grupos foram formados quando a superfície ativada foi exposta à atmosfera. Já em tratamentos contendo N2, grupos oxigenados e possíveis grupos nitrogenados foram identificados por FT-IR. Redução nos valores do ângulo de contato, aumento no trabalho de adesão e aumento no ensaio de resistência ao descascamento (EPDM × Poliuretano foram observados após tratamento com Ar e N2/H2, resultando em melhora nas propriedades adesivas da superfície tratada.

  8. Multivariate analysis of attenuated total reflection Fourier transform infrared (ATR FT-IR) spectroscopic data to confirm phase partitioning in methacrylate-based dentin adhesive.

    Science.gov (United States)

    Ye, Qiang; Parthasarathy, Ranganathan; Abedin, Farhana; Laurence, Jennifer S; Misra, Anil; Spencer, Paulette

    2013-12-01

    Water is ubiquitous in the mouths of healthy individuals and is a major interfering factor in the development of a durable seal between the tooth and composite restoration. Water leads to the formation of a variety of defects in dentin adhesives; these defects undermine the tooth-composite bond. Our group recently analyzed phase partitioning of dentin adhesives using high-performance liquid chromatography (HPLC). The concentration measurements provided by HPLC offered a more thorough representation of current adhesive performance and elucidated directions to be taken for further improvement. The sample preparation and instrument analysis using HPLC are, however, time-consuming and labor-intensive. The objective of this work was to develop a methodology for rapid, reliable, and accurate quantitative analysis of near-equilibrium phase partitioning in adhesives exposed to conditions simulating the wet oral environment. Analysis by Fourier transform infrared (FT-IR) spectroscopy in combination with multivariate statistical methods, including partial least squares (PLS) regression and principal component regression (PCR), were used for multivariate calibration to quantify the compositions in separated phases. Excellent predictions were achieved when either the hydrophobic-rich phase or the hydrophilic-rich phase mixtures were analyzed. These results indicate that FT-IR spectroscopy has excellent potential as a rapid method of detection and quantification of dentin adhesives that experience phase separation under conditions that simulate the wet oral environment.

  9. Attenuated Total Reflection Fourier Transform Infrared (ATR FT-IR) for Rapid Determination of Microbial Cell Lipid Content: Correlation with Gas Chromatography-Mass Spectrometry (GC-MS).

    Science.gov (United States)

    Millan-Oropeza, Aaron; Rebois, Rolando; David, Michelle; Moussa, Fathi; Dazzi, Alexandre; Bleton, Jean; Virolle, Marie-Joelle; Deniset-Besseau, Ariane

    2017-10-01

    There is a growing interest worldwide for the production of renewable oil without mobilizing agriculture lands; fast and reliable methods are needed to identify highly oleaginous microorganisms of potential industrial interest. The aim of this study was to demonstrate the relevance of attenuated total reflection (ATR) spectroscopy to achieve this goal. To do so, the total lipid content of lyophilized samples of five Streptomyces strains with varying lipid content was assessed with two classical quantitative but time-consuming methods, gas chromatography-mass spectrometry (GC-MS) and ATR Fourier transform infrared (ATR FT-IR) spectroscopy in transmission mode with KBr pellets and the fast ATR method, often questioned for its lack of reliability. A linear correlation between these three methods was demonstrated allowing the establishment of equations to convert ATR values expressed as CO/amide I ratio, into micrograms of lipid per milligram of biomass. The ATR method proved to be as reliable and quantitative as the classical GC-MS and FT-IR in transmission mode methods but faster and more reproducible than the latter since it involves far less manipulation for sample preparation than the two others. Attenuated total reflection could be regarded as an efficient fast screening method to identify natural or genetically modified oleaginous microorganisms by the scientific community working in the field of bio-lipids.

  10. Comparison of FTIR-ATR and Raman spectroscopy in determination of VLDL triglycerides in blood serum with PLS regression

    Science.gov (United States)

    Oleszko, Adam; Hartwich, Jadwiga; Wójtowicz, Anna; Gąsior-Głogowska, Marlena; Huras, Hubert; Komorowska, Małgorzata

    2017-08-01

    Hypertriglyceridemia, related with triglyceride (TG) in plasma above 1.7 mmol/L is one of the cardiovascular risk factors. Very low density lipoproteins (VLDL) are the main TG carriers. Despite being time consuming, demanding well-qualified staff and expensive instrumentation, ultracentrifugation technique still remains the gold standard for the VLDL isolation. Therefore faster and simpler method of VLDL-TG determination is needed. Vibrational spectroscopy, including FT-IR and Raman, is widely used technique in lipid and protein research. The aim of this study was assessment of Raman and FT-IR spectroscopy in determination of VLDL-TG directly in serum with the isolation step omitted. TG concentration in serum and in ultracentrifugated VLDL fractions from 32 patients were measured with reference colorimetric method. FT-IR and Raman spectra of VLDL and serum samples were acquired. Partial least square (PLS) regression was used for calibration and leave-one-out cross validation. Our results confirmed possibility of reagent-free determination of VLDL-TG directly in serum with both Raman and FT-IR spectroscopy. Quantitative VLDL testing by FT-IR and/or Raman spectroscopy applied directly to maternal serum seems to be promising screening test to identify women with increased risk of adverse pregnancy outcomes and patient friendly method of choice based on ease of performance, accuracy and efficiency.

  11. Caracterização de um pré-impregnado aeronáutico por FT-IR e análise térmica Characterization of pre-impregnated of epoxy resin/carbon fiber

    Directory of Open Access Journals (Sweden)

    Vanesa C. G. M. Ferrari

    2012-01-01

    Full Text Available Este trabalho consiste na caracterização de um pré-impregnado ("prepreg" de resina epoxídica/fibra de carbono, usando-se espectroscopia no infravermelho com transformada de Fourier (FT-IR, análise termogravimétrica (TG, calorimetria exploratória diferencial (DSC e análise térmica dinâmico-mecânica (DMTA. A análise por FT-IR foi realizada nos modos de transmissão (pastilha de KBr, pirólise em bico de Bunsen e controlada e detecção fotoacústica (PAS. Os espectros de FT-IR de transmissão revelaram a presença de resina epoxídica, grupos ciano, amínicos e bisfenol A, que possibilitaram identificar o provável agente de cura:a cianoguanidina (ou dicianodiamida do sistema epoxídico. Os espectros de FT-IR/PAS permitiram acompanhar as alterações espectrométricas causadas pela cura. A análise térmica auxiliou na observação e compreensão dos eventos durante o processo de cura, etapas de gelificação e vitrificação, e da influência destas nas temperaturas de transição vítrea (Tg do material curado e na escolha do intervalo de temperatura de cura, que é um dos parâmetros mais importantes do processo produtivo.This work explores the characterization of pre-impregnated ("prepreg" materials made with an epoxy resin/carbon fiber, using FT-IR spectroscopy, thermogravimetry (TG, differential scanning calorimetry (DSC and dynamic mechanical thermal analysis (DMTA. FT-IR spectroscopy was used in the transmission mode (KBr pellets, pyrolysis without control and controlled pyrolysis and photoacoustic detection (FT-IR/PAS. The transmission FT-IR spectra revealed the presence of epoxy resin, cyano groups, amine and bisphenol A, which allowed us to identify the probable agent of cure: cyanoguanidine (or DCD. With FT-IR/PAS it was possible to monitor spectrometric changes caused by curing. The thermal analysis assisted in observing and understanding events during the curing process, including the gelation and vitrification steps. It

  12. 2DCOS and PCMW2D analysis of FT-IR/ATR spectra measured at variable temperatures on-line to a polyurethane polymerization

    Science.gov (United States)

    Schuchardt, Patrick; Unger, Miriam; Siesler, Heinz W.

    2018-01-01

    In the present communication the potential of 2DCOS analysis and the spin-off technique perturbation-correlation moving window 2D (PCMW2D) analysis is illustrated with reference to spectroscopic changes observed in a data set recorded by in-line fiber-coupled FT-IR spectroscopy in the attenuated total reflection (ATR) mode during a polyurethane solution polymerization at different temperatures. In view of the chemical functionalities involved, hydrogen bonding plays an important role in this polymerization reaction. Based on the 2DCOS and PCMW2D analysis, the sequence of hydrogen bonding changes accompanying the progress of polymerization and precipitation of solid polymer can be determined. Complementary to the kinetic data derived from the original variable-temperature spectra in a previous publication the results provide a more detailed picture of the investigated solution polymerization.

  13. Conversion of Natural Aldehydes from Eucalyptus citriodora, Cymbopogon citratus, and Lippia multiflora into Oximes: GC-MS and FT-IR Analysis †

    Directory of Open Access Journals (Sweden)

    Igor W. Ouédraogo

    2009-08-01

    Full Text Available Three carbonyl-containing extracts of essential oils from Eucalyptus citriodora (Myrtaceae, Cymbopogon citratus (Gramineae and Lippia multiflora (Verbenaceae were used for the preparation of oximes. The reaction mixtures were analyzed by GC-MS and different compounds were identified on the basis of their retention times and mass spectra. We observed quantitative conversion of aldehydes to their corresponding oximes with a purity of 95 to 99%. E and Z stereoisomers of the oximes were obtained and separated by GC-MS. During GC analysis, the high temperature in the injector was shown to cause partial dehydratation of oximes and the resulting nitriles were readily identified. Based on FT-IR spectroscopy, that revealed the high stability and low volatility of these compounds, the so-obtained oximes could be useful for future biological studies.

  14. DSC, FT-IR, NIR, NIR-PCA and NIR-ANOVA for determination of chemical stability of diuretic drugs: impact of excipients

    Directory of Open Access Journals (Sweden)

    Gumieniczek Anna

    2018-03-01

    Full Text Available It is well known that drugs can directly react with excipients. In addition, excipients can be a source of impurities that either directly react with drugs or catalyze their degradation. Thus, binary mixtures of three diuretics, torasemide, furosemide and amiloride with different excipients, i.e. citric acid anhydrous, povidone K25 (PVP, magnesium stearate (Mg stearate, lactose, D-mannitol, glycine, calcium hydrogen phosphate anhydrous (CaHPO4 and starch, were examined to detect interactions. High temperature and humidity or UV/VIS irradiation were applied as stressing conditions. Differential scanning calorimetry (DSC, FT-IR and NIR were used to adequately collect information. In addition, chemometric assessments of NIR signals with principal component analysis (PCA and ANOVA were applied.

  15. Green synthesis and characterization of graphene nanosheets

    Energy Technology Data Exchange (ETDEWEB)

    Tavakoli, Farnosh [School of Chemistry, College of Science, University of Tehran, Tehran (Iran, Islamic Republic of); Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir [Institute of Nano Science and Nano Technology, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Badiei, Alireza [School of Chemistry, College of Science, University of Tehran, Tehran (Iran, Islamic Republic of); Mohandes, Fatemeh [Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of)

    2015-03-15

    Highlights: • For the first time, we have synthesized graphene nanosheets in the presence of pomegranate juice. • Here pomegranate juice was used not only as reductant but also as capping agent. • FT-IR, XRD, SEM, EDS and TEM were used to characterize the samples. • According to TEM image, graphene nanosheet is individually exfoliated after stirring for 24 h. • As shown in the TEM image, graphene monolayer is obtained. - Abstract: For the first time, we have successfully synthesized graphene nanosheets in the presence of pomegranate juice. In this approach, pomegranate juice was used not only as reductant but also as capping agent to form graphene nanosheets. At first, the improved Hummer method to oxidize graphite for the synthesis of graphene oxide (GO) was applied, and then the as-produced graphene oxide was reduced by pomegranate juice to form graphene nanosheets. Fourier transformed infrared (FT-IR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and raman were used to characterize the samples. The results obtained from the characterization techniques proved high purity of the final products.

  16. Green synthesis and characterization of graphene nanosheets

    International Nuclear Information System (INIS)

    Tavakoli, Farnosh; Salavati-Niasari, Masoud; Badiei, Alireza; Mohandes, Fatemeh

    2015-01-01

    Highlights: • For the first time, we have synthesized graphene nanosheets in the presence of pomegranate juice. • Here pomegranate juice was used not only as reductant but also as capping agent. • FT-IR, XRD, SEM, EDS and TEM were used to characterize the samples. • According to TEM image, graphene nanosheet is individually exfoliated after stirring for 24 h. • As shown in the TEM image, graphene monolayer is obtained. - Abstract: For the first time, we have successfully synthesized graphene nanosheets in the presence of pomegranate juice. In this approach, pomegranate juice was used not only as reductant but also as capping agent to form graphene nanosheets. At first, the improved Hummer method to oxidize graphite for the synthesis of graphene oxide (GO) was applied, and then the as-produced graphene oxide was reduced by pomegranate juice to form graphene nanosheets. Fourier transformed infrared (FT-IR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and raman were used to characterize the samples. The results obtained from the characterization techniques proved high purity of the final products

  17. Automated Fast Screening Method for Cocaine Identification in Seized Drug Samples Using a Portable Fourier Transform Infrared (FT-IR) Instrument.

    Science.gov (United States)

    Mainali, Dipak; Seelenbinder, John

    2016-05-01

    Quick and presumptive identification of seized drug samples without destroying evidence is necessary for law enforcement officials to control the trafficking and abuse of drugs. This work reports an automated screening method to detect the presence of cocaine in seized samples using portable Fourier transform infrared (FT-IR) spectrometers. The method is based on the identification of well-defined characteristic vibrational frequencies related to the functional group of the cocaine molecule and is fully automated through the use of an expert system. Traditionally, analysts look for key functional group bands in the infrared spectra and characterization of the molecules present is dependent on user interpretation. This implies the need for user expertise, especially in samples that likely are mixtures. As such, this approach is biased and also not suitable for non-experts. The method proposed in this work uses the well-established "center of gravity" peak picking mathematical algorithm and combines it with the conditional reporting feature in MicroLab software to provide an automated method that can be successfully employed by users with varied experience levels. The method reports the confidence level of cocaine present only when a certain number of cocaine related peaks are identified by the automated method. Unlike library search and chemometric methods that are dependent on the library database or the training set samples used to build the calibration model, the proposed method is relatively independent of adulterants and diluents present in the seized mixture. This automated method in combination with a portable FT-IR spectrometer provides law enforcement officials, criminal investigators, or forensic experts a quick field-based prescreening capability for the presence of cocaine in seized drug samples. © The Author(s) 2016.

  18. Application of PCA and SIMCA statistical analysis of FT-IR spectra for the classification and identification of different slag types with environmental origin.

    Science.gov (United States)

    Stumpe, B; Engel, T; Steinweg, B; Marschner, B

    2012-04-03

    In the past, different slag materials were often used for landscaping and construction purposes or simply dumped. Nowadays German environmental laws strictly control the use of slags, but there is still a remaining part of 35% which is uncontrolled dumped in landfills. Since some slags have high heavy metal contents and different slag types have typical chemical and physical properties that will influence the risk potential and other characteristics of the deposits, an identification of the slag types is needed. We developed a FT-IR-based statistical method to identify different slags classes. Slags samples were collected at different sites throughout various cities within the industrial Ruhr area. Then, spectra of 35 samples from four different slags classes, ladle furnace (LF), blast furnace (BF), oxygen furnace steel (OF), and zinc furnace slags (ZF), were determined in the mid-infrared region (4000-400 cm(-1)). The spectra data sets were subject to statistical classification methods for the separation of separate spectral data of different slag classes. Principal component analysis (PCA) models for each slag class were developed and further used for soft independent modeling of class analogy (SIMCA). Precise classification of slag samples into four different slag classes were achieved using two different SIMCA models stepwise. At first, SIMCA 1 was used for classification of ZF as well as OF slags over the total spectral range. If no correct classification was found, then the spectrum was analyzed with SIMCA 2 at reduced wavenumbers for the classification of LF as well as BF spectra. As a result, we provide a time- and cost-efficient method based on FT-IR spectroscopy for processing and identifying large numbers of environmental slag samples.

  19. Correcting the effect of refraction and dispersion of light in FT-IR spectroscopic imaging in transmission through thick infrared windows.

    Science.gov (United States)

    Chan, K L Andrew; Kazarian, Sergei G

    2013-01-15

    Transmission mode is one of the most common sampling methods for FT-IR spectroscopic imaging because the spectra obtained generally have a reasonable signal-to-noise ratio. However, dispersion and refraction of infrared light occurs when samples are sandwiched between infrared windows or placed underneath a layer of liquid. Dispersion and refraction cause infrared light to focus with different focal lengths depending on the wavelength (wavenumber) of the light. As a result, images obtained are in focus only at a particular wavenumber while they are defocused at other wavenumber values. In this work, a solution to correct this spread of focus by means of adding a lens on top of the infrared transparent window, such that a pseudo hemisphere is formed, has been investigated. Through this lens (or pseudo hemisphere), refraction of light is removed and the light across the spectral range has the same focal depth. Furthermore, the lens acts as a solid immersion objective and an increase of both magnification and spatial resolution (by 1.4 times) is demonstrated. The spatial resolution was investigated using an USAF resolution target, showing that the Rayleigh criterion can be achieved, as well as a sample with a sharp polymer interface to indicate the spatial resolution that can be expected in real samples. The reported approach was used to obtain chemical images of cross sections of cancer tissue and hair samples sandwiched between infrared windows showing the versatility and applicability of the method. In addition to the improved spatial resolution, the results reported herein also demonstrate that the lens can reduce the effect of scattering near the edges of tissue samples. The advantages of the presented approach, obtaining FT-IR spectroscopic images in transmission mode with the same focus across all wavenumber values and simultaneous improvement in spatial resolution, will have wide implications ranging from studies of live cells to sorption of drugs into tissues.

  20. Real time observation of proteolysis with Fourier transform infrared (FT-IR) and UV-circular dichroism spectroscopy: Watching a protease eat a protein

    Science.gov (United States)

    Güler, Günnur; Džafić, Enela; Vorob'ev, Mikhail M.; Vogel, Vitali; Mäntele, Werner

    2011-06-01

    Fourier transform infrared (FT-IR)- and UV-circular dichroism (UV-CD) spectroscopy have been used to study real-time proteolytic digestion of β-lactoglobulin (β-LG) and β-casein (β-CN) by trypsin at various substrate/enzyme ratios in D 2O-buffer at 37 °C. Both techniques confirm that protein substrate looses its secondary structure upon conversion to the peptide fragments. This perturbation alters the backbone of the protein chain resulting in conformational changes and degrading of the intact protein. Precisely, the most significant spectral changes which arise from digestion take place in the amide I and amide II regions. The FT-IR spectra for the degraded β-LG show a decrease around 1634 cm -1, suggesting a decrease of β-sheet structure in the course of hydrolysis. Similarly, the intensity around the 1654 cm -1 band decreases for β-CN digested by trypsin, indicating a reduction in the α-helical part. On the other hand, the intensity around ˜1594 cm -1 and ˜1406 cm -1 increases upon enzymatic breakdown of both substrates, suggesting an increase in the antisymmetric and symmetric stretching modes of free carboxylates, respectively, as released digestion products. Observation of further H/D exchange in the course of digestion manifests the structural opening of the buried groups and accessibility to the core of the substrate. On the basis of the UV-CD spectra recorded for β-LG and β-CN digested by trypsin, the unordered structure increases concomitant with a decrease in the remaining structure, thus, revealing breakdown of the intact protein into smaller fragments. This model study in a closed reaction system may serve as a basis for the much more complex digestion processes in an open reaction system such as the stomach.

  1. Comparison of Fiber Optic and Conduit Attenuated Total Reflection (ATR) Fourier Transform Infrared (FT-IR) Setup for In-Line Fermentation Monitoring.

    Science.gov (United States)

    Koch, Cosima; Posch, Andreas E; Herwig, Christoph; Lendl, Bernhard

    2016-12-01

    The performance of a fiber optic and an optical conduit in-line attenuated total reflection mid-infrared (IR) probe during in situ monitoring of Penicillium chrysogenum fermentation were compared. The fiber optic probe was connected to a sealed, portable, Fourier transform infrared (FT-IR) process spectrometer via a plug-and-play interface. The optical conduit, on the other hand, was connected to a FT-IR process spectrometer via a knuckled probe with mirrors that had to be adjusted prior to each fermentation, which were purged with dry air. Penicillin V (PenV) and its precursor phenoxyacetic acid (POX) concentrations were determined by online high-performance liquid chromatography and the obtained concentrations were used as reference to build partial least squares regression models. Cross-validated root-mean-square errors of prediction were found to be 0.2 g L -1 (POX) and 0.19 g L -1 (PenV) for the fiber optic setup and 0.17 g L -1 (both POX and PenV) for the conduit setup. Higher noise-levels and spectrum-to-spectrum variations of the fiber optic setup lead to higher noise of estimated (i.e., unknown) POX and PenV concentrations than was found for the conduit setup. It seems that trade-off has to be made between ease of handling (fiber optic setup) and measurement accuracy (optical conduit setup) when choosing one of these systems for bioprocess monitoring. © The Author(s) 2016.

  2. DFT, FT-IR, FT-Raman and NMR studies of 4-(substituted phenylazo)-3,5-diacetamido-1H-pyrazoles

    Science.gov (United States)

    Kınalı, Selin; Demirci, Serkan; Çalışır, Zühre; Kurt, Mustafa; Ataç, Ahmet

    2011-05-01

    We present a detailed analysis of the structural and vibrational spectra of some novel azo dyes. 2-(Substituted phenylazo)malononitriles were synthesized by the coupling reaction of the diazonium salts, which were prepared with the use of various aniline derivatives with malononitrile, and then 4-(substituted phenylazo)-3,5-diamino-1H-pyrazole azo dyes were obtained via the ring closure of the azo compounds with hydrazine monohydrate. The experimental and theoretical vibrational spectra of azo dyes were studied. The structural and spectroscopic analysis of the molecules were carried out by using Becke's three-parameters hybrid functional (B3LYP) and density functional harmonic calculations. The 1H nuclear magnetic resonance (NMR) chemical shifts of the azo dye molecules were calculated using the gauge-invariant-atomic orbital (GIAO) method. The calculated vibrational wavenumbers and chemical shifts were compared with the experimental data of the molecules.

  3. Physicochemical characterization by AFM, FT-IR and DSC and biological assays of a promising antileishmania delivery system loaded with a natural Brazilian product.

    Science.gov (United States)

    Marquele-Oliveira, Franciane; Torres, Elina Cassia; Barud, Hernane da Silva; Zoccal, Karina Furlani; Faccioli, Lúcia Helena; Hori, Juliana I; Berretta, Andresa Aparecida

    2016-05-10

    The control and treatment of Leishmaniasis, a neglected and infectious disease affecting approximately 12 million people worldwide, are challenging. Leishmania parasites multiply intracellularly within macrophages located in deep skin and in visceral tissues, and the currently employed treatments for this disease are subject to significant drawbacks, such as resistance and toxicity. Thus, the search for new Leishmaniasis treatments is compulsory, and Ocotea duckei Vattimo, a plant-derived product from the biodiverse Brazilian flora, may be a promising new treatment for this disease. In this regard, the aim of this work was to develop and characterize a delivery system based on solid lipid nanoparticles (SLN) that contain the liposoluble lignan fraction (LF) of Ocotea duckei Vattimo, which targets the Leishmania phagolysosome of infected macrophages. LF-loaded SLNs were obtained via the hot microemulsion method, and their physical and chemical properties were comprehensively assessed using PCS, AFM, SEM, FT-IR, DSC, HPLC, kinetic drug release studies, and biological assays. The size of the developed delivery system was 218.85±14.2 nm, its zeta potential was -30 mV and its entrapment efficiency (EE%) was high (the EEs% of YAN [yangambin] and EPI-YAN [epi-yangambin] markers were 94.21±0.40% and 94.20±0.00%, respectively). Microscopy, FT-IR and DSC assays confirmed that the delivery system was nanosized and indicated a core-shell encapsulation model, which corroborated the measured kinetics of drug release. The total in vitro release rates of YAN and EPI-YAN in buffer (with sink conditions attained) were 29.6±8.3% and 34.3±8.9%, respectively, via diffusion through the cellulose acetate membrane of the SLN over a period of 4 h. After 24 h, the release rates of both markers reached approximately 45%, suggesting a sustained pattern of release. Mathematical modeling indicated that both markers, YAN and EPI-YAN, followed matrix diffusion-based release kinetics (Higuchi

  4. Facile green synthesis of fluorescent N-doped carbon dots from Actinidia deliciosa and their catalytic activity and cytotoxicity applications

    Science.gov (United States)

    Arul, Velusamy; Sethuraman, Mathur Gopalakrishnan

    2018-04-01

    Green synthesis of fluorescent nitrogen doped carbon dots (N-CDs) using Actinidia deliciosa (A. deliciosa) fruit extract as a carbon precursor and aqueous ammonia as a nitrogen dopant is reported here. The synthesized N-CDs were characterized by high resolution transmission electron microscopy (HR-TEM), energy dispersive spectroscopy (EDS), selected area electron diffraction (SAED), UV-Visible spectroscopy (UV-Vis), fluorescence spectroscopy, Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). The average size of the N-CDs was approximately 3.59 nm and the calculated inter layer distance was found to be 0.21 nm. Raman spectroscopy and SAED pattern revealed the graphitic nature of the synthesized N-CDs. The N-CDs were found to emit intense blue color at 405 nm under the excitation of 315 nm. The doping of nitrogen over the surface of the N-CDs was confirmed by EDS, FT-IR and XPS studies. The synthesized N-CDs were found to exhibit excellent catalytic activity in the reduction of Rhodamine-B using sodium borohydrate. The MTT assay was used to evaluate the cytotoxicity and biocompatibility of N-CDs towards L-929 and MCF-7 cells. From the results obtained, it was found that the N-CDs exhibit low cytotoxicity and superior biocompatibility on both L-929 and MCF-7 cells.

  5. Ferutinin as a Ca(2+) complexone: lipid bilayers, conductometry, FT-IR, NMR studies and DFT-B3LYP calculations.

    Science.gov (United States)

    Dubis, A; Zamaraeva, M V; Siergiejczyk, L; Charishnikova, O; Shlyonsky, V

    2015-10-07

    Calcium ionophoretic properties of ferutinin were re-evaluated in solvent-containing bilayer lipid membranes. The slopes of conductance-concentration curves suggest that in the presence of a solvent in the membrane the majority of complexes appear to consist of a single terpenoid molecule bound to one Ca ion. By contrast, the stoichiometry of ferutinin-Ca(2+) complexes in acetone determined using the conductometric method was 2 : 1. While the cation-cation selectivity of ferutinin did not change, the cation-anion selectivity slightly decreased in solvent containing membranes. FT-IR and NMR data together with DFT calculations at the B3LYP/6-31G(d) level of theory indicate that in the absence of Ca ions ferutinin molecules are hydrogen-bonded at the phenol hydroxyl groups. The variations of absorption assigned to -OH and -C-O stretching mode suggest that ferutinin interacts strongly with Ca ions via the hydroxyl group of ferutinol and carboxyl oxygen of the complex ether bond. The coordination through the carbonyl group of ferutinin was demonstrated by theoretical calculations. Taken together, ferutinin molecules form H-bonded dimers, while complexation of Ca(2+) by ferutinin ruptures this hydrogen bond due to spatial re-orientation of the ferutinin molecules from parallel to antiparallel alignment.

  6. FT-IR spectra of the anti-HIV nucleoside analogue d4T (Stavudine). Solid state simulation by DFT methods and scaling by different procedures

    Science.gov (United States)

    Alcolea Palafox, M.; Kattan, D.; Afseth, N. K.

    2018-04-01

    A theoretical and experimental vibrational study of the anti-HIV d4T (stavudine or Zerit) nucleoside analogue was carried out. The predicted spectra in the three most stable conformers in the biological active anti-form of the isolated state were compared. Comparison of the conformers with those of the natural nucleoside thymidine was carried out. The calculated spectra were scaled by using different scaling procedures and three DFT methods. The TLSE procedure leads to the lowest error and is thus recommended for scaling. With the population of these conformers the IR gas-phase spectra were predicted. The crystal unit cell of the different polymorphism forms of d4T were simulated through dimer forms by using DFT methods. The scaled spectra of these dimer forms were compared. The FT-IR spectrum was recorded in the solid state in the 400-4000 cm-1 range. The respective vibrational bands were analyzed and assigned to different normal modes of vibration by comparison with the scaled vibrational values of the different dimer forms. Through this comparison, the polymorphous form of the solid state sample was identified. The study indicates that d4T exist only in the ketonic form in the solid state. The results obtained were in agreement with those determined in related anti-HIV nucleoside analogues.

  7. FT-IR spectroelectrochemical study of the reduction of 1,4-dinitrobenzene on Au electrode: Hydrogen bonding and protonation in proton donor mixed media

    International Nuclear Information System (INIS)

    Tian Dexiang; Jin Baokang

    2011-01-01

    Highlights: → 1,4-Dinitrobenzene electrochemical reduction on the Au electrode is explored. → Radical anion (PNB· - ) is found both in aprotic media and in proton donors mixed media. → The H-bonding forming between PNB· - , PNB 2- and proton donors in low donors concentration. → The protonation of PNB 2- occurs in high concentration proton donor mixed media. - Abstract: The electrochemical behavior of 1,4-dinitrobenzene (1,4-PNB) on the Au electrode was investigated by cyclic voltammetry (CV), in situ FT-IR spectroelectrochemistry, cyclic voltabsorptometry (CVA) and derivative cyclic voltabsorptometry (DCVA) techniques. In aprotic media, 1,4-dinitrobenzene is reversibly reduced in two-step one-electron transfer. A series of IR absorption bands at 1056, 1210, 1341, 1356, 1464 and 1549 cm -1 , tracing to PNB; PNB· - and PNB 2- are observed. In the presence of proton donors mixed media, with increasing concentrations of proton donors, hydrogen-bonding and protonation process are found successively. The values of combining proton donors with per PNB 2- to form hydrogen-bonding are estimated by using electrochemical parameters. The result of forming aromatic nitroso compound is supported by tracing the change of IR absorption bands at 1149 and 1587 cm -1 at high concentration of proton donors. Based on CVA and DCVA techniques, it is clearly distinguished that the mechanisms of electrochemical reduction of PNB are elaborated in different systems.

  8. Structural, spectroscopic (FT-IR, NMR, UV-visible), nonlinear optical (NLO), cytotoxic and molecular docking studies of 4-nitro-isonitrosoacetophenone (ninapH) by DFT method

    Science.gov (United States)

    Kucuk, Ilhan; Kaya, Yunus; Kaya, A. Asli

    2017-07-01

    (4-Nitro-phenyl)-oxo-acetaldehyde oxime (ninapH) is a type of oxime, which has a oxime and α-carbonyl groups. This molecule has been synthesized from literature procedure. The structural properties and conformational behaviors were examined using the density functional theory (DFT) with the B3LYP method combined with the 6-311++G(d,p) basis set. As a result of the conformational studies, the most stable conformer was determined, and then this molecule was optimized with the same basis set. Comprehensive theoretical and experimental structural studies on the molecule have been carried out by FT-IR, NMR and UV-vis spectrometry. The calculated HOMO and LUMO energies show that charge transfer within the molecule. The first order hyperpolarizability and molecular electrostatic potential (MEP) were also performed. The thermodynamic properties (heat capacity, entropy, and enthalpy) of the ninapH have been calculated at different temperatures, 100-1000 K. In addition, the molecular docking studies have been performed with DNA and protein structures (downloaded from Protein Data Bank).

  9. Vibrational frequency analysis, FT-IR, DFT and M06-2X studies on tert-Butyl N-(thiophen-2yl)carbamate

    Science.gov (United States)

    Sert, Yusuf; Singer, L. M.; Findlater, M.; Doğan, Hatice; Çırak, Ç.

    2014-07-01

    In this study, the experimental and theoretical vibrational frequencies of a newly synthesized tert-Butyl N-(thiophen-2yl)carbamate have been investigated. The experimental FT-IR (4000-400 cm-1) spectrum of the molecule in the solid phase have been recorded. The theoretical vibrational frequencies and optimized geometric parameters (bond lengths and bond angles) have been calculated by using density functional theory (DFT/B3LYP: Becke, 3-parameter, Lee-Yang-Parr) and DFT/M06-2X (the highly parametrized, empirical exchange correlation function) quantum chemical methods with the 6-311++G(d,p) basis set by Gaussian 09W software, for the first time. The vibrational frequencies have been assigned using potential energy distribution (PED) analysis by using VEDA 4 software. The computational optimized geometric parameters and vibrational frequencies have been found to be in good agreement with the corresponding experimental data, and with related literature results. In addition, the highest occupied molecular orbital (HOMO) and the lowest unoccupied molecular orbital (LUMO) energies and the other related molecular energy values have been calculated and are depicted.

  10. Pressure effects on the structure, kinetic, and thermodynamic properties of heat-induced aggregation of protein studied by FT-IR spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Taniguchi, Y [Applied Chemistry Department, Ritsumeikan University, Kusatsu, Shiga 525-8577 (Japan); Okuno, A [Research Department 3, Central Research, Bridgestone Co. Kodaira, Tokyo 187-8531 (Japan); Kato, M, E-mail: taniguti@sk.ritsumei.ac.j [Pharmaceutical Sciences Department, Ritsumeikan University, Kusatsu, Shiga 525-8577 (Japan)

    2010-03-01

    Pressure can retrain the heat-induced aggregation and dissociate the heat-induced aggregates. We observed the aggregation-preventing pressure effect and the aggregates-dissociating pressure effect to characterize the heat-induced aggregation of equine serum albumin (ESA) by FT-IR spectroscopy. The results suggest the {alpha}-helical structure collapses at the beginning of heat-induced aggregation through the swollen structure, and then the rearrangement of structure to the intermolecular {beta}-sheet takes place through partially unfolded structure. We determined the activation volume for the heat-induced aggregation ({Delta}V'' = +93 ml/mol) and the partial molar volume difference between native state and heat-induced aggregates ({Delta}V=+32 ml/mol). This positive partial molar volume difference suggests that the heat-induced aggregates have larger internal voids than the native structure. Moreover, the positive volume change implies that the formation of the intermolecular {beta}-sheet is unfavorable under high pressure.

  11. Advantages of TOF-SIMS analysis of hydroxyapatite and fluorapatite in comparison with XRD, HR-TEM and FT-IR.

    Science.gov (United States)

    Okazaki, Masayuki; Hirata, Isao; Matsumoto, Takuya; Takahashi, Junzo

    2005-12-01

    The chemical analysis of hydroxyapatite and fluorapatite was carried out using time-of-flight secondary ion mass spectrometry (TOF-SIMS). Hydroxyapatite and fluorapatite were synthesized at 80 +/- 1 degrees C and pH 7.4 +/- 0.2. Fluorapatite was better crystallized, with its (300) reflection shifted to a slightly higher angle. High-resolution transmission electron microscopy clearly revealed a typical, regular hexagonal cross section perpendicular to the c-axis for fluorapatite and a flattened hexagonal cross section for hydroxyapatite. FT-IR spectra of fluorapatite confirmed the absence of OH absorption peak--which was seen in hydroxyapatite at about 3570 cm(-1). TOF-SIMS mass spectra showed a peak at 40 amu due to calcium. In addition, a peak at 19 amu due to fluorine could be clearly seen, although the intensities of PO, PO2, and PO3 were very low. It was confirmed that TOF-SIMS clearly showed the differences between positive and negative mass spectra of hydroxyapatite and fluorapatite, especially for F-. We concluded that TOF-SIMS exhibited distinct advantages compared with other methods of analysis.

  12. Copper Enhanced Monooxygenase Activity and FT-IR Spectroscopic Characterisation of Biotransformation Products in Trichloroethylene Degrading Bacterium: Stenotrophomonas maltophilia PM102

    Directory of Open Access Journals (Sweden)

    Piyali Mukherjee

    2013-01-01

    Full Text Available Stenotrophomonas maltophilia PM102 (NCBI GenBank Acc. no. JQ797560 is capable of growth on trichloroethylene as the sole carbon source. In this paper, we report the purification and characterisation of oxygenase present in the PM102 isolate. Enzyme activity was found to be induced 10.3-fold in presence of 0.7 mM copper with a further increment to 14.96-fold in presence of 0.05 mM NADH. Optimum temperature for oxygenase activity was recorded at 36∘C. The reported enzyme was found to have enhanced activity at pH 5 and pH 8, indicating presence of two isoforms. Maximum activity was seen on incubation with benzene compared to other substrates like TCE, chloroform, toluene, hexane, and petroleum benzene. Km and Vmax for benzene were 3.8 mM and 340 U/mg/min and those for TCE were 2.1 mM and 170 U/mg/min. The crude enzyme was partially purified by ammonium sulphate precipitation followed by dialysis. Zymogram analysis revealed two isoforms in the 70% purified enzyme fraction. The activity stain was more prominent when the native gel was incubated in benzene as substrate in comparison to TCE. Crude enzyme and purified enzyme fractions were assayed for TCE degradation by the Fujiwara test. TCE biotransformation products were analysed by FT-IR spectroscopy.

  13. Elastic properties and structural studies on some zinc-borate glasses derived from ultrasonic, FT-IR and X-ray techniques

    International Nuclear Information System (INIS)

    Gaafar, M.S.; El-Aal, N.S. Abd; Gerges, O.W.; El-Amir, G.

    2009-01-01

    Glasses in the system (1 - x) [29Na 2 O- 4Al 2 O 3 - 67B 2 O 3 ]- xZnO (0 ≤ x ≤ 35 mol%), have been prepared by the melt quenching technique. Elastic properties, X-ray and FT-IR spectroscopic studies have been employed to study the role of ZnO on the structure of the investigated glass system. Elastic properties and Debye temperature have been investigated using sound wave velocity measurements at 4 MHz at room temperature. The results showed that the density increases and the molar volume decreases while both sound velocities and the determined glass transition temperatures decrease with increase in x. X-ray and infrared spectra of the glasses reveal that the borate network consists of diborate units and is affected by the increase in the concentration of ZnO content. These results are interpreted in terms of the decrease in the N 4 values (fraction of tetrahedral coordinated boron atoms), and substitution of longer bond lengths of Zn-O in place of shorter B-O bond. The results indicate that Zinc ions have been substituted for boron ions as tetrahedral network former ions. The elastic moduli are observed to increase with the increase of ZnO content.

  14. Speciation of organic matter in sandy soil size fractions as revealed by analytical pyrolysis (Py-GC/MS) and FT-IR spectroscopy

    Science.gov (United States)

    Jiménez-Morillo, Nicasio T.; González-Vila, Francisco J.; Jordán, Antonio; Zavala, Lorena M.; de la Rosa, José M.; González-Pérez, José A.

    2015-04-01

    This research deals with the assessment of organic matter structural differences in soil physical fractions before and after lipid extractions. Soil samples were collected in sandy soils, Arenosols (WRB 2006) from the Doñana National Park (SW Spain) under different vegetation cover: cork oak (Quercus suber, QS), eagle fern (Pteridium aquilinum, PA), pine (Pinus pinea, PP) and rockrose (Halimium halimifolium, HH). Two size fractions; coarse (C: 1-2 mm) and fine (F: 0.05-0.25 mm) were studied from each soil. . In addition, the two fractions from each soil were exhaustively Soxhlet extracted with a Dichlorometane-Methanol (3:1) mixture to obtain the lipid-free fractions (LF) from each size fraction (LFC and LFF). The composition of the organic matter at a molecular level in the different soil fractions was approached by analytical pyrolysis (Py-GC/MS) and FT-IR spectroscopy. These techniques are complementary and have been found suitable for the structural characterization of complex organic matrices (Moldoveanu, 1998; Piccolo and Stevenson, 1982); whereas Py-GC/MS provides detailed structural information of individual compounds present and a finger-printing of soil organic matter, FT-IR is informative about major functional groups present. The advantages of these techniques are well known: no need for pretreatment are fast to perform, highly reproducible and only small amount of samples are needed. Soil size fractions show contrasting differences in organic matter content (C 4-7 % and F > 40 %) and conspicuous differences were found in the pyrolysis products released by the fractions studied. The main families of pyrolysis compounds have well defined macromolecular precursors, such as lignin, polypeptides, polysaccharides and lipids (González-Vila et al., 2001). The C fractions yield higher relative abundance of lignin and polysaccharide derived pyrolysis compounds. Regarding the differences in the soil organic matter as affected by the different vegetation covers

  15. Archaeometric investigation of red-figured pottery fragments from Gioiosa Guardia (Messina, Sicily) by INAA, FT-IR and TOF-ND techniques

    International Nuclear Information System (INIS)

    Barilaro, D.; Crupi, V.; Interdonato, S.

    2008-01-01

    The present work is addressed to the study of some precious ancient pottery fragments, coming from the archaeological site of Gioiosa Guardia, in the Tirrenean Coast of Sicily. On the basis of historical and aesthetic considerations, the findings are dated back to 6.-5. Century b.C. and show a surface entirely decorated by red-figured technique, typical of Attic production. Many doubts arise about the real provenance of the artefacts. On one side, they could come directly from Greece, as attested by trading patterns between Greece and Southern Italy, on the other side, they could be produced in Sicily under the Greek artistic influence. In order to obtain a detailed characterization of the samples, a microdistruttive investigation was performed by Instrumental Neutron Activation Analysis (INAA), Fourier transform infrared absorption (FT-IR) and a non-invasive analysis by time-of-flight neutron diffraction (TOF-ND). Starting from the identification of the mineralogical and geochemical composition, a correct classification of the shards can be achieved.

  16. Tianeptine, olanzapine and fluoxetine show similar restoring effects on stress induced molecular changes in mice brain: An FT-IR study

    Science.gov (United States)

    Türker-Kaya, Sevgi; Mutlu, Oğuz; Çelikyurt, İpek K.; Akar, Furuzan; Ulak, Güner

    2016-05-01

    Chronic stress which can cause a variety of disorders and illness ranging from metabolic and cardiovascular to mental leads to alterations in content, structure and dynamics of biomolecules in brain. The determination of stress-induced changes along with the effects of antidepressant treatment on these parameters might bring about more effective therapeutic strategies. In the present study, we investigated unpredictable chronic mild stress (UCMS)-induced changes in biomolecules in mouse brain and the restoring effects of tianeptine (TIA), olanzapine (OLZ) and fluoxetine (FLX) on these variations, by Fourier transform infrared (FT-IR) spectroscopy. The results revealed that chronic stress causes different membrane packing and an increase in lipid peroxidation, membrane fluidity. A significant increment for lipid/protein, Cdbnd O/lipid, CH3/lipid, CH2/lipid, PO-2/lipid, COO-/lipid and RNA/protein ratios but a significant decrease for lipid/protein ratios were also obtained. Additionally, altered protein secondary structure components were estimated, such as increment in random coils and beta structures. The administration of TIA, OLZ and FLX drugs restored these stress-induced variations except for alterations in protein structure and RNA/protein ratio. This may suggest that these drugs have similar restoring effects on the consequences of stress activity in brain, in spite of the differences in their action mechanisms. All findings might have importance in understanding molecular mechanisms underlying chronic stress and contribute to studies aimed for drug development.

  17. Application of experimental design in examination of the dissolution rate of carbamazepine from formulations: Characterization of the optimal formulation by DSC, TGA, FT-IR and PXRD analysis

    Directory of Open Access Journals (Sweden)

    Krstić Marko

    2015-01-01

    Full Text Available Poor solubility is one of the key reasons for the poor bioavailability of these drugs. This paper displays a formulation of a solid surfactant system with carbamazepine, in order to increase its dissolution rate. Solid state surfactant systems are formed by application of fractal experimental design. Poloxamer 237 and Poloxamer 338 were used as surfactants and Brij® 35 was used as the co-surfactant. The ratios of the excipients and carbamazepine were varied and their effects on the dissolution rate of carbamazepine were examined. Moreover, the effects of the addition of natural (diatomite and a synthetic adsorbent carrier (Neusiline UFL2 on the dissolution rate of carbamazepine were also tested. The prepared surfactant systems were characterized and the influence of the excipients on possible changes of the polymorphous form of carbamazepine examined by application of analytical techniques (DSC, TGA, FT-IR, PXRD. It was determined that an appropriate selection of the excipient type and ratio could provide a significant increase in the carbamazepine dissolution rate. By application of analytical techniques, it was found that that the employed excipients induce a transition of carbamazepine into the amorphous form and that the selected sample was stable for three months, when kept under ambient conditions. [Projekat Ministarstva nauke Republike Srbije, br. TR34007

  18. ac impedance, DSC and FT-IR investigations on (x)PVAc-(1 - x)PVdF blends with LiClO4

    International Nuclear Information System (INIS)

    Baskaran, R.; Selvasekarapandian, S.; Kuwata, N.; Kawamura, J.; Hattori, T.

    2006-01-01

    The blended polymer electrolytes comprising poly(vinyl acetate) (PVAc)-poly(vinylidene fluoride) (PVdF) have been prepared for different blend composition with constant lithium perchlorate (LiClO 4 ) ratio by solution casting technique. The formation of the blend polymer electrolyte complex has been confirmed by FT-IR spectroscopy analysis. DSC analysis has been performed in order to observe the change in transition temperature that is caused by the blending of polymers and addition of LiClO 4 . The ac impedance and dielectric spectroscopy studies are carried out on the blended matrix to identify the optimized blend composition, which is having high ionic conductivity. The temperature dependence of conductivity of the polymer electrolytes is found to follow VTF type equation. The high ionic conductivity of 6.4 x 10 -4 S cm -1 at 343 K has been observed for blended polymer electrolyte having blend ratio 75:25 (PVAc:PVdF). The ionic transference number of mobile ions has been estimated by Wagner's polarization method and the value is reported to be t ion is 0.95-0.98 for all the blended samples. The modulus spectra reveal the non-Debye nature and distribution of relaxation times of the samples. The dielectric spectra show the low frequency dispersion, which implies the space charge effects arising from the electrodes

  19. Application of fiber-optic attenuated total reflection-FT-IR methods for in situ characterization of protein delivery systems in real time.

    Science.gov (United States)

    McFearin, Cathryn L; Sankaranarayanan, Jagadis; Almutairi, Adah

    2011-05-15

    A fiber-optic coupled attenuated total reflection (ATR)-FT-IR spectroscopy technique was applied to the study of two different therapeutic delivery systems, acid degradable hydrogels and nanoparticles. Real time exponential release of a model protein, human serum albumin (HSA), was observed from two different polymeric hydrogels formulated with a pH sensitive cross-linker. Spectroscopic examination of nanoparticles formulated with an acid degradable polymer shell and encapsulated HSA exhibited vibrational signatures characteristic of both particle and payload when exposed to lowered pH conditions, demonstrating the ability of this methodology to simultaneously measure phenomena arising from a system with a mixture of components. In addition, thorough characterization of these pH sensitive delivery vehicles without encapsulated protein was also accomplished in order to separate the effects of the payload during degradation. When in situ, real time detection in combination with the ability to specifically identify different components in a mixture without involved sample preparation and minimal sample disturbance is provided, the versatility and suitability of this type of experiment for research in the pharmaceutical field is demonstrated.

  20. Attenuated Total Reflection Fourier Transform Infrared (ATR FT-IR) Spectroscopy as an Analytical Method to Investigate the Secondary Structure of a Model Protein Embedded in Solid Lipid Matrices.

    Science.gov (United States)

    Zeeshan, Farrukh; Tabbassum, Misbah; Jorgensen, Lene; Medlicott, Natalie J

    2018-02-01

    Protein drugs may encounter conformational perturbations during the formulation processing of lipid-based solid dosage forms. In aqueous protein solutions, attenuated total reflection Fourier transform infrared (ATR FT-IR) spectroscopy can investigate these conformational changes following the subtraction of spectral interference of solvent with protein amide I bands. However, in solid dosage forms, the possible spectral contribution of lipid carriers to protein amide I band may be an obstacle to determine conformational alterations. The objective of this study was to develop an ATR FT-IR spectroscopic method for the analysis of protein secondary structure embedded in solid lipid matrices. Bovine serum albumin (BSA) was chosen as a model protein, while Precirol AT05 (glycerol palmitostearate, melting point 58 ℃) was employed as the model lipid matrix. Bovine serum albumin was incorporated into lipid using physical mixing, melting and mixing, or wet granulation mixing methods. Attenuated total reflection FT-IR spectroscopy and size exclusion chromatography (SEC) were performed for the analysis of BSA secondary structure and its dissolution in aqueous media, respectively. The results showed significant interference of Precirol ATO5 with BSA amide I band which was subtracted up to 90% w/w lipid content to analyze BSA secondary structure. In addition, ATR FT-IR spectroscopy also detected thermally denatured BSA solid alone and in the presence of lipid matrix indicating its suitability for the detection of denatured protein solids in lipid matrices. Despite being in the solid state, conformational changes occurred to BSA upon incorporation into solid lipid matrices. However, the extent of these conformational alterations was found to be dependent on the mixing method employed as indicated by area overlap calculations. For instance, the melting and mixing method imparted negligible effect on BSA secondary structure, whereas the wet granulation mixing method promoted

  1. Seguimiento por espectroscopia infrarroja (FT-IR de la copolimerización de TEOS (tetraetilortosilicato y PDMS (polidimetilsiloxano en presencia de tbt (tetrabutiltitanio

    Directory of Open Access Journals (Sweden)

    Téllez, L.

    2004-10-01

    Full Text Available Hybrid materials have been prepared in this work through the reactions of Si and Ti alkoxides (TEOS and TBT, respectively and polydimethil siloxane (PDMS. These reactions have been studied by means of FT-IR spectroscopy during the whole reaction time. The hydrolysis of TEOS molecule has been followed by the 880 cm-1 band, and the self-condensation reactions through the 1180 and 1150 cm-1 bands. Polycondesation reaction between Si-OH groups and PDMS molecules has been followed by the 850 cm-1 band. On the other hand, the hydrolysis reaction of TBT and the self-condensation of Ti-OH groups have been followed by the 1130 and 770-510 cm-1 bands, respectively. Finally the condensation reaction between Si-OH and Ti-OH groups have been studied by the 936 cm-1 band. Results have shown that hydrolysis and condensation reactions are depending on TBT concentration. The formation of Si-O-Si cross-linked structures increases with the TBT concentrations in the reaction. The selfcondensation reaction of Si-OH grups or Ti-OH grous is very reapid forming Si-O-Si and Ti-O-Ti bonds, respectively. However, the Si-O-Ti bonds which are formed during the first moments of reaction are also rapidly broken due to H2O molecules or the reaction medium. The evolution of PDMS linear and cyclic molecules is also studied.

    Se han preparado materiales híbridos por medio de reacciones de hidrólisis y condensación de alcóxidos de Si y Ti (TEOS y TBT, respectivamente y de reacciones de copolimerización de éstos con polidimetilsiloxano (PDMS. Se han estudiado las citadas reacciones mediante espectroscopia FT-IR, desde el mismo comienzo hasta la obtención del material final. La hidrólisis del TEOS así como la autocondensación del os grupos Si-OH generados tanto para formar cadenas entrecruzadas como lineales se han seguido mediante las bandas situadas a 880, 1180 y 1150 cm-1, respectivamente. La policondensación de dichos grupos con PDMS se ha seguido por la banda a

  2. Biological activities of Allium sativum and Zingiber officinale extracts on clinically important bacterial pathogens, their phytochemical and FT-IR spectroscopic analysis.

    Science.gov (United States)

    Awan, Uzma Azeem; Ali, Shaukat; Shahnawaz, Amna Mir; Shafique, Irsa; Zafar, Atiya; Khan, Muhammad Abdul Rauf; Ghous, Tahseen; Saleem, Azhar; Andleeb, Saiqa

    2017-05-01

    The spread of bacterial infectious diseases is a major public threat. Herbs and spices have offered an excellent, important and useful source of antimicrobial agents against many pathological infections. In the current study, the antimicrobial potency of fresh, naturally and commercial dried Allium sativum and Zingiber officinale extracts had been investigated against seven local clinical bacterial isolates such as Escherichia coli, Pseudomonas aeruginosa, Klebsiella pneumonia, Staphylococcus aureus, Streptococcus pyogenes, Staphylococcus epidermidis, and Serratia marcesnces by the agar disc diffusion method. All tested pathogens except P. aeruginosa and E. coli were most susceptible to ethanolic and methanolic extracts of A. sativum. Similarly, chloroform and diethyl ether extracts of Z. officinale showed a greater zone of inhibition of tested pathogens except for P. aeruginosa and E. coli. We found that all extracts of A. sativum and Z. officinale have a strong antibacterial effect compared to recommended standard antibiotics through activity index. All results were evaluated statistically and a significant difference was recorded at Psativum and Z. officinale proposed the presence of various phytochemicals such as tannins, phenols, alkaloids, steroids and saponins. Retention factor of diverse phytochemicals provides a valuable clue regarding their polarity and the selection of solvents for separation of phytochemicals. Significant inhibition of S. aureus was also observed through TLC-Bioautography. FT-IR Spectrometry was also performed to characterize both natural and commercial extracts of A. sativum and Z. officinale to evaluate bioactive compounds. These findings provide new insights to use A. sativum and Z. officinale as potential plant sources for controlling pathogenic bacteria and potentially considered as cost-effective in the management of diseases and to the threat of drug resistance phenomenon.

  3. FT-IR study and solvent-implicit and explicit effect on stepwise tautomerism of Guanylurea: M06-2X as a case of study.

    Science.gov (United States)

    Karimzadeh, Morteza; Manouchehri, Neda; Saberi, Dariush; Niknam, Khodabakhsh

    2018-06-15

    All 66 conformers of guanylurea were optimized and frequency calculations were performed at M06-2X/6-311++G(d,p) level of theory. Theses conformers were categorized into five tautomers, and the most stable conformer of each tautomer were found. Geometrical parameters indicated that these tautomers have almost planar structure. Complete stepwise tautomerism were studied through both intramolecular proton transfer routs and internal rotations. Results indicated that the proton transfer routs involving four-membered heterocyclic structures were rate-determining steps. Also, intramolecular proton movement having six-membered transition state structures had very low energy barrier comparable to the transition states of internal rotation routs. Differentiation of studied tautomers could easily be done through their FT-IR spectra in the range of 3200 to 3900cm -1 by comparing absorption bands and intensity of peaks. Solvent-implicit effects on the stability of tautomers were also studied through re-optimization and frequency calculation in four solvents. Water, DMSO, acetone and toluene had stabilization effect on all considered tautomers, but the order of stabilization effect was as follows: water>DMSO>acetone>toluene. Finally, solvent-explicit, base-explicit and acid-explicit effect were also studied by taking place of studied tautomer nearside of acid, base or solvent and optimization of them. Frequency calculation for proton movement by contribution of explicit effect showed that formic acid had a very strong effect on proton transfer from tautomer A1 to tautomer D8 by lowering the energy barrier from 42.57 to 0.8kcal/mol. In addition, ammonia-explicit effect was found to lower the barrier from 42.57 to 22.46kcal/mol, but this effect is lower than that of water and methanol-explicit effect. Copyright © 2018 Elsevier B.V. All rights reserved.

  4. FT-IR study and solvent-implicit and explicit effect on stepwise tautomerism of Guanylurea: M06-2X as a case of study

    Science.gov (United States)

    Karimzadeh, Morteza; Manouchehri, Neda; Saberi, Dariush; Niknam, Khodabakhsh

    2018-06-01

    All 66 conformers of guanylurea were optimized and frequency calculations were performed at M06-2X/6-311++G(d,p) level of theory. Theses conformers were categorized into five tautomers, and the most stable conformer of each tautomer were found. Geometrical parameters indicated that these tautomers have almost planar structure. Complete stepwise tautomerism were studied through both intramolecular proton transfer routs and internal rotations. Results indicated that the proton transfer routs involving four-membered heterocyclic structures were rate-determining steps. Also, intramolecular proton movement having six-membered transition state structures had very low energy barrier comparable to the transition states of internal rotation routs. Differentiation of studied tautomers could easily be done through their FT-IR spectra in the range of 3200 to 3900 cm-1 by comparing absorption bands and intensity of peaks. Solvent-implicit effects on the stability of tautomers were also studied through re-optimization and frequency calculation in four solvents. Water, DMSO, acetone and toluene had stabilization effect on all considered tautomers, but the order of stabilization effect was as follows: water > DMSO > acetone > toluene. Finally, solvent-explicit, base-explicit and acid-explicit effect were also studied by taking place of studied tautomer nearside of acid, base or solvent and optimization of them. Frequency calculation for proton movement by contribution of explicit effect showed that formic acid had a very strong effect on proton transfer from tautomer A1 to tautomer D8 by lowering the energy barrier from 42.57 to 0.8 kcal/mol. In addition, ammonia-explicit effect was found to lower the barrier from 42.57 to 22.46 kcal/mol, but this effect is lower than that of water and methanol-explicit effect.

  5. Comprehensive GC–FID, GC–MS and FT-IR spectroscopic analysis of the volatile aroma constituents of Artemisia indica and Artemisia vestita essential oils

    Directory of Open Access Journals (Sweden)

    Manzoor A. Rather

    2017-05-01

    Full Text Available In the current study, the leaf volatile constituents of the essential oils of Artemisia indica Willd. and Artemisia vestita Wall were studied using a combination of capillary GC–FID, GC–MS and FT-IR (Fourier-Transform Infra-Red analytical techniques. The analysis led to the identification of 42 compounds in the essential oil of A. indica, representing 96.6% of the essential oil and the major components were found to be artemisia ketone (42.1%, germacrene D (8.6%, borneol (6.1% and cis-chrysanthenyl acetate (4.8%. The essential oil was dominated by the presence of oxygenated monoterpenes constituting 65.2% of the total oil composition followed by sesquiterpene hydrocarbons and monoterpene hydrocarbons constituting 15.7% and 10.7%, respectively of the total oil composition. The essential oil composition of A. vestita was found to contain a total of 18 components representing 94.2% of the total oil composition. The principal components were found to be 1,8-cineole (46.8%, (E-citral (13.7%, limonene (9.8%, α-phellandrene (6.4%, camphor (5.0%, (Z and (E-thujones (3.0% each. Oxygenated monoterpenes were the dominant group of terpenes in the essential oil constituting 73.1% of the total oil composition followed by monoterpene hydrocarbons (17.3%. The results of the current study reveal remarkable differences in the essential oil compositions of these two Artemisia species already reported in the literature from other parts of the globe.

  6. Solvent-Mediated Eco-Friendly Synthesis and Characterization of Monodispersed Bimetallic Ag/Pd Nano composites for Sensing and Raman Scattering Applications

    International Nuclear Information System (INIS)

    Sathiyadevi, G.; Loganathan, B.; Karthikeyan, B.; Karthikeyan, B.

    2014-01-01

    The solvent-mediated eco-friendly monodispersed Ag/Pd bimetallic nano composites (BNCs) having thick core and thin shell have been prepared through novel green chemical solvent reduction method. Reducing solvent, dimethyl formamide (DMF) is employed for the controlled green synthesis. Characterization of the synthesized Ag/Pd BNCs has been done by x-ray diffraction (XRD) studies, high-resolution scanning electron microscopy (HR-SEM), energy-dispersive X-ray analysis (EDX), and high-resolution transmission electron microscopy (HR-TEM) with selected area electron diffraction (SAED) pattern. The nature of the interaction of L-cysteine with Ag/Pd BNCs has been studied by using surface plasmon spectroscopy, Fourier transform-infrared spectroscopy (FT-IR), cyclic voltammetry (CV), and theoretical methods.

  7. Determinação quantitativa da concentração de silicone em antiespumantes por espectroscopia FT-IR / ATR e calibração multivariada Quantitative determination of silicone in antifoaming products by FT-IR / ATR spectroscopy and multivariate calibration

    Directory of Open Access Journals (Sweden)

    Marcelo H. F. Garcia

    2004-12-01

    Full Text Available Neste trabalho apresentamos uma alternativa para a dosagem do teor de silicone (polidimetilsiloxano em antiespumantes por meio da técnica de espectroscopia no infravermelho com transformada de Fourier (FT-IR, com a utilização do acessório de reflectância total atenuada (ATR. Os espectros foram registrados na faixa espectral de 2500 a 780 cm-1, com resolução de 4 cm-1 e 128 varreduras. A calibração de um modelo linear por meio da utilização do método de mínimos quadrados parciais (PLS aplicado aos espectros foi capaz de determinar satisfatoriamente a concentração de silicone nas amostras. Este método é de extrema importância para indústrias produtoras de antiespumantes siliconados, uma vez que o desempenho de tais produtos geralmente é avaliado em função da viscosidade dos mesmos. Muitas vezes no processo de fabricação de tais produtos ocorre uma homogeneização incompleta do silicone no solvente, o que leva a resultados de viscosidade que não são representativos das amostras analisadas. A determinação da concentração do teor de silicone é uma importante ferramenta para o Controle Estatístico de Processo (CEP, pois evita o desperdício de matérias-primas empregadas na fabricação dos antiespumantes.This work presents an alternative method to determine the concentration of silicone (polydimethylsiloxane in antifoaming products using Fourier Transformed Infrared Spectroscopy (FT-IR with the attenuated total reflectance (ATR accessory. The spectra were recorded in the range from 2500 to 780 cm-1, with a resolution of 4 cm-1 and 128 scans. With calibration of a linear model using PLS regression method applied to spectral data we were able to determine the silicone concentration in the samples. This method may be useful for antifoaming producers since the performance of such products generally is evaluated as a function of their viscosity. Moreover, during manufacturing an incomplete homogenization of silicone in the

  8. Synthesis, structural and vibrational investigation on 2-phenyl-N-(pyrazin-2-yl)acetamide combining XRD diffraction, FT-IR and NMR spectroscopies with DFT calculations.

    Science.gov (United States)

    Lukose, Jilu; Yohannan Panicker, C; Nayak, Prakash S; Narayana, B; Sarojini, B K; Van Alsenoy, C; Al-Saadi, Abdulaziz A

    2015-01-25

    The optimized molecular structure, vibrational frequencies, corresponding vibrational assignments of 2-phenyl-N-(pyrazin-2-yl)acetamide have been investigated experimentally and theoretically using Gaussian09 software package. The title compound was optimized by using the HF/6-31G(6D,7F) and B3LYP/6-31G(6D,7F) calculations. The geometrical parameters are in agreement with the XRD data. The stability of the molecule arising from hyper-conjugative interaction and charge delocalization has been analyzed using NBO analysis. Gauge-including atomic orbital (1)H-NMR chemical shifts calculations were carried out and compared with experimental data. The HOMO and LUMO analysis is used to determine the charge transfer within the molecule. Molecular electrostatic potential was performed by the DFT method. First hyperpolarizability is calculated in order to find its role in non linear optics. From the XRD data, in the crystal, molecules are held together by strong C-H⋯O and N-H⋯O intermolecular interactions. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Synthesis, spectroscopic analyses (FT-IR and NMR), vibrational study, chemical reactivity and molecular docking study and anti-tubercular activity of condensed oxadiazole and pyrazine derivatives

    Science.gov (United States)

    El-Azab, Adel S.; Mary, Y. Sheena; Abdel-Aziz, Alaa A. M.; Miniyar, Pankaj B.; Armaković, Stevan; Armaković, Sanja J.

    2018-03-01

    The Fourier transform infrared spectra of the compounds 2-(5-phenyl-1,3,4-oxadiazol-2-yl)pyrazine (PHOXPY), 2-(5-styryl-1,3,4-oxadiazol-2-yl)pyrazine (STOXPY) and 2-(5-(furan-2-yl)-1,3,4-oxadiazol-2-yl)pyrazine (FUOXPY) have been recorded and the wavenumbers are computed at the density functional theory level. The assignments of all the fundamental bands of each molecule are made using potential energy distribution. The computed values of dipole moment, polarizability and hyperpolarizability values indicate that the title molecules exhibit NLO properties. The HOMO and LUMO energies demonstrate the chemical stability of the molecules and NBO analysis is made to study the stability of molecules arising from hyper conjugative interactions and charge delocalization. Detailed computational analysis and spectroscopic characterization has been performed for three newly synthesized oxadiazole derivatives. Obtained computational and experimental results have been mutually compared in order to understand the influence of structural parts specific for each derivative. From the MIC determination, MTb H37Rv was found to be sensitive to compounds, PHOXPY, STOXPY and FUOXPY. The results obtained from anti-TB activity are more promising as the compounds were found to be more potent than reference standards, streptomycin and pyrazinamide. Efforts were made in order to predict both global and local reactive properties of the title oxadiazole derivatives, including their sensitivity towards autoxidation mechanism and influence of water. The results obtained from anti-TB activity are more promising for the title compounds. Interaction with representative protein Pterindeaminase inhibitor asricin A was also investigated using the molecular docking procedure. The docked ligands form stable complexes with the receptor ricin A and the docking results suggest that these compounds can be developed as new anti-cancer drugs.

  10. Synthesis of biodiesel from rocket seed oil and its characterization by FT-IR, NMR (/sup 1/H and /sup 13/C) and GC-MS

    International Nuclear Information System (INIS)

    Khalid, N.

    2012-01-01

    The limited resources of fossil fuel, increasing prices of crude oils and environmental concerns have motivated the researcher for alternate fuels, such as bio diesel that is obtained from vegetable oils. Therefore, bio diesel was synthesized from Rocket seed oil by base catalyzed transesterification with methanol. The physical parameters like dynamic viscosity (3.88 cp), specific gravity (0.893 g cm/sup 3/), kinematic viscosity (5.85 mm/sup 2/s/sup 1/)), density (0.877 g cm/sup 3/), cloud point (3 deg. C), flash point (110 deg. C) and acid number (0.07 mg KOH g/sup 1/) of the synthesized rocket seed oil bio diesel (RSOB) were determined and were found to be comparable with ASTM recommended values for diesels. Chemical composition of the bio diesels formed was determined by various techniques like Fourier transform infrared (FTIR) spectroscopy, nuclear magnetic resonance (NMR) spectroscopy (/sup 1/H, 13/C) and gas chromatography-mass spectrometry (GCMS). The /sup 1/H NMR spectrum of RSOB is given. (Orig./A.B.)

  11. Synthesis and XRD, FT-IR vibrational, UV-vis, and nonlinear optical exploration of novel tetra substituted imidazole derivatives: A synergistic experimental-computational analysis

    Science.gov (United States)

    Ahmad, Muhammad Saeed; Khalid, Muhammad; Shaheen, Muhammad Ashraf; Tahir, Muhammad Nawaz; Khan, Muhammad Usman; Braga, Ataualpa Albert Carmo; Shad, Hazoor Ahmad

    2018-04-01

    Heterocyclic compounds have potential applications in many fields of life. We synthesized novel tetra substituted imidazoles by four-component condensation of benzil, substituted aldehydes, substituted anilines and ammonium acetate as a source of ammonia and acetic acid as the solvent. Their chemical structures were resolved through X-ray crystallographic and spectroscopic (Fourier transform IR and UV-vis) techniques. In addition to experimental analysis, density functional theory (DFT) calculations at the B3LYP/6-311 + G(d,p) level were performed on 4-bromo-2-(1-(4-methoxyphenyl)-4,5-diphenyl-1H-imidazole-2-yl)phenol (1), 4-bromo-2-(1-(1-naphthalen-yl)-4,5-diphenyl-1H-imidazole-2-yl)phenol (2), and 2-(1-(2-chlorophenyl)-4,5-diphenyl-1-H-imidazole-2-yl)-6-methoxyphenol (3) to obtain the optimized geometry and spectroscopic (Fourier transform IR and UV-vis) and non-linear optical properties. Frontier molecular orbital analysis was performed at the Hartee-Fock/6-311+g(d,p) and DFT/B3LYP/6-311+G(d,p) levels of theory. Natural bond orbital (NBO) and UV-vis spectral analyses were performed at the M06-2X/6-31+G(d,p) and time-dependent DFT/B3LYP/6-311+G(d,p) levels, respectively. Overall, the DFT findings show good agreement with the experimental data. The hyper conjugative interaction network, which is responsible for the stability of compounds 1, 2 and 3 was explored by the NBO approach. The global reactivity parameters were explored with use of the energy of the frontier molecular orbitals. DFT calculations predict the first-order hyperpolarizabilities of compounds 1, 2 and 3 are 294.89 × 10-30, 219.45 × 10-30 and 146.77 × 10-30 esu, respectively. A two-state model was used to describe the non-linear optical properties of the compounds investigated.

  12. Synthesis, physicochemical and optical properties of bis-thiosemicarbazone functionalized graphene oxide

    Science.gov (United States)

    Kumar, Santosh; Wani, Mohmmad Y.; Arranja, Claudia T.; Castro, Ricardo A. E.; Paixão, José A.; Sobral, Abilio J. F. N.

    2018-01-01

    Fluorescent materials are important for low-cost opto-electronic and biomedical sensor devices. In this study we present the synthesis and characterization of graphene modified with bis-thiosemicarbazone (BTS). This new material was characterized using Fourier transform infrared spectroscopy (FT-IR), Ultraviolet-visible (UV-Vis) and Raman spectroscopy techniques. Further evaluation by X-ray diffraction (XRD), thermo-gravimetric analysis (TGA), differential scanning calorimetry (DSC), scanning electron microscopy (SEM) and atomic-force microscopy (AFM) allowed us to fully characterize the morphology of the fabricated material. The average height of the BTSGO sheet is around 10 nm. Optical properties of BTSGO evaluated by photoluminescence (PL) spectroscopy showed red shift at different excitation wavelength compared to graphene oxide or bisthiosemicarbazide alone. These results strongly suggest that BTSGO material could find potential applications in graphene based optoelectronic devices.

  13. Low temperature FT-IR and molecular orbital study of N,N-dimethylglycine methyl ester: Proof for different ground conformational states in gas phase and in condensed media

    OpenAIRE

    Gómez-Zavaglia, A.; Fausto, R.

    2002-01-01

    N,N-dimethylglycine methyl ester (DMG-Me) was studied by FT-IR spectroscopy under several experimental conditions, including low temperature solid state and isolated in low temperature inert gas matrices, and by molecular orbital calculations. In agreement with the theoretical predictions, the experimental data show that in the gaseous phase the most stable conformer (ASC) has the ester group in cis configuration and the N–C–CO and Lp–N–C–C (Lp=lone electron pair) dihedral angles equal to 0° ...

  14. Templated green synthesis of plasmonic silver nanoparticles in onion epidermal cells suitable for surface-enhanced Raman and hyper-Raman scattering

    DEFF Research Database (Denmark)

    Palanco, Marta Espina; Mogensen, Klaus Bo; Guehlke, Marina

    2016-01-01

    We report fast and simple green synthesis of plasmonic silver nanoparticles in the epidermal cells of onions after incubation with AgNO3 solution. The biological environment supports the generation of silver nanostructures in two ways. The plant tissue delivers reducing chemicals for the initial...... for one-and two-photon-excited spectroscopy such as surface enhanced Raman scattering (SERS) and surface enhanced hyper-Raman scattering (SEHRS). Our studies demonstrate a templated green preparation of enhancing plasmonic nanoparticles and suggest a new route to deliver silver nanoparticles as basic...... building blocks of plasmonic nanosensors to plants by the uptake of solutions of metal salts....

  15. Comparison between infrared and Raman spectroscopic analysis of maturing rabbit cortical bone.

    Science.gov (United States)

    Turunen, Mikael J; Saarakkala, Simo; Rieppo, Lassi; Helminen, Heikki J; Jurvelin, Jukka S; Isaksson, Hanna

    2011-06-01

    The molecular composition of the organic and inorganic matrices of bone undergoes alterations during maturation. The aim of this study was to compare Fourier transform infrared (FT-IR) and near-infrared (NIR) Raman microspectroscopy techniques for characterization of the composition of growing and developing bone from young to skeletally mature rabbits. Moreover, the specificity and differences of the techniques for determining bone composition were clarified. The humeri of female New Zealand White rabbits, with age range from young to skeletally mature animals (four age groups, n = 7 per group), were studied. Spectral peak areas, intensities, and ratios related to organic and inorganic matrices of bone were analyzed and compared between the age groups and between FT-IR and Raman microspectroscopic techniques. Specifically, the degree of mineralization, type-B carbonate substitution, crystallinity of hydroxyapatite (HA), mineral content, and collagen maturity were examined. Significant changes during maturation were observed in various compositional parameters with one or both techniques. Overall, the compositional parameters calculated from the Raman spectra correlated with analogous parameters calculated from the IR spectra. Collagen cross-linking (XLR), as determined through peak fitting and directly from the IR spectra, were highly correlated. The mineral/matrix ratio in the Raman spectra was evaluated with multiple different peaks representing the organic matrix. The results showed high correlation with each other. After comparison with the bone mineral density (BMD) values from micro-computed tomography (micro-CT) imaging measurements and crystal size from XRD measurements, it is suggested that Raman microspectroscopy is more sensitive than FT-IR microspectroscopy for the inorganic matrix of the bone. In the literature, similar spectroscopic parameters obtained with FT-IR and NIR Raman microspectroscopic techniques are often compared. According to the present

  16. Fourier Transform Infrared (FT-IR) and Laser Ablation Inductively Coupled Plasma-Mass Spectrometry (LA-ICP-MS) Imaging of Cerebral Ischemia: Combined Analysis of Rat Brain Thin Cuts Toward Improved Tissue Classification.

    Science.gov (United States)

    Balbekova, Anna; Lohninger, Hans; van Tilborg, Geralda A F; Dijkhuizen, Rick M; Bonta, Maximilian; Limbeck, Andreas; Lendl, Bernhard; Al-Saad, Khalid A; Ali, Mohamed; Celikic, Minja; Ofner, Johannes

    2018-02-01

    Microspectroscopic techniques are widely used to complement histological studies. Due to recent developments in the field of chemical imaging, combined chemical analysis has become attractive. This technique facilitates a deepened analysis compared to single techniques or side-by-side analysis. In this study, rat brains harvested one week after induction of photothrombotic stroke were investigated. Adjacent thin cuts from rats' brains were imaged using Fourier transform infrared (FT-IR) microspectroscopy and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The LA-ICP-MS data were normalized using an internal standard (a thin gold layer). The acquired hyperspectral data cubes were fused and subjected to multivariate analysis. Brain regions affected by stroke as well as unaffected gray and white matter were identified and classified using a model based on either partial least squares discriminant analysis (PLS-DA) or random decision forest (RDF) algorithms. The RDF algorithm demonstrated the best results for classification. Improved classification was observed in the case of fused data in comparison to individual data sets (either FT-IR or LA-ICP-MS). Variable importance analysis demonstrated that both molecular and elemental content contribute to the improved RDF classification. Univariate spectral analysis identified biochemical properties of the assigned tissue types. Classification of multisensor hyperspectral data sets using an RDF algorithm allows access to a novel and in-depth understanding of biochemical processes and solid chemical allocation of different brain regions.

  17. Combining TXRF, FT-IR and GC-MS information for identification of inorganic and organic components in black pigments of rock art from Alero Hornillos 2 (Jujuy, Argentina).

    Science.gov (United States)

    Vázquez, Cristina; Maier, Marta S; Parera, Sara D; Yacobaccio, Hugo; Solá, Patricia

    2008-06-01

    Archaeological samples are complex in composition since they generally comprise a mixture of materials submitted to deterioration factors largely dependent on the environmental conditions. Therefore, the integration of analytical tools such as TXRF, FT-IR and GC-MS can maximize the amount of information provided by the sample. Recently, two black rock art samples of camelid figures at Alero Hornillos 2, an archaeological site located near the town of Susques (Jujuy Province, Argentina), were investigated. TXRF, selected for inorganic information, showed the presence of manganese and iron among other elements, consistent with an iron and manganese oxide as the black pigment. Aiming at the detection of any residual organic compounds, the samples were extracted with a chloroform-methanol mixture and the extracts were analyzed by FT-IR, showing the presence of bands attributable to lipids. Analysis by GC-MS of the carboxylic acid methyl esters prepared from the sample extracts, indicated that the main organic constituents were saturated (C(16:0) and C(18:0)) fatty acids in relative abundance characteristic of degraded animal fat. The presence of minor C(15:0) and C(17:0) fatty acids and branched-chain iso-C(16:0) pointed to a ruminant animal source.

  18. The Synthesis and Physical Properties of Magnesium Borate Mineral of Admontite Synthesized from Sodium Borates

    Directory of Open Access Journals (Sweden)

    Azmi Seyhun Kipcak

    2014-01-01

    Full Text Available Magnesium borates are significant compounds due to their advanced mechanical and thermal durability properties. This group of minerals can be used in ceramic industry, in detergent industry, and as neutron shielding material, phosphor of thermoluminescence by dint of their extraordinary specialties. In the present study, the synthesis of magnesium borate via hydrothermal method from sodium borates and physical properties of synthesized magnesium borate minerals were investigated. The characterization of the products was carried out by X-ray diffraction (XRD, Fourier transform infrared (FT-IR and Raman spectroscopies, and differential thermal analysis and thermal gravimetry (DTA/TG. The surface morphology was examined by scanning electron microscopy (SEM. B2O3 content was determined through titration. The electrical resistivity/conductivity properties of products were measured by Picoammeter Voltage Source. UV-vis spectrometer was used to investigate optical absorption characteristics of synthesized minerals in the range 200–1000 nm at room temperature. XRD results identified the synthesized borate minerals as admontite [MgO(B2O33·7(H2O] with code number “01-076-0540” and mcallisterite [Mg2(B6O7(OH62·9(H2O] with code number “01-070-1902.” The FT-IR and Raman spectra of the obtained samples were similar with characteristic magnesium borate bands. The investigation of the SEM images remarked that both nano- and microscale minerals were produced. The reaction yields were between 75.1 and 98.7%.

  19. Solid-State synthesis of POPD@AgNPs nanocomposites for electrochemical sensors

    CSIR Research Space (South Africa)

    Paulraj, P

    2017-07-01

    Full Text Available techniques. POPD and POPD@AgNPs were characterized using HR-TEM, FE-SEM, XRD, UV-Visible, FT-IR, Micro Raman spectroscopy and those results were confirmed their chemical purity, particle size, shape and its elemental compositions. Moreover, the DPV...

  20. Characterization of Archaeological Sediments Using Fourier Transform Infrared (FT-IR) and Portable X-ray Fluorescence (pXRF): An Application to Formative Period Pyro-Industrial Sites in Pacific Coastal Southern Chiapas, Mexico.

    Science.gov (United States)

    Neff, Hector; Bigney, Scott J; Sakai, Sachiko; Burger, Paul R; Garfin, Timothy; George, Richard G; Culleton, Brendan J; Kennett, Douglas J

    2016-01-01

    Archaeological sediments from mounds within the mangrove zone of far-southern Pacific coastal Chiapas, Mexico, are characterized in order to test the hypothesis that specialized pyro-technological activities of the region's prehistoric inhabitants (salt and ceramic production) created the accumulations visible today. Fourier transform infrared spectroscopy (FT-IR) is used to characterize sediment mineralogy, while portable X-ray fluorescence (pXRF) is used to determine elemental concentrations. Elemental characterization of natural sediments by both instrumental neutron activation analysis (INAA) and pXRF also contribute to understanding of processes that created the archaeological deposits. Radiocarbon dates combined with typological analysis of ceramics indicate that pyro-industrial activity in the mangrove zone peaked during the Late Formative and Terminal Formative periods, when population and monumental activity on the coastal plain and piedmont were also at their peaks. © The Author(s) 2015.

  1. Synthesis and investigation of PMMA films with homogeneously dispersed multiwalled carbon nanotubes

    International Nuclear Information System (INIS)

    Pantoja-Castro, M.A.; Pérez-Robles, J.F.; González-Rodríguez, H.; Vorobiev-Vasilievitch, Y.; Martínez-Tejada, H.V.; Velasco-Santos, C.

    2013-01-01

    Multiwalled carbon nanotubes (MWNT) modified by 2.2′-azoiso-butyronitrile (AIBN) were incorporated into methyl methacrylate (MMA) by sonochemistry method, resulting in homogenous dispersion of MWNT, which makes possible to obtain flexible conductive polymer-matrix nanocomposites films of PMMA, with MWNT concentrations ranging from 0 to 0.5 wt%. Modified MWNT (AIBN-MWNT) were studied by Fourier transform infrared (FT-IR), Raman spectroscopy, X-ray Photoelectron Spectroscopy (XPS) and through visual observations in order to compare the dispersion in 2-propanone and toluene with that of pristine MWNT. Synthesized PMMA-AIBN-MWNT films were studied by FT-IR and Raman spectroscopy. Using FT-IR for the AIBN-MWNT it was not possible to identify any group or groups attached to the nanotubes. Raman spectroscopy shows a small modification in the Lorentzian peaks ratio I D/G of AIBN-MWNT, meanwhile XPS showed that atomic compositions does not change for AIBN-MWNT compared to the pristine nanotubes. Also by impedance it was analyzed the conductivity of PMMA-MWNT films and the results showed a threshold percolation at 0.5 wt%. FT-IR and Raman analyses for PMMA-AIBN-MWNT composite indicate a covalent bonding between PMMA and MWNT due to the opening of π-bonds of the nanotubes, which is related with a possible proposed reaction scheme. - Graphical abstract: Display Omitted - Highlights: • We used sonochemistry-in situ polymerization to disperse MWNT very soon in PMMA. • A high and homogenous dispersion of MWNT in PMMA was achieved. • The modification of MWNT by AIBN was analyzed using Raman. • A covalent bonding between PMMA and MWNT was analyzed by FT-IR and Raman. • According to the results of PMMA-MWNT it was proposed a scheme reaction

  2. Synthesis and investigation of PMMA films with homogeneously dispersed multiwalled carbon nanotubes

    Energy Technology Data Exchange (ETDEWEB)

    Pantoja-Castro, M.A., E-mail: m_pantojaq@yahoo.com.mx [Facultad de Ingeniería Química, Universidad Michoacana de San Nicolás de Hidalgo, Av. J. Múgica S/N Col., Villa Universidad, CP 58040 Morelia, Michoacán (Mexico); Pérez-Robles, J.F. [Centro de Investigación y de Estudios Avanzados del IPN, Unidad Querétaro, Libramiento Norponiente #2000, Fracc. Real de Juriquilla, CP 76230 Querétaro (Mexico); González-Rodríguez, H. [Facultad de Ingeniería Química, Universidad Michoacana de San Nicolás de Hidalgo, Av. J. Múgica S/N Col., Villa Universidad, CP 58040 Morelia, Michoacán (Mexico); Vorobiev-Vasilievitch, Y. [Centro de Investigación y de Estudios Avanzados del IPN, Unidad Querétaro, Libramiento Norponiente #2000, Fracc. Real de Juriquilla, CP 76230 Querétaro (Mexico); Martínez-Tejada, H.V. [Instituto de Energía, Materiales y Medio Ambiente, Universidad Pontificia Bolivariana, Circular 1 No. 70-01, Bloque 22, Medellín (Colombia); Velasco-Santos, C. [Centro de Física Aplicada y Tecnología Avanzada, Universidad Autónoma de México, Av. Boulevard Juriquilla, No. 3001 Juriquilla, CP 76230 Querétaro (Mexico)

    2013-07-15

    Multiwalled carbon nanotubes (MWNT) modified by 2.2′-azoiso-butyronitrile (AIBN) were incorporated into methyl methacrylate (MMA) by sonochemistry method, resulting in homogenous dispersion of MWNT, which makes possible to obtain flexible conductive polymer-matrix nanocomposites films of PMMA, with MWNT concentrations ranging from 0 to 0.5 wt%. Modified MWNT (AIBN-MWNT) were studied by Fourier transform infrared (FT-IR), Raman spectroscopy, X-ray Photoelectron Spectroscopy (XPS) and through visual observations in order to compare the dispersion in 2-propanone and toluene with that of pristine MWNT. Synthesized PMMA-AIBN-MWNT films were studied by FT-IR and Raman spectroscopy. Using FT-IR for the AIBN-MWNT it was not possible to identify any group or groups attached to the nanotubes. Raman spectroscopy shows a small modification in the Lorentzian peaks ratio I{sub D/G} of AIBN-MWNT, meanwhile XPS showed that atomic compositions does not change for AIBN-MWNT compared to the pristine nanotubes. Also by impedance it was analyzed the conductivity of PMMA-MWNT films and the results showed a threshold percolation at 0.5 wt%. FT-IR and Raman analyses for PMMA-AIBN-MWNT composite indicate a covalent bonding between PMMA and MWNT due to the opening of π-bonds of the nanotubes, which is related with a possible proposed reaction scheme. - Graphical abstract: Display Omitted - Highlights: • We used sonochemistry-in situ polymerization to disperse MWNT very soon in PMMA. • A high and homogenous dispersion of MWNT in PMMA was achieved. • The modification of MWNT by AIBN was analyzed using Raman. • A covalent bonding between PMMA and MWNT was analyzed by FT-IR and Raman. • According to the results of PMMA-MWNT it was proposed a scheme reaction.

  3. Synthesis and characterization of nano-crystalline Ce1-xGd xO2-x/2 (x = 0-0.30) solid solutions

    DEFF Research Database (Denmark)

    Jadhav, L. D.; Chourashiya, M. G.; Jamale, A. P.

    2010-01-01

    glycine-nitrate process (GNP) has been presented. Evolution of structural and morphological properties of nano-powders as a function of heat treatment has also been studied. The prepared samples were characterized using TG-DTA, FT-IR, Raman spectroscopy, XRD, SEM, etc. In addition, the effect of Gd......In recent years, doped ceria is an established and promising candidate as solid electrolyte for intermediate temperature solid oxide fuel cell (IT-SOFC). In this investigation, synthesis and characterizations of nano-crystalline Gd doped ceria, (Ce1-xGdxO2-x/2, where x = 0-0.3), prepared using...... of sintered samples was observed to hinder with an increase in Gd content....

  4. Rapid and simple determination of polyphyllin I, II, VI, and VII in different harvest times of cultivated Paris polyphylla Smith var. yunnanensis (Franch.) Hand.-Mazz by UPLC-MS/MS and FT-IR.

    Science.gov (United States)

    Wu, Zhe; Zhang, Ji; Xu, Furong; Wang, Yuanzhong; Zhang, Jinyu

    2017-01-01

    Paris Polyphylla Smith var. yunnanensis (Franch.) Hand.-Mazz ("Dian Chonglou" in Chinese) is a famous herbal medicine in China, which is usually well known for activities of anti-cancer, hemolysis, and cytotoxicity. In this study, Fourier transform infrared (FT-IR) spectroscopy coupled with principal component analysis (PCA) and partial least-squares regression (PLSR) was applied to discriminate samples of P. polyphylla var. yunnanensis harvested in different years and determine the content of polyphyllin I, II, VI, and VII in P. polyphylla var. yunnanensis. Meanwhile, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was used to study the dynamic changes of P. polyphylla var. yunnanensis harvested in different years (4, 5, 7, 8, 9, 12, and 13 years old). According to the UPLC-MS/MS result, the optimum harvest time of P. polyphylla var. yunnanensis is 8 years, due to the highest yield of four active components. By the PCA model, P. polyphylla var. yunnanensis could be exactly discriminated, except that two 8-year-old samples were misclassified as 9-year-old samples. For the prediction of polyphyllin I, II, VI, and VII, the quantitative results are satisfactory, with a high value for the determination coefficient (R 2 ) and low values for the root-mean-square error of estimation (RMSEE), root-mean-square error of cross-validation (RMSECV), and root-mean-square error of prediction (RMSEP). In conclusion, FT-IR combined with chemometrics is a promising method to accurately discriminate samples of P. polyphylla var. yunnanensis harvested in different years and determine the content of polyphyllin I, II, VI, and VII in P. polyphylla var. yunnanensis.

  5. Synthesis of gold nanoflowers using deep eutectic solvent with high surface enhanced Raman scattering properties

    Science.gov (United States)

    Aghakhani Mahyari, Farzaneh; Tohidi, Maryam; Safavi, Afsaneh

    2016-09-01

    A facile, seed-less and one-pot method was developed for synthesis of gold nanoflowers with multiple tips through reduction of HAuCl4 with deep eutectic solvent at room temperature. This solvent is eco-friendly, low-cost, non-toxic and biodegradable and can act as both reducing and shape-controlling agent. In this protocol, highly branched and stable gold nanoflowers were obtained without using any capping agent. The obtained products were characterized by different techniques including, field emission scanning electron microscopy, transmission electron microscopy, x-ray diffraction and UV-vis spectroscopy. The as-prepared gold nanoflowers exhibit efficient surface-enhanced Raman scattering (SERS) properties which can be used as excellent substrates for SERS.

  6. Sonochemical-assisted magnesium borate synthesis from different boron sources

    Directory of Open Access Journals (Sweden)

    Yildirim Meral

    2017-03-01

    Full Text Available In this study, sonochemical-assisted magnesium borate synthesis is studied from different boron sources. Various reaction parameters are successfully applied by a simple and green method. X-ray diffraction (XRD, Fourier transform infrared (FT-IR and Raman spectroscopies are used to characterize the synthesized magnesium borates on the other hand surface morphologies are investigated by using scanning electron microscope (SEM. The XRD analyses showed that the products were admontite [MgO(B2O33 · 7(H2O] with JCPDS (Joint Committee on Powder Diffraction Standards no. of 01-076-0540 and mcallisterite [Mg2(B6O7(OH62 · 9(H2O] with JCPDS no. of 01-070-1902. The results that found in the spectroscopic studies were in a good agreement with characteristic magnesium borate bands in both regions of infra-red and visible. According to SEM results, obtained borates were in micro and sub-micro scales. By the use of ultrasonication, reaction yields were found between 84.2 and 97.9%. As a result, it is concluded that the sonochemical approach is a practicable synthesis method to get high efficiency and high crystallinity in the synthesis magnesium borate compounds.

  7. Size-controlled synthesis of biodegradable nanocarriers for targeted ...

    Indian Academy of Sciences (India)

    Research for synthesis of size-controlled carriers is currently challenging one. In this research paper, a ... There are many methods available for the prepara- tion of drug-loaded ... 2.3 Characterization of nanoparticles. 2.3a FT-IR spectral ...

  8. Using ATR-FT/IR to detect carbohydrate-related molecular structure features of carinata meal and their in situ residues of ruminal fermentation in comparison with canola meal

    Science.gov (United States)

    Xin, Hangshu; Yu, Peiqiang

    2013-10-01

    There is no information on the co-products from carinata bio-fuel and bio-oil processing (carinata meal) in molecular structural profiles mainly related to carbohydrate biopolymers in relation to ruminant nutrition. Molecular analyses with Fourier transform infrared spectroscopy (FT/IR) technique with attenuated total reflectance (ATR) and chemometrics enable to detect structural features on a molecular basis. The objectives of this study were to: (1) determine carbohydrate conformation spectral features in original carinata meal, co-products from bio-fuel/bio-oil processing; and (2) investigate differences in carbohydrate molecular composition and functional group spectral intensities after in situ ruminal fermentation at 0, 12, 24 and 48 h compared to canola meal as a reference. The molecular spectroscopic parameters of carbohydrate profiles detected were structural carbohydrates (STCHO, mainly associated with hemi-cellulosic and cellulosic compounds; region and baseline ca. 1483-1184 cm-1), cellulosic compounds (CELC, region and baseline ca. 1304-1184 cm-1), total carbohydrates (CHO, region and baseline ca. 1193-889 cm-1) as well as the spectral ratios calculated based on respective spectral intensity data. The results showed that the spectral profiles of carinata meal were significantly different from that of canola meal in CHO 2nd peak area (center at ca. 1091 cm-1, region: 1102-1083 cm-1) and functional group peak intensity ratios such as STCHO 1st peak (ca. 1415 cm-1) to 2nd peak (ca. 1374 cm-1) height ratio, CHO 1st peak (ca. 1149 cm-1) to 3rd peak (ca. 1032 cm-1) height ratio, CELC to total CHO area ratio and STCHO to CELC area ratio, indicating that carinata meal may not in full accord with canola meal in carbohydrate utilization and availability in ruminants. Carbohydrate conformation and spectral features were changed by significant interaction of meal type and incubation time and almost all the spectral parameters were significantly decreased (P

  9. FT-Raman and FT-Infrared investigations of archaeological artefacts from Foeni Neolithic site (Banat, Romania)

    OpenAIRE

    Simona Cîntă Pînzaru; Dana Pop; Loredana Nemeth

    2008-01-01

    An impressive collection of chert artefacts from the Foeni Neolithic archaeological site (Timiş County, Banat region, Romania) is hosted by the Banat Museum in Timişoara. A representative set of seven specimens was non-destructively investigated using FT-Raman and ATR-FT-IR spectroscopy. The research was carried out for checking if these readily-available, non-destructive, fast, and cheap methods, which do not require preliminary sample preparation could provide significant information for ch...

  10. Green synthesis of silver nanoparticles using a Melissa officinalis leaf extract with antibacterial properties

    Directory of Open Access Journals (Sweden)

    Álvaro de Jesús Ruíz-Baltazar

    Full Text Available The exceptional properties of the silver nanoparticles offer several applications in the biomedicine field. The development of antibiotics which are clinically useful against bacteria and drug resistant microorganisms, it is one of the main approaches of silver nanoparticles. However, it is necessary to develop environmentally friendly methods for their synthesis. In this sense, the main objective of this work is focused on to propose a simplified and efficient green synthesis of silver nanoparticles with proven antibacterial properties. The green synthesis route is based on the use of the Melissa officinalis as reducing agent of the silver ions in aqueous solution at room temperature. Complementary, the antibacterial activity of the silver nanoparticles against Staphylococcus aureus and Escherichia coli was confirmed. The silver nanoparticles obtained were characterized by transmission electron microscopy, X-ray diffraction, UV–vis, Raman and FT-IR spectroscopy. The observed results suggested that using Melissa officinalis, it is possible to performed silver nanoparticles with controlled characteristics and with significant inhibitory activity against the Staphylococcus aureus and Escherichia coli. Keywords: Green synthesis, Nanoparticles, Antibacterial effect

  11. Attenuated Total Reflection Fourier Transform Infrared (ATR FT-IR) Spectroscopy as a Forensic Method to Determine the Composition of Inks Used to Print the United States One-cent Blue Benjamin Franklin Postage Stamps of the 19th Century.

    Science.gov (United States)

    Brittain, Harry G

    2016-01-01

    Through the combined use of infrared (IR) absorption spectroscopy and attenuated total reflectance (ATR) sampling, the composition of inks used to print the many different types of one-cent Benjamin Franklin stamps of the 19th century has been established. This information permits a historical evaluation of the formulations used at various times, and also facilitates the differentiation of the various stamps from each other. In two instances, the ink composition permits the unambiguous identification of stamps whose appearance is identical, and which (until now) have only been differentiated through estimates of the degree of hardness or softness of the stamp paper, or through the presence or absence of a watermark in the paper. In these instances, the use of ATR Fourier transform infrared spectroscopy (FT-IR) spectroscopy effectively renders irrelevant two 100-year-old practices of stamp identification. Furthermore, since the use of ATR sampling makes it possible to obtain the spectrum of a stamp still attached to its cover, it is no longer necessary to identify these blue Franklin stamps using their cancellation dates. © The Author(s) 2015.

  12. Copper(II) complex with 6-methylpyridine-2-carboxyclic acid: Experimental and computational study on the XRD, FT-IR and UV-Vis spectra, refractive index, band gap and NLO parameters.

    Science.gov (United States)

    Altürk, Sümeyye; Avcı, Davut; Başoğlu, Adil; Tamer, Ömer; Atalay, Yusuf; Dege, Necmi

    2018-02-05

    Crystal structure of the synthesized copper(II) complex with 6-methylpyridine-2-carboxylic acid, [Cu(6-Mepic) 2 ·H 2 O]·H 2 O, was determined by XRD, FT-IR and UV-Vis spectroscopic techniques. Furthermore, the geometry optimization, harmonic vibration frequencies for the Cu(II) complex were carried out by using Density Functional Theory calculations with HSEh1PBE/6-311G(d,p)/LanL2DZ level. Electronic absorption wavelengths were obtained by using TD-DFT/HSEh1PBE/6-311G(d,p)/LanL2DZ level with CPCM model and major contributions were determined via Swizard/Chemissian program. Additionally, the refractive index, linear optical (LO) and non-nonlinear optical (NLO) parameters of the Cu(II) complex were calculated at HSEh1PBE/6-311G(d,p) level. The experimental and computed small energy gap shows the charge transfer in the Cu(II) complex. Finally, the hyperconjugative interactions and intramolecular charge transfer (ICT) were studied by performing of natural bond orbital (NBO) analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Isolation and structural characterization of a novel sibutramine analogue, chlorosipentramine, in a slimming dietary supplement, by using HPLC-PDA, LC-Q-TOF/MS, FT-IR, and NMR.

    Science.gov (United States)

    Yun, Jisuk; Shin, Kye Jung; Choi, Jangduck; Jo, Cheon-Ho

    2018-05-01

    A novel sibutramine analogue was detected in a slimming formula by high performance liquid chromatography with a photo diode detector array (HPLC-PDA). The unknown compound exhibited an ultraviolet (UV) spectrum that was similar to that of chlorosibutramine, despite having a different HPLC retention time. Further analysis of the slimming formula by LC-quadrupole time-of-flight mass spectrometry (LC-Q-TOF/MS) showed that the unknown compound had the formula C 18 H 27 Cl 2 N. To elucidate the structure of this new sibutramine analogue, the target compound in the slimming formula was isolated on a preparative-LC system equipped with a PDA. After analysis by fourier transform infrared (FT-IR) and nuclear magnetic resonance (NMR) spectroscopy, the unknown compound was identified as a sibutramine analogue in which the iso-butyl group on the side chain is replaced with an iso-pentyl group. This new sibutramine analogue was identified to be 1-(1-(3,4-dichlorophenyl)cyclobutyl)-N,N,4-trimethylpentan-1-amine and has been named as chlorosipentramine. Copyright © 2018 Elsevier B.V. All rights reserved.

  14. Spectroscopic (FT-IR, FT-Raman and UV-Visible) investigations, NMR chemical shielding anisotropy (CSA) parameters of 2,6-Diamino-4-chloropyrimidine for dye sensitized solar cells using density functional theory.

    Science.gov (United States)

    Gladis Anitha, E; Joseph Vedhagiri, S; Parimala, K

    2015-02-05

    The molecular structure, geometry optimization, vibrational frequencies of organic dye sensitizer 2,6-Diamino-4-chloropyrimidine (DACP) were studied based on Hartree-Fock (HF) and density functional theory (DFT) using B3LYP methods with 6-311++G(d,p) basis set. Ultraviolet-Visible (UV-Vis) spectrum was investigated by time dependent DFT (TD-DFT). Features of the electronic absorption spectrum in the UV-Visible regions were assigned based on TD-DFT calculation. The absorption bands are assigned to transitions. The interfacial electron transfer between semiconductor TiO2 electrode and dye sensitizer DACP is due to an electron injection process from excited dye to the semiconductor's conduction band. The observed and the calculated frequencies are found to be in good agreement. The energies of the frontier molecular orbitals (FMOS) have also been determined. The chemical shielding anisotropic (CSA) parameters are calculated from the NMR analysis, Stability of the molecule arising from hyperconjugative interactions and charge delocalization has been analyzed using natural bond orbital (NBO) analysis. Copyright © 2014 Elsevier B.V. All rights reserved.

  15. Experimental (FT-IR and FT-Raman) and theoretical (HF and DFT) investigation, NMR, NBO, electronic properties and frequency estimation analyses on 2,4,5-trichlorobenzene sulfonyl chloride

    Science.gov (United States)

    Gayathri, R.; Arivazhagan, M.

    2012-11-01

    The present work deals with the structural, electronic, and vibrational analyses of the biomolecule 2,4,5-trichlorobenzene sulfonyl chloride (TCBSC). TCBSC is a novel pharmaceutical compound used in dyes, pesticides, pigments, fluorescence brighteners and intermediate for agricultural chemicals in the manufacture of insecticides. Quantum chemical calculation of geometrical structure and energies of TCBSC was carried out by density functional theory (B3LYP) and ab initio (HF) methods at 6-311+G(d,p) and 6-311++G(d,p) standard basis set. The stability of the molecule arising from hyperconjugative interaction and charge delocalization has been analyzed using natural bond orbital (NBO) analysis. NMR analysis shows that the isotropic chemical shifts of carbon and hydrogen atom of TCBSC are giving the reasonable shielding to the molecule. Another interesting property shows nonlinear optical (NLO) behavior. Moreover, we have not only simulated highest occupied molecular orbital (HOMO) and lowest unoccupied molecular orbital (LUMO) but also determined the transition state and energy band gap.

  16. Synthesis and Characterization of Highly Intercalated Graphite Bisulfate

    Science.gov (United States)

    Salvatore, Marcella; Carotenuto, Gianfranco; De Nicola, Sergio; Camerlingo, Carlo; Ambrogi, Veronica; Carfagna, Cosimo

    2017-03-01

    Different chemical formulations for the synthesis of highly intercalated graphite bisulfate have been tested. In particular, nitric acid, potassium nitrate, potassium dichromate, potassium permanganate, sodium periodate, sodium chlorate, and hydrogen peroxide have been used in this synthesis scheme as the auxiliary reagent (oxidizing agent). In order to evaluate the presence of delamination, and pre-expansion phenomena, and the achieved intercalation degree in the prepared samples, the obtained graphite intercalation compounds have been characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray powder diffraction (XRD), infrared spectroscopy (FT-IR), micro-Raman spectroscopy ( μ-RS), and thermal analysis (TGA). Delamination and pre-expansion phenomena were observed only for nitric acid, sodium chlorate, and hydrogen peroxide, while the presence of strong oxidizers (KMnO4, K2Cr2O7) led to stable graphite intercalation compounds. The largest content of intercalated bisulfate is achieved in the intercalated compounds obtained from NaIO4 and NaClO3.

  17. Microscale Solubility Measurements of Matrix-Assisted Laser Desorption-Ionization (MALDI) Matrices Using Attenuated Total Reflection (ATR) Fourier Transform Infrared Spectroscopy (FT-IR) Coupled with Partial Least Squares (PLS) Analysis.

    Science.gov (United States)

    Gorre, Elsa; Owens, Kevin G

    2016-11-01

    In this work an attenuated total reflection Fourier transform infrared (FT-IR) absorption based method is used to measure the solubility of two matrix-assisted laser desorption-ionization (MALDI) matrices in a few pure solvents and mixtures of acetonitrile and water using low microliter amounts of solution. Results from a method that averages the values obtained from multiple calibration curves created by manual peak picking are compared to those predicted using a partial least squares (PLS) chemometrics approach. The PLS method provided solubility values that were in good agreement with the manual method with significantly greater ease of analysis. As a test, the solubility of adipic acid in acetone was measured using the two methods of analysis, and the values are in good agreement with solubility values reported in literature. The solubilities of the MALDI matrices α-cyano-4-hydroxy cinnamic acid (CHCA) and sinapinic acid (SA) were measured in a series of mixtures made from acetonitrile (ACN) and water; surprisingly, the results show a highly nonlinear trend. While both CHCA and SA show solubility values of less than 10 mg/mL in the pure solvents, the solubility value for SA increases to 56.3 mg/mL in a 75:25 v/v ACN:water mixture. This can have a significant effect on the matrix-to-analyte ratios in the MALDI experiment when sample protocols call for preparation of a saturated solution of the matrix in the chosen solvent system. © The Author(s) 2016.

  18. Synthesis of 3-Methyl-1-morpholin-4-ylmethyl-2,6-diphenylpiperidin-4-one

    Directory of Open Access Journals (Sweden)

    Bathey R. Venkatraman

    2009-09-01

    Full Text Available This paper describes the synthesis of 3-methyl-1-morpholin-4-ylmethyl-2,6-diphenylpiperidin-4-one from 3-methyl-2,6-diphenylpiperidin-4-one. The synthesized compound was characterized by FT-IR, 1H NMR, EI-MS and elemental analysis.

  19. Synthesis of Au Nanostars and Their Application as Surface Enhanced Raman Scattering-Activity Tags Inside Living Cells.

    Science.gov (United States)

    Cao, Xiaowei; Shi, Chaowen; Lu, Wenbo; Zhao, Hang; Wang, Man; Tong, Wei; Dong, Jian; Han, Xiaodong; Qian, Weiping

    2015-07-01

    This work presents the synthesis and characterization of Au nanostars (AuNSs) and demonstrates their application as surface enhanced Raman scattering (SERS)-activity tags for cellular imaging and sensing. Nile blue A (NBA) and bovine serum albumin (BSA) were used as Raman reporter molecules and capping materials, respectively. The SERS-activity tags were tested on human lung adenocarcinoma cell (A549) and alveolar type II cell (AT II) and found to present a low level of cytotoxicity and high chemical stability. These SERS-activity tags not only can be applied in multiplexed cellular imaging, including dark field imaging, transmission electron microscopy (TEM) and SERS imaging, but also can be used for cellular sensing. The SERS spectra clearly identified cellular important components such as proteins, nucleic acids, lipids, and carbohydrates. This study also shows that endocytosis is the main channel of tags internalized in cells. The AuNSs exhibiting strong surface enhanced Raman effects are utilized in the design of an efficient, stable SERS-activity tag for intracellular applications.

  20. Efficient synthesis of highly fluorescent nitrogen-doped carbon dots for cell imaging using unripe fruit extract of Prunus mume

    International Nuclear Information System (INIS)

    Atchudan, Raji; Edison, Thomas Nesakumar Jebakumar Immanuel; Sethuraman, Mathur Gopalakrishnan; Lee, Yong Rok

    2016-01-01

    Graphical abstract: The green synthesis of highly fluorescent N-CDs was achieved using the extract of unripe P. mume fruit as a carbon precursor by a one-pot simple hydrothermal-carbonization method. The resulting N-CDs were used as a staining agent for the fluorescence imaging of MDA-MB-231 cells. Display Omitted - Highlights: • The green synthesis of highly fluorescent N-CDs using the extract of unripe P. mume. • The N-CDs were synthesized by one-pot hydrothermal-carbonization method. • This method of synthesis is a simple, cost effective and eco-friendly route. • N-CDs will be a good alternative for fluorescent dyes and SQDs for bio-applications. - Abstract: Highly fluorescent nitrogen-doped carbon dots (N-CDs) were synthesized using the extract of unripe Prunus mume (P. mume) fruit by a simple one step hydrothermal-carbonization method. The N-CDs were synthesized at different pH ranges, 2.3, 5, 7, and 9. The pH of the P. mume extract was adjusted using an aqueous ammonia solution (25%). The optical properties of N-CDs were examined by UV–vis and fluorescence spectroscopy. The N-CDs synthesized at pH 9 emitted high fluorescence intensity compared to other obtained N-CDs. The N-CDs synthesized at pH 9 was further characterized by high resolution transmission electron microscopy (HR-TEM), X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and Fourier transform-infra red (FT-IR) spectroscopy. HR-TEM showed that the average size of the synthesized N-CDs was approximately 9 nm and the interlayer distance was 0.21 nm, which was validated by XRD. The graphitic nature of the synthesized N-CDs were confirmed by Raman spectroscopy. XPS and FT-IR spectroscopy confirmed the doping of the nitrogen moiety over the synthesized CDs. The synthesized nitrogen doped CDs (N-CDs) were low toxicity and were used as a staining probe for fluorescence cell imaging.

  1. Efficient synthesis of highly fluorescent nitrogen-doped carbon dots for cell imaging using unripe fruit extract of Prunus mume

    Energy Technology Data Exchange (ETDEWEB)

    Atchudan, Raji; Edison, Thomas Nesakumar Jebakumar Immanuel [School of Chemical Engineering, Yeungnam University, Gyeongsan 38541 (Korea, Republic of); Sethuraman, Mathur Gopalakrishnan, E-mail: mgsethu@gmail.com [Department of Chemistry, Gandhigram Rural Institute-Deemed University, Gandhigram 624 302, Tamilnadu (India); Lee, Yong Rok, E-mail: yrlee@yu.ac.kr [School of Chemical Engineering, Yeungnam University, Gyeongsan 38541 (Korea, Republic of)

    2016-10-30

    Graphical abstract: The green synthesis of highly fluorescent N-CDs was achieved using the extract of unripe P. mume fruit as a carbon precursor by a one-pot simple hydrothermal-carbonization method. The resulting N-CDs were used as a staining agent for the fluorescence imaging of MDA-MB-231 cells. Display Omitted - Highlights: • The green synthesis of highly fluorescent N-CDs using the extract of unripe P. mume. • The N-CDs were synthesized by one-pot hydrothermal-carbonization method. • This method of synthesis is a simple, cost effective and eco-friendly route. • N-CDs will be a good alternative for fluorescent dyes and SQDs for bio-applications. - Abstract: Highly fluorescent nitrogen-doped carbon dots (N-CDs) were synthesized using the extract of unripe Prunus mume (P. mume) fruit by a simple one step hydrothermal-carbonization method. The N-CDs were synthesized at different pH ranges, 2.3, 5, 7, and 9. The pH of the P. mume extract was adjusted using an aqueous ammonia solution (25%). The optical properties of N-CDs were examined by UV–vis and fluorescence spectroscopy. The N-CDs synthesized at pH 9 emitted high fluorescence intensity compared to other obtained N-CDs. The N-CDs synthesized at pH 9 was further characterized by high resolution transmission electron microscopy (HR-TEM), X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and Fourier transform-infra red (FT-IR) spectroscopy. HR-TEM showed that the average size of the synthesized N-CDs was approximately 9 nm and the interlayer distance was 0.21 nm, which was validated by XRD. The graphitic nature of the synthesized N-CDs were confirmed by Raman spectroscopy. XPS and FT-IR spectroscopy confirmed the doping of the nitrogen moiety over the synthesized CDs. The synthesized nitrogen doped CDs (N-CDs) were low toxicity and were used as a staining probe for fluorescence cell imaging.

  2. Synthesis, spectroscopic, thermal and structural properties of [M(3-aminopyridine)2Ni(μ-CN)2(CN)2]n (M(II) = Co and Cu) heteropolynuclear cyano-bridged complexes

    Science.gov (United States)

    Kartal, Zeki

    2016-01-01

    Two novel cyano-bridged heteropolynuclear complexes, [Co(3-aminopyridine)2Ni(μ-CN)2(CN)2]n and [Cu(3-aminopyridine)2Ni(μ-CN)2(CN)2]n have been synthesized and characterized by elemental, thermal, FT-IR and FT-Raman spectroscopies. The structures of complexes have been determined by X-ray powder diffraction. The FT-IR and FT-Raman spectra of complexes have been recorded in the region of 3500-400 cm-1 and 3500-100 cm-1, respectively. General information was acquired about structural properties of these complexes from FT-IR and FT-Raman spectra by considering changes at characteristic peaks of the cyano group and 3AP. The splitting of the ν(Ctbnd N) stretching bands in the FT-IR spectra for complexes indicates the presence of terminal and bridging cyanides. The thermal behaviors of these complexes have been also investigated in the range of 25-950 °C using TG and DTG methods. Magnetic susceptibility measurements were made at room temperature using Gouy-balance.

  3. Mg-doped hydroxyapatite nanoplates for biomedical applications: A surfactant assisted microwave synthesis and spectroscopic investigations

    International Nuclear Information System (INIS)

    Mishra, Vijay Kumar; Bhattacharjee, Birendra Nath; Parkash, Om; Kumar, Devendra; Rai, Shyam Bahadur

    2014-01-01

    Highlights: • Microwave irradiation technique: employed for the synthesis of Mg-HAp nanoplates. • Surfactant (EDTA) assisted synthesis of Mg-HAp. • FT-IR and Raman analysis of functional groups of Mg-HAp. - Abstract: Nanoplates of Mg doped hydroxyapatite (Mg-HAp) were derived successfully and rapidly via microwave irradiation technique. Hydroxyapatite (HAp) is the hard tissues and main inorganic component in mammals. Different nanostructures of HAp exist in different parts of human bone but nanorods are very common due to its intrinsic nature to grow in rode-like structure under physiological as well as under applied ambient conditions in laboratory. On the addition of Mg at very low level (0.06 mol%) in pure HAp results the formation of 2-D plate-like nanostructures rather than rod-like which is the matter of interest. In this attempt our efforts have been focused on the study of effect of Mg incorporation on structural and spectroscopic properties of HAp prepared via microwave irradiation technique. This technique is preferred due to several advantages viz. very fast as well as homogeneous heating, time/energy saving and eco-friendliness. The calcium nitrate tetrahydrate (Ca(NO 3 ) 2 ⋅4H 2 O)) as a source of calcium, magnesium nitrate hexahydrate (Mg(NO 3 ) 2 ⋅6H 2 O) as a source of magnesium, disodium hydrogen phosphate dihydrate (NaH 2 PO 4 ⋅2H 2 O) as a source of phosphorous and sodium ethylene diamine tetra acetate (NaEDTA) as a surfactant were used as starting reagents. Sodium hydroxide (NaOH) pellets were employed to adjust the pH value of final solution. The solution of fixed pH value was kept into the microwave oven generating waves of frequency 2.45 GHz (water absorption frequency) and power 750 W for 8 min. The precipitate thus obtained was washed, centrifuged and then dried at 100 °C for 2 h. Dried powder was then calcined at 700 °C for 2 h. The bright white powder thus obtained was characterized structurally using X-ray diffraction and

  4. Mg-doped hydroxyapatite nanoplates for biomedical applications: A surfactant assisted microwave synthesis and spectroscopic investigations

    Energy Technology Data Exchange (ETDEWEB)

    Mishra, Vijay Kumar [Department of Physics, Faculty of Science, Banaras Hindu University, Varanasi 221005 (India); Bhattacharjee, Birendra Nath; Parkash, Om [Department of Ceramic Engineering, Indian Institute of Technology, Banaras Hindu University, Varanasi 221005 (India); Kumar, Devendra, E-mail: devendra.cer@iitbhu.ac.in [Department of Ceramic Engineering, Indian Institute of Technology, Banaras Hindu University, Varanasi 221005 (India); Rai, Shyam Bahadur, E-mail: sbrai49@yahoo.co.in [Department of Physics, Faculty of Science, Banaras Hindu University, Varanasi 221005 (India)

    2014-11-25

    Highlights: • Microwave irradiation technique: employed for the synthesis of Mg-HAp nanoplates. • Surfactant (EDTA) assisted synthesis of Mg-HAp. • FT-IR and Raman analysis of functional groups of Mg-HAp. - Abstract: Nanoplates of Mg doped hydroxyapatite (Mg-HAp) were derived successfully and rapidly via microwave irradiation technique. Hydroxyapatite (HAp) is the hard tissues and main inorganic component in mammals. Different nanostructures of HAp exist in different parts of human bone but nanorods are very common due to its intrinsic nature to grow in rode-like structure under physiological as well as under applied ambient conditions in laboratory. On the addition of Mg at very low level (0.06 mol%) in pure HAp results the formation of 2-D plate-like nanostructures rather than rod-like which is the matter of interest. In this attempt our efforts have been focused on the study of effect of Mg incorporation on structural and spectroscopic properties of HAp prepared via microwave irradiation technique. This technique is preferred due to several advantages viz. very fast as well as homogeneous heating, time/energy saving and eco-friendliness. The calcium nitrate tetrahydrate (Ca(NO{sub 3}){sub 2}⋅4H{sub 2}O)) as a source of calcium, magnesium nitrate hexahydrate (Mg(NO{sub 3}){sub 2}⋅6H{sub 2}O) as a source of magnesium, disodium hydrogen phosphate dihydrate (NaH{sub 2}PO{sub 4}⋅2H{sub 2}O) as a source of phosphorous and sodium ethylene diamine tetra acetate (NaEDTA) as a surfactant were used as starting reagents. Sodium hydroxide (NaOH) pellets were employed to adjust the pH value of final solution. The solution of fixed pH value was kept into the microwave oven generating waves of frequency 2.45 GHz (water absorption frequency) and power 750 W for 8 min. The precipitate thus obtained was washed, centrifuged and then dried at 100 °C for 2 h. Dried powder was then calcined at 700 °C for 2 h. The bright white powder thus obtained was characterized

  5. Reversible dimer formation and stability of the anti-tumour single-chain Fv antibody MFE-23 by neutron scattering, analytical ultracentrifugation, and NMR and FT-IR spectroscopy.

    Science.gov (United States)

    Lee, Yie Chia; Boehm, Mark K; Chester, Kerry A; Begent, Richard H J; Perkins, Stephen J

    2002-06-28

    MFE-23 is a single chain Fv (scFv) antibody molecule used to target colorectal cancer through its high affinity for the tumour marker carcinoembryonic antigen (CEA). ScFv molecules are formed from peptide-linked antibody V(H) and V(L) domains, and many of these form dimers. Our recent crystal structure for MFE-23 showed that this formed an unusual symmetric back-to-back association of two monomers that is consistent with a domain-swapped diabody structure. Neutron scattering and modelling fits showed that MFE-23 existed as compact V(H)-V(L)-linked monomers at therapeutically relevant concentrations below 1 mg/ml. Size-exclusion gel chromatography showed that the monomeric and dimeric forms of MFE-23 could be separated, and that the proportions of these two forms depended on the starting MFE-23 concentration. Sedimentation equilibrium experiments by analytical ultracentrifugation at nine concentrations of MFE-23 indicated a reversible monomer-dimer self-association equilibrium with an association constant of 1.9x10(3)-2.2x10(3) M(-1). Sedimentation velocity experiments using the time derivative g(s(*)) method showed that MFE-23-His has a concentration-dependent weight average sedimentation coefficient that increased from 1.8 S for the monomer to about 3-6 S for the dimer. Both values agreed with those calculated from the MFE-23 crystal structure. In relation to the thermal stability of MFE-23, denaturation experiments by (1)H NMR and FT-IR spectroscopy showed that the molecule is stable up to 47 degrees C, after which denaturation was irreversible. MFE-23 dimerisation is discussed in terms of a new model for diabody structures, in which the V(H) and V(L) domains in the monomer are able to dissociate and reassociate to form a dimer, or diabody, but in which symmetric back-to-back contacts between the two monomers are formed. This dimerisation in solution is attributed to the complementary nature of the C-terminal surface of the MFE-23 monomer. Crystal structures for

  6. Synthesis and high (pressure, temperature) stability of ZnTiO3 polymorphs studied by Raman spectroscopy

    Science.gov (United States)

    Bernert, T.; Ruiz-Fuertes, J.; Bayarjargal, L.; Winkler, B.

    2015-05-01

    The phase-purity of ilmenite-type ZnTiO3 prepared by the ceramic method was investigated in dependence of the conditions during ball milling. The previously proposed addition of 2 ml ethanol to the starting materials led to a significant contamination of the product phase after a subsequent sintering process at 1073 K. However, by omitting ethanol this synthesis route led to a phase-pure sample of ZnTiO3 as confirmed by X-ray powder diffraction and Raman spectroscopy. High-temperature high-pressure experiments gave an ilmenite-type to perovskite-type phase boundary with a slope of dT/dP∼-135 K GPa-1 crossing ambient temperature conditions at ∼ 24 GPa in good agreement with previous calculations. Room-temperature high-pressure Raman spectroscopy experiments have shown the stability of the ilmenite-type phase up to a pressure of at least 38.5 GPa, the highest pressure applied in this study, indicating the presence of a kinetic barrier in this phase transition. The synthesis of ferroelectric LiNbO3-type ZnTiO3 was confirmed by second harmonic generation.

  7. Synthesis and Mechanism of Tetracalcium Phosphate from Nanocrystalline Precursor

    Directory of Open Access Journals (Sweden)

    Jianguo Liao

    2014-01-01

    Full Text Available Tetracalcium phosphate (TTCP, Ca4(PO42O was prepared by the calcination of coprecipitated mixture of nanoscale hydroxyapatite (HA, Ca10(PO46(OH2 and calcium carbonate crystal (CaCO3, followed by cooling in the air or furnace. The effect of calcination temperature on crystal structure and phase composition of the coprecipitation mixture was characterized by transmission electron microscope (TEM, thermal analysis-thermogravimetry (DTA-TG, X-ray diffraction (XRD, Fourier transform-infrared spectroscopy (FT-IR, and Raman spectroscopy (RS. The obtained results indicated that the synthesized mixture consisted of nanoscale HA and CaCO3 with uniform distribution throughout the composite. TTCP was observed in the air quenching samples when the calcination temperature was above 1185°C. With the increase of the calcination temperature, the amount of the intermediate products in the air quenching samples decreased and cannot be detected when calcination temperature reached 1450°C. Unexpectedly, the mixture of HA and calcium oxide was observed in the furnace cooling samples. Clearly, the calcination temperature and cooling methods are critical for the synthesis of high-purity TTCP. The results indicate that the nanosize of precursors can decrease the calcination temperature, and TTCP can be calcinated by low temperature.

  8. Low Temperature Solid-State Synthesis and Characterization of LaBO3

    Directory of Open Access Journals (Sweden)

    Azmi Seyhun KIPÇAK

    2016-11-01

    Full Text Available Rare earth (lanthanide series borates, possess high vacuum ultraviolet (VUV transparency, large electronic band gaps, chemical and environmental stability and exceptionally large optical damage thresholds and used in the development of plasma display panels (PDPs. In this study the synthesis of lanthanum borates via solid-state method is studied. For this purpose, lanthanum oxide (La2O3 and boric acid (H3BO3 are used for as lanthanum and boron sources, respectively. Different elemental molar ratios of La to B (between 3:1 to 1:6 as La2O3:H3BO3 were reacted by solid-state method at the reaction temperatures between 500°C - 700°C with the constant reaction time of 4 h. Following the synthesis, characterizations of the synthesized products are conducted by X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FT-IR, Raman spectroscopy and scanning electron microscope (SEM. From the results of the experiments, three types of lanthanum borates of; La3BO6, LaBO3 and La(BO23 were observed at different reaction parameters. Among these three types of lanthanum borates LaBO3 phase were obtained as a major phase.

  9. Sulfonic acid functionalized boron nitride nanomaterials as a microwave-assisted efficient and highly biologically active one-pot synthesis of piperazinyl-quinolinyl fused Benzo[c]acridine derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Murugesan, Arul; Gengan, R.M., E-mail: genganrm@dut.ac.za; Krishnan, Anand

    2017-02-15

    Boron nitride nano material based solid acid catalyst was found to be an efficient and reusable sulfonic acid catalyst for the synthesis of one-pot Knoevenagel and Michael type reactions in 3, 3-dimethyl-9-(2-(4-methylpiperazin-1-yl) quinolin-3-yl)-3, 4, 9, 10-tetrahydroacridin-1(2H)-one derivatives under microwave irradiation conditions. The catalyst was prepared by mixing boron nitrile and (3-mercaptopropyl) trimethoxysilane. This is simple and safe method for the preparation of solid acid catalysts. The morphological properties of catalyst determined by using FT-IR, XRD, TEM, SEM and Raman spectroscopy. The synthesised catalyst was employed in Knoevenagel and Michael type reactions to synthesise novel piperazinyl-quinolinyl based acridine derivatives. Furthermore the newly-synthesised compounds have been used for molecular docking in DNA binding studies. The method developed in this study has the advantages of good yield, simplicity coupled with safety and short reaction time. Most importantly it was found that the solid acid catalyst can be recycled with only 5% loss of activity. - Highlights: • One-pot Synthesis of Knoevenagel and Michel type reactions. • Synthesis of Sulfonic acid Functionalized Boron nitride nano materials. • Synthesis of piperazinyl-quinolinyl fused Benzo[c]acridine derivatives under Microwave irradiation. • Molecular docking studies were performed on piperazinyl-quinolinyl acridine derivatives using DNA.

  10. Synthesis and Characterizations of Poly(3-hexylthiophene and Modified Carbon Nanotube Composites

    Directory of Open Access Journals (Sweden)

    Mohammad Rezaul Karim

    2012-01-01

    Full Text Available Poly(3-hexylthiophene and modified (functionalized and silanized multiwall carbon nanotube (MWNT nanocomposites have been prepared through in situ polymerization process in chloroform medium with FeCl3 oxidant at room temperature. The composites are characterized through Fourier transfer infrared spectroscopy (FT-IR, Raman, and X-ray diffraction (XRD measurements to probe the nature of interaction between the moieties. Optical properties of the composites are measured from ultraviolet-visible (UV-Vis and photoluminescence (PL spectroscopy. Conductivity of the composites is followed by four probe techniques to understand the conduction mechanism. The change (if any in C=C symmetric and antisymmetric stretching frequencies in FT-IR, the shift in G band frequencies in Raman, any alterations in λmax of UV-Vis, and PL spectroscopic measurements are monitored with modified MWNT loading in the polymer matrix.

  11. Iodide-conducting polymer electrolytes based on poly-ethylene glycol and MgI2: Synthesis and structural characterization

    International Nuclear Information System (INIS)

    Vittadello, Michele; Waxman, David I.; Sideris, Paul J.; Gan Zhehong; Vezzù, Keti; Negro, Enrico; Safari, Ahmad; Greenbaum, Steve G.; Di Noto, Vito

    2011-01-01

    A major obstacle for a viable technological development of dye sensitized solar cells (DSSCs) is still the synthesis of a high performance iodide-conducting polymer electrolyte. Here we present a series of eight electrolytic complexes with formula PEG1000/(MgI 2 ) x (I 2 ) y (0.0038 ≤ x ≤ 0.5801, 0 ≤ y ≤ 0.0636). The synthesis involves the preparation of a disordered form of MgI 2 by a metallorganic route, which enables us to dissolve high amounts of salt in the chosen polymer host. The thermal analysis of the resulting polymer electrolytes was performed using modulated differential scanning calorimetry measurements. Vibrational studies were carried out using medium FT-IR, far FT-IR and FT-Raman. The variation of the CO and OH stretching modes in the medium infrared, as a function of the mole-to-mole ratio n Mg /n O , was investigated by Gaussian decomposition to provide insight into the polymer–polymer and salt–polymer interactions in these materials. The FT-Raman spectra confirmed and complemented the vibrational assignment. The conductivity study of these systems was performed by electrical spectroscopy in the frequency interval 10 mHz–10 MHz. The direct current conductivity (σ DC ) profiles versus the reciprocal temperature exhibited a Vögel-Tamman-Fülcher (VTF) behavior. The best σ DC at 50 °C was 5 × 10 −5 S cm −1 . The overall results indicate the presence of bivalent, monovalent and neutral species, Mg 2+ , [MgI] + and MgI 2 , respectively, which participate in the conduction process. These results are consistent with what was previously observed in PEG400-based systems doped with δ-MgCl 2 . The presence of at least one Mg site containing a distribution in parameters was observed using 25 Mg solid state magic angle spinning nuclear magnetic resonance (MAS NMR) spectroscopy. The site has been assigned to a Mg complex involving the coordination by oxygen atoms of the polymer backbone.

  12. A combined in situ XAS-XRPD-Raman study of Fischer-Tropsch synthesis over a carbon supported Co catalyst

    DEFF Research Database (Denmark)

    Tsakoumis, Nikolaos E.; Dehghan, Roya; Johnsen, Rune

    2013-01-01

    A cobalt based Fischer-Tropsch synthesis (FTS) catalyst, supported on a carbon nanofibers/carbon felt composite (Co/CNF/CF) was studied in situ at realistic conditions. The catalyst was monitored by Xray absorption spectroscopy (XAS), high-resolution X-ray powder diffraction (HR-XRPD) and Raman...... spectroscopy, while changes in the gas phase were observed by mass spectrometry (MS). Transmission electron microscopy (TEM) was also applied to characterise the catalyst. The catalyst has a bimodal particle size distribution and exhibits a high deactivation rate. During the in situ study the catalyst appears...... to reduce further at the induction period of FTS, while crystallite growth is been detected in the same period. At steady state FTS the amount of metallic Co is constant. A change in the volumetric flow towards higher conversions did not affect the degree of reduction or the crystallite size of the catalyst...

  13. Mesoporous CdS via Network of Self-Assembled Nanocrystals: Synthesis, Characterization and Enhanced Photoconducting Property.

    Science.gov (United States)

    Patra, Astam K; Banerjee, Biplab; Bhaumik, Asim

    2018-01-01

    Semiconduction nanoparticles are intensively studied due to their huge potential in optoelctronic applications. Here we report an efficient chemical route for hydrothermal synthesis of aggregated mesoporous cadmium sulfide (CdS) nanoparticles using supramolecular-assembly of ionic and water soluble sodium salicylate as the capping agent. The nanostructure, mesophase, optical property and photoconductivity of these mesoporous CdS materials have been characterized by using small and wide angle powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), N2-sorption, Raman analysis, Fourier transformed infrared (FT-IR), UV-Visible DSR spectroscopy, and photoconductivity measurement. Wide angle XRD pattern and high resolution TEM image analysis suggested that the particle size of the materials is within 10 nm and the nanoparticles are in well-crystallized cubic phase. Mesoporous CdS nanoparticles showed drastically enhanced photoelectrochemical response under visible light irradiation on entrapping a photosensitizer (dye) molecule in the interparticle spaces. Efficient synthesis strategy and the enhanced photo response in the mesoporous CdS material could facilitate the designing of other porous semiconductor oxide/sulfide and their applications in photon-to-electron conversion processes.

  14. Synthesis and Raman analysis of SnS nanoparticles synthesized by PVP assisted polyol method

    Energy Technology Data Exchange (ETDEWEB)

    Baby, Benjamin Hudson; Mohan, D. Bharathi, E-mail: d.bharathimohan@gmail.com [Department of Physics, School of Physical, Chemical and Applied Sciences, Pondicherry University, R.V. Nagar, Kalapet, Puducherry-605014 (India)

    2015-06-24

    SnS film was prepared by a simple drop casting method after synthesizing SnS nanoparticles by using PVP assisted polyol method. Confocal Raman study was carried out for the as deposited and annealed (150, 300 and 400 °C) films at two different excitation wavelengths 514 and 785 nm. At the excitation wavelength of 514 nm, the Raman modes showed for a mixed phase of SnS and SnS{sub 2} up to 150 °C and then only a pure SnS phase was observed up to 400 °C due to the dissociation of SnS{sub 2} in to SnS by releasing S. The increase in intensity of Raman (A{sub g} and B{sub 3g}) as well as IR (B{sub 3u}) active modes of SnS are observed with increasing annealing temperature at excitation wavelength 785 nm due to the increased crystallinity and inactiveness of SnS{sub 2} modes. X-ray diffraction confirming the formation of a single phase of SnS while the greater homogeneity in both size and shape of SnS nanoparticles were confirmed through surface morphology from SEM.

  15. Synthesis, FTIR, FT-Raman, UV-visible, ab initio and DFT studies on benzohydrazide.

    Science.gov (United States)

    Arjunan, V; Rani, T; Mythili, C V; Mohan, S

    2011-08-01

    A systematic vibrational spectroscopic assignment and analysis of benzohydrazide (BH) has been carried out by using FTIR and FT-Raman spectral data. The vibrational analysis were aided by electronic structure calculations--ab initio (RHF) and hybrid density functional methods (B3LYP and B3PW91) performed with 6-31G(d,p) and 6-311++G(d,p) basis sets. Molecular equilibrium geometries, electronic energies, IR intensities, harmonic vibrational frequencies, depolarization ratios and Raman activities have been computed. Potential energy distribution (PED) and normal mode analysis have also been performed. The assignments proposed based on the experimental IR and Raman spectra have been reviewed and complete assignment of the observed spectra have been proposed. UV-visible spectrum of the compound was also recorded and the electronic properties, such as HOMO and LUMO energies and λ(max) were determined by time-dependent DFT (TD-DFT) method. The geometrical, thermodynamical parameters and absorption wavelengths were compared with the experimental data. The interactions of carbonyl and hydrazide groups on the benzene ring skeletal modes were investigated. Copyright © 2011 Elsevier B.V. All rights reserved.

  16. Synthesis of gold nanostars with fractal structure: application in surface-enhanced Raman scattering

    Science.gov (United States)

    Zhu, Jian; Liu, Mei-Jin; Li, Jian-Jun; Zhao, Jun-Wu

    2017-11-01

    Multi-branched gold nanostars with fractal feature were synthesized using the Triton X-100 participant seed-growth method. By increasing the amount of ascorbic acid, the branch length of gold nanostars could be greatly increased. It has been interesting to find that the secondary growth of new branches takes place from the elementary structure when the aspect ratio of the branches is greater than 8.0 and the corresponding plasmon absorption wavelength is greater than 900 nm. Raman activity of the gold nanostar films has been investigated by using the 4-mercaptobenzoic acid (4-MBA) as Raman active probe. Experimental results show that the surface-enhanced Raman scattering (SERS) ability of the gold nanostars could be efficiently improved when the fractal structure appears. The physical mechanism has been attributed to the intense increased secondary branch number and the increased "hot spots". These unique multi-branched gold nanostars with fractal feature and great SERS activity should have great potential in sensing applications.

  17. Microwave assisted in situ synthesis of Ag–NaCMC films and their reproducible surface-enhanced Raman scattering signals

    International Nuclear Information System (INIS)

    Jiang, Tao; Li, Junpeng; Zhang, Li; Wang, Binbing; Zhou, Jun

    2014-01-01

    Graphical abstract: Two kinds of Ag–NaCMC films for surface-enhanced Raman scattering (SERS) were prepared by conventional heating and microwave assisted in situ reduction methods without any additional capping or reducing agents. A relatively narrow and symmetric surface plasmon resonance band was observed in the absorption spectra of the films fabricated by the microwave assisted in situ reduction method. More uniform silver nanoparticles (NPs) implied by the symmetric absorption spectrum were further confirmed by the scanning electron microscopy images. After the simulation of the E-field intensity distribution around the silver NPs in NaCMC film, the Raman scattering enhancement factors (EFs) of these films were then investigated with 4-mercaptobenzoic acid molecule as a SERS reporter. Improved reproducibility of SERS signal was obtained in the microwave assisted synthesized Ag–NaCMC film, although it maintained an EF as only 1.11 × 10 8 . The reproducible SERS signal of the Ag–NaCMC film is particularly attractive and this microwave assisted in situ reduction method is suitable for the production of excellent substrate for biosensor application. - Highlights: • The synthesis of Ag–NaCMC films was successfully fulfilled by a low-cost microwave method. • More uniform silver nanoparticles were observed in Ag–NaCMC film synthesized by microwave. • Improved reproducibility of SERS signal was obtained in microwave synthesized Ag–NaCMC film. - Abstract: Two kinds of Ag–NaCMC films for surface-enhanced Raman scattering (SERS) were prepared by conventional heating and microwave assisted in situ reduction methods without any additional capping or reducing agents. A relatively narrow and symmetric surface plasmon resonance band was observed in the absorption spectra of the films fabricated by the microwave assisted in situ reduction method. More uniform silver nanoparticles (NPs) implied by the symmetric absorption spectrum were further confirmed by

  18. Ba3NbAs3O: synthesis, crystal structure, Raman spectroscopy and bonding analysis

    International Nuclear Information System (INIS)

    Monconduit, L.; Tillard, M.; Favier, F.; Belin, C.

    1999-01-01

    The crystal structure of Ba 3 NbAs 3 O has been solved by crystal X-ray analysis (CAD-4 automatic diffractometer, Mo Kα radiation). The compound crystallizes in space group Pnma, a=6.724(2), b=11.100(2), c=13.462(3) A, V=1004.7(4) A 3 , Z=4. The structure has been refined to R1=0.0343 for 964 independent reflections, it can be described as packing of nearly tetrahedral NbAs 3 O 6- anions, their coordination by Ba 2+ cations forming interconnected trigonal prisms. The chemical bonding has been analyzed by MO calculations and Raman spectroscopy. (orig.)

  19. Synthesis and Raman scattering of GaN nanorings, nanoribbons and nanowires

    Energy Technology Data Exchange (ETDEWEB)

    Li, Z.J. [Academia Sinica, Beijing, BJ (China). Inst. of Physics; Northwestern Polytechnical Univ., Xian, SN (China). Dept. of Materials Science and Engineering; Chen, X.L.; Tu, Q.Y.; Yang, Z.; Xu, Y.P.; Hu, B.Q. [Academia Sinica, Beijing, BJ (China). Inst. of Physics; Li, H.J. [Northwestern Polytechnical Univ., Xian, SN (China). Dept. of Materials Science and Engineering

    2001-05-01

    Low-dimensional GaN materials, including nanorings, nanoribbons and smooth nanowires have been synthesized by reacting gallium and ammonia using Ag particles as a catalyst on the substrate of MgO single crystals. They were characterized by field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD). EDX, XRD indicated that the low-dimensional nanomaterials were wurtzite GaN. New features are found in Raman scatterings for these low-dimensional GaN materials, which are different from the previous observations of GaN materials. (orig.)

  20. Boric Acid Catalyzed Convenient Synthesis of Benzimidazoles in Aqueous Media

    OpenAIRE

    Poor Heravi, Mohammad Reza; Ashori, Marjan

    2013-01-01

    Synthesis of benzimidazoles has been developed by the o-phenylenediamine with aldehydes using boric acid an efficient catalyst under mild reaction conditions in aqueous media. The product is applicable to aryl and heteroaryl aldehydes. This reaction led to the formation of benzimidazoles new derivatives in good yields. The FT-IR, 19F-NMR, 1H-NMR, 13C-NMR spectra and elemental analysis confirm the structure of compounds.

  1. Boric Acid Catalyzed Convenient Synthesis of Benzimidazoles in Aqueous Media

    Directory of Open Access Journals (Sweden)

    Mohammad Reza Poor Heravi

    2013-01-01

    Full Text Available Synthesis of benzimidazoles has been developed by the o-phenylenediamine with aldehydes using boric acid an efficient catalyst under mild reaction conditions in aqueous media. The product is applicable to aryl and heteroaryl aldehydes. This reaction led to the formation of benzimidazoles new derivatives in good yields. The FT-IR, 19F-NMR, 1H-NMR, 13C-NMR spectra and elemental analysis confirm the structure of compounds.

  2. Novel method of room temperature ionic liquid assisted Fe3O4 nanocubes and nanoflakes synthesis

    International Nuclear Information System (INIS)

    Ramalakshmi, M.; Shakkthivel, P.; Sundrarajan, M.; Chen, S.M.

    2013-01-01

    Graphical abstract: - Highlights: • First time [Bmim][TfO] IL is used for the Fe 3 O 4 nanoparticle synthesis. • Novel method tunes Fe 3 O 4 nanocubes and nanoflakes forms influenced by the base and IL. • Fe 3 O 4 oxidized topotactically into γ-Fe 2 O 3 nanoparticles by annealing and base. • Uniform morphology with average size of 33 nm negligible superstructure are formed. • Ms values are characterized by thin layer of γ-Fe 2 O 3 on the nanoparticle surface. - Abstract: For the first time, the nanomagnetite superparamagnetic particles are successfully synthesized by precipitation method using 1-n-butyl-3-methylimidazolium trifluoromethane sulfonate [Bmim][TfO] ionic liquid medium/surfactant. The obtained Fe 3 O 4 particles are nanocubes and nanoflakes and this formation is influenced by the base concentration and anisotropic circumstances produced by the ionic liquid and their size varies from 20 nm to 150 × 300 nm (width × length). The synthesized magnetite nanoparticles are characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, Field emission scanning electron microscopy (FE-SEM), Transmission electron microscopy (TEM) and Vibrating sample magnetometer (VSM) studies. The results show that the core of the Fe 3 O 4 nanoparticles is surrounded by a thin layer of γ-Fe 2 O 3 by topotactical partial oxidation, which is remarkably proceed with the subsequent calcination. The magnetite nanocubes have high saturation magnetization value and exhibit superparamagnetic hysteresis loop

  3. MnWO{sub 4} nanocapsules: Synthesis, characterization and its electrochemical sensing property

    Energy Technology Data Exchange (ETDEWEB)

    Muthamizh, Selvamani; Suresh, Ranganathan; Giribabu, Krishnamoorthy; Manigandan, Ramadoss; Praveen Kumar, Sivakumar; Munusamy, Settu; Narayanan, Vengidusamy, E-mail: vnnara@yahoo.co.in

    2015-01-15

    Highlights: • Synthesis of MnWO{sub 4} nanocapsules without use of any other external reagent. • High crystalline MnWO{sub 4} was obtained with phase purity. • Electrochemical sensing platform based on MnWO{sub 4} for sensing quercetin. • Micromolar detection ability of MnWO{sub 4} modified GCE. - Abstract: Manganese tungstate (MnWO{sub 4}) was synthesized by surfactant free precipitation method. MnWO{sub 4} was characterized by using various spectroscopic techniques. The phase, crystalline nature and the morphological analysis were carried out using XRD, scanning electron microscopy (SEM), and high resolution transmission electron microscopy (HR-TEM). Further, FT-IR, Raman, and DRS-UV–Vis spectral analysis were carried out in order to ascertain the optical property and the presence of functional groups. From the analysis, the morphology of the MnWO{sub 4} was observed to be in capsules with breadth and thickness were in nm range. The oxidation state of tungsten (W), and manganese (Mn) were investigated using X-ray photo electron spectroscopy (XPS) and electron paramagnetic resonance spectroscopy (EPR). The synthesized MnWO{sub 4} nanocapsules were used to modify glassy carbon electrode (GCE) to detect quercetin.

  4. Synthesis of Mn3O4 nanoparticles via chemical precipitation approach for supercapacitor application

    International Nuclear Information System (INIS)

    Gnana Sundara Raj, Balasubramaniam; Asiri, Abdullah M.; Wu, Jerry J.; Anandan, Sambandam

    2015-01-01

    Highlights: • Facile synthesis of Mn 3 O 4 nanoparticles at room temperature via simple chemical precipitation method. • Fabricated supercapacitor device shows maximum specific capacitance in 1 M Na 2 SO 4 . • 77% of specific capacitance is retained even after 1000 cycles. - Abstract: A simple chemical precipitation method has been used for the preparation of Mn 3 O 4 nanoparticles at room temperature. The crystal structure and morphology studies of the resulting Mn 3 O 4 nanoparticles were characterized by powder X-ray diffraction (XRD), Fourier transform-infrared spectroscopy (FT-IR), Raman spectroscopy, scanning electron microscope (SEM), transmission electron microscope (TEM), N 2 adsorption and desorption and X-ray photoelectron spectroscopy (XPS). The electrochemical properties of the Mn 3 O 4 nanoparticles were then investigated using cyclic voltammetry (CV), galvanostatic charge–discharge and electrochemical impedance spectroscopy (EIS) analysis. The supercapacitive properties of Mn 3 O 4 nanoparticles in the presence of 1 M Na 2 SO 4 exhibited a high specific capacitance of 322 F g −1 at a current density of 0.5 mA cm −2 in the potential range from −0.1 to +0.9 V and about 77% of the initial capacitance was retained after 1000 cycles, indicating that the Mn 3 O 4 electrode owns a good electrochemical stability and capacitance retention capability. The results suggest that the obtained Mn 3 O 4 nanoparticles is a promising electrode material for supercapacitor applications

  5. Hydrothermal synthesis, structural elucidation, spectroscopic studies, thermal behavior and luminescence properties of a new 3-d compound: FeAlF2(C10H8N2)(HPO4)2(H2O)

    Science.gov (United States)

    Bouzidia, Nabaa; Salah, Najet; Hamdi, Besma; Ben Salah, Abdelhamid

    2017-04-01

    The study of metal phosphate has been a proactive field of research thanks to its applied and scientific importance, especially in terms of the development of optical devices such as solid state lasers as well as optical fibers. The present paper seeks to investigate the synthesis, crystal structure, elemental analysis and properties of FeAlF2(C10H8N2)(HPO4)2(H2O) compound investigated by spectroscopic studies (FT-IR and FT-Raman), thermal behavior and luminescence. The Hirshfeld surface analysis and 2-D fingerprint plot have been performed to explore the behavior of these weak interactions and crystal cohesion. This investigation shows that the molecules are connected by hydrogen bonds of the type Osbnd H⋯O and Osbnd H⋯F. In addition, the 2,2'‒bipyridine ligand plays a significant role in the construction of 3-D supramolecular framework via π‒π stacking. FT‒IR and FT‒Raman spectra were used so as to ease the responsibilities of the vibration modes of the title compound. The thermal analysis (TGA) study shows a mass loss evolution as a temperature function. Finally, the optical properties were evaluated by photoluminescence spectroscopy.

  6. Synthesis, X-ray crystallography characterization, vibrational spectroscopic, molecular electrostatic potential maps, thermodynamic properties studies of N,N'-di(p-thiazole)formamidine.

    Science.gov (United States)

    Rofouei, M K; Fereyduni, E; Sohrabi, N; Shamsipur, M; Attar Gharamaleki, J; Sundaraganesan, N

    2011-01-01

    In this work, we will report a combined experimental and theoretical study on molecular and vibrational structure of N,N'-di(p-thiazole)formamidine (DpTF). DpTF has been synthesized and characterized by elemental analysis, FT-IR, FT-Raman, 1H NMR, 13C NMR spectroscopy and X-ray single crystal diffraction. The FT-IR and FT-Raman spectra of DpTF were recorded in the solid phase. The optimized geometry was calculated by HF and B3LYP methods using 6-31G(d) basis set. The FT-IR and FT-Raman spectra of DpTF was calculated at the HF/B3LYP/6-31G(d) level and were interpreted in terms of potential energy distribution (PED) analysis. The scaled theoretical wavenumber showed very good agreement with the experimental values. A detailed interpretation of the infrared and Raman spectra of DpTF was reported. On the basis of vibrational analyses, the thermodynamic properties of the title compound at different temperatures have been calculated, revealing the correlations between Cp,m°, Sm°, Hm° and temperatures. Furthermore, molecular electrostatic potential maps (MESP) and total dipole moment properties of the compound have been calculated. Copyright © 2010 Elsevier B.V. All rights reserved.

  7. Synthesis of 2.5 nm colloidal iridium nanoparticles with strong surface enhanced Raman scattering activity

    International Nuclear Information System (INIS)

    Cui, Malin; Zhao, Yuan; Wang, Chan; Song, Qijun

    2016-01-01

    Colloidal iridium nanoparticles (IrNPs) were synthesized through an environmentally friendly approach by using trisodium citrate as the capping molecule in an aqueous medium. The resulting colloidal IrNPs have a typical diameter of 2.5 nm and display absorption bands at 250, 400 and 600 nm. They possess uniform morphology, good dispersibility, excellent stability in water, and exhibit strong surface enhanced Raman scattering (SERS) activity with an enhancement factor (EF) of 3.5 × 10 5 at the 1512 cm -1 peak when using Rhodamine 6G as the probe molecule. The excellent SERS performance of the IrNPs was exemplarily applied to the determination of the industrial colorant Sudan Red I. The peak intensity of the Raman band at 1236 cm -1 is linearly related to the concentration of Sudan Red I which can be determined by SERS in the 2 nM to 8 μM concentration range with a limit of detection as low as 0.6 nM. In our perception, this strong SERS activity of the IrNPs has a large potential in the SERS-based quantitation of various chemical substances. (author)

  8. CuO and Co3O4 Nanoparticles: Synthesis, Characterizations, and Raman Spectroscopy

    Directory of Open Access Journals (Sweden)

    M. Rashad

    2013-01-01

    Full Text Available Copper oxide and cobalt oxide (CuO, Co3O4 nanocrystals (NCs have been successfully prepared in a short time using microwave irradiation without any postannealing treatment. Both kinds of nanocrystals (NCs have been prepared using copper nitrate and cobalt nitrate as the starting materials and distilled water as the solvent. The resulted powders of nanocrystals (NCs were characterized by X-ray diffraction (XRD, transmission electron microscopy (TEM, scanning electron microscopy (SEM, and atomic force microscopy (AFM measurements. The obtained results confirm the presence of the both of oxides nanopowders produced during chemical precipitation using microwave irradiation. A strong emission under UV excitation is obtained from the prepared CuO and Co3O4 nanoparticles. The results show that the nanoparticles have high dispersion and narrow size distribution. The line scans of atomic force microscopy (AFM images of the nanocrystals (NCs sprayed on GaAs substrates confirm the results of both X-ray diffraction and transmission electron microscopy. Furthermore, vibrational studies have been carried out using Raman spectroscopic technique. Specific Raman peaks have been observed in the CuO and Co3O4 nanostructures, and the full width at half maximum (FWHM of the peaks indicates a small particle size of the nanocrystals.

  9. Rapid, green synthesis and surface-enhanced Raman scattering effect of single-crystal silver nanocubes

    Science.gov (United States)

    Mao, Aiqin; Jin, Xia; Gu, Xiaolong; Wei, Xiaoqing; Yang, Guojing

    2012-08-01

    Single-crystal silver (Ag) nanocubes have been synthesized by a rapid and green method at room temperature by adding sodium hydroxide solution to the mixed solutions of silver nitrate, glucose and polyvinylpyrrolidone (PVP). The X-ray diffraction (XRD), ultraviolet-visible (UV-visible) and transmission electron microscopy (TEM) were used to characterize the phase composition and morphology. The results showed that the as-prepared particles were single-crystal Ag nanocubes with edge lengths of around 77 nm and a growing direction along {1 0 0} facets. As substrates for surface-enhanced Raman scattering (SERS) experiment on crystal violet (CV), the SERS enhancement factor of the as-prepared Ag nanocubes were measured to be 5.5 × 104, indicating potential applications in chemical and biological analysis.

  10. High-sensitivity Raman spectrometer to study pristine and irradiated interstellar ice analogs.

    Science.gov (United States)

    Bennett, Chris J; Brotton, Stephen J; Jones, Brant M; Misra, Anupam K; Sharma, Shiv K; Kaiser, Ralf I

    2013-06-18

    We discuss the novel design of a sensitive, normal-Raman spectrometer interfaced to an ultra-high vacuum chamber (5 × 10(-11) Torr) utilized to investigate the interaction of ionizing radiation with low temperature ices relevant to the solar system and interstellar medium. The design is based on a pulsed Nd:YAG laser which takes advantage of gating techniques to isolate the scattered Raman signal from the competing fluorescence signal. The setup incorporates innovations to achieve maximum sensitivity without detectable heating of the sample. Thin films of carbon dioxide (CO2) ices of 10 to 396 nm thickness were prepared and characterized using both Fourier transform infrared (FT-IR) spectroscopy and HeNe interference techniques. The ν+ and ν- Fermi resonance bands of CO2 ices were observed by Raman spectroscopy at 1385 and 1278 cm(-1), respectively, and the band areas showed a linear dependence on ice thickness. Preliminary irradiation experiments are conducted on a 450 nm thick sample of CO2 ice using energetic electrons. Both carbon monoxide (CO) and the infrared inactive molecular oxygen (O2) products are readily detected from their characteristic Raman bands at 2145 and 1545 cm(-1), respectively. Detection limits of 4 ± 3 and 6 ± 4 monolayers of CO and O2 were derived, demonstrating the unique power to detect newly formed molecules in irradiated ices in situ. The setup is universally applicable to the detection of low-abundance species, since no Raman signal enhancement is required, demonstrating Raman spectroscopy as a reliable alternative, or complement, to FT-IR spectroscopy in space science applications.

  11. Green synthesis of graphene/Ag nanocomposites

    International Nuclear Information System (INIS)

    Yuan Wenhui; Gu Yejian; Li Li

    2012-01-01

    Graphical abstract: A facile and green approach to synthesis of GNS/AgNPs is reported by employing sodium citrate as reductant, and this study represents the use of biocompounds for nontoxic and scalable production of GNS/AgNPs under a suitable concentration of silver ions and the prepared GNS/AgNPs can be used in the field of disinfection. Highlights: ► Graphene/Ag nanocomposites were prepared by a green and facile strategy based on sodium citrate. ► The influence of AgNO 3 amount on particle size and size range of AgNPs was studied. ► The surface plasmon resonance properties of AgNPs on graphene was investigated. ► The antibacterial activity of silver nanoparticles was retained in the nanocomposites. - Abstract: Graphene/Ag nanocomposites (GNS/AgNPs) were fabricated via a green and facile method, employing graphite oxide (GO) as a precursor of graphene, AgNO 3 as a precursor of Ag nanoparticles, and sodium citrate as an environmentally friendly reducing and stabilizing agent. The synthesized GNS/AgNPs were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS) and Raman spectra (RS), respectively. The results indicated that graphite oxide was completely reduced to graphene, and the silver ion was reduced by sodium citrate simultaneously. Under a suitable dosage of silver ions, well-dispersed AgNPs on the graphene sheets mostly centralized at 20–25 nm. The surface plasmon resonance property of AgNPs on graphene showed that there was a interaction between AgNPs and graphene supports. In addition, antibacterial activity of silver nanoparticles was retained in the nanocomposites, suggesting that they can be potentially used as a graphene-based biomaterial.

  12. Biomolecule-assisted synthesis of Ag/reduced graphene oxide nanocomposite with excellent electrocatalytic and antibacterial performance

    Energy Technology Data Exchange (ETDEWEB)

    Fathalipour, Soghra, E-mail: fathalipour@pnu.ac.ir [Department of Chemistry, Payame Noor University, PO Box: 19395-3697, Tehran (Iran, Islamic Republic of); Pourbeyram, Sima; Sharafian, Aziaeh [Department of Chemistry, Payame Noor University, PO Box: 19395-3697, Tehran (Iran, Islamic Republic of); Tanomand, Asghar [Department of Basic Sciences, Faculty Of Medicine, Maragheh University of Medical Sciences, PO Box: 78151-55158 (Iran, Islamic Republic of); Azam, Parisa [Department of Chemistry, Payame Noor University, PO Box: 19395-3697, Tehran (Iran, Islamic Republic of)

    2017-06-01

    In this work, an environmentally friendly method was applied for the synthesis of aqueous suspension of L-cysteine modified Ag nanoparticles (NPs)-decorated reduced graphene oxide (rGO) nanocomposite. L-cysteine played a triple role as reducing agent, stabilizer and linker of Ag NPs onto the surface of rGO. The resultant nanocomposite was characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction studies (XRD), zeta potential, Raman spectroscopy, scanning electron microscopy (SEM) and energy dispersive analysis of X-ray (EDX). Meanwhile, minimum inhibitory concentration (MIC), minimum bacterial concentration (MBC), agar well diffusion and cyclic voltammetry (CV) techniques were used for the investigation of antibacterial and electrocatalytic behaviors of the nanocomposite, respectively. The obtained nanocomposite showed not only enhanced electrocatalytic activity for glucose but also excellent antibacterial activity against Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus). - Highlights: • Biocompatible reduced graphene oxide/ Ag nanocomposite was synthesized based on cysteine- Ag nanoparticles. • The reaction was carried out at room temperature without any further reducer. • The nanocomposite displayed excellent antibacterial and electrocatalytic activity against glucose.

  13. Chitosan supramolecularly cross linked with trimesic acid - Facile synthesis, characterization and evaluation of adsorption potential for chromium(VI).

    Science.gov (United States)

    Bhatt, Ronak; Sreedhar, B; Padmaja, P

    2017-11-01

    A facile synthesis of Chitosan Supramolecularly cross-linked with Trimesic Acid (CTMA) is reported in this work. The adsorption potential of CTMA for removal of hexavalent chromium was evaluated and the influence of pH, temperature, contact time and adsorbent dose on the adsorption process was investigated. The experimental results showed that CTMA could efficiently adsorb Cr 6+ and partially reduce it to the less toxic Cr 3+ state. The maximum adsorption capacity of CTMA for Cr 6+ was found to be 129.53mg/g at pH 2.0. CTMA and chromium loaded CTMA were characterised by FT-IR, Raman, TGA-DSC, SEM-EDX, XRD, ESR and XPS spectroscopic techniques. Chitosan was observed to be cross- linked with TMA via ionic, hydrogen bonding and pi-pi supramolecular interactions while adsorption of chromium onto CTMA was by electrostatic forces and hydrogen bonding. From the observed results it was evident that CTMA was successfully applied for simultaneous removal of chromium, lead and iron from chrome plating effluent. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Green synthesis of graphene from recycled PET bottle wastes for use in the adsorption of dyes in aqueous solution.

    Science.gov (United States)

    El Essawy, Noha A; Ali, Safa M; Farag, Hassan A; Konsowa, Abdelaziz H; Elnouby, Mohamed; Hamad, Hesham A

    2017-11-01

    Polyethyleneterephthalate (PET) is an important component of post-consumer plastic waste. This study focuses on the potential of utilizing "waste-treats-waste" by synthesis of graphene using PET bottle waste as a source material. The synthesized graphene is characterized by SEM, TEM, BET, Raman, TGA, and FT-IR. The adsorption of methylene blue (MB) and acid blue 25 (AB25) by graphene is studied and parameters such as contact time, adsorbent dosage were optimized. The Response Surface Methodology (RSM) is applied to investigate the effect of three variables (dye concentration, time and temperature) and their interaction on the removal efficiency. Adsorption kinetics and isotherm are followed a pseudo-second-order model and Langmuir and Freundlich isotherm models, respectively. Thermodynamic parameters demonstrated that adsorption of dye is spontaneous and endothermic in nature. The plastic waste can be used after transformation into valuable carbon-based nanomaterials for use in the adsorption of organic contaminants from aqueous solution. Copyright © 2017 Elsevier Inc. All rights reserved.

  15. FeNi{sub 3} alloy nanocrystals grown on graphene: Controllable synthesis, in-depth characterization and enhanced electromagnetic performance

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Teng; Yuan, Mengwei [Beijing Key Laboratory of Energy Conversion and Storage Materials and College of Chemistry, Beijing Normal University, Beijing 100875 (China); Islam, Saiful M. [Department of Chemistry, Northwestern University, 2145 Sheridan Road, Evanston, IL 60208 (United States); Li, Huifeng [Beijing Key Laboratory of Energy Conversion and Storage Materials and College of Chemistry, Beijing Normal University, Beijing 100875 (China); Ma, Shulan, E-mail: mashulan@bnu.edu.cn [Beijing Key Laboratory of Energy Conversion and Storage Materials and College of Chemistry, Beijing Normal University, Beijing 100875 (China); Sun, Genban, E-mail: gbsun@bnu.edu.cn [Beijing Key Laboratory of Energy Conversion and Storage Materials and College of Chemistry, Beijing Normal University, Beijing 100875 (China); Department of Materials Physics and Chemistry, University of Science and Technology Beijing, Beijing 100083 (China); Yang, Xiaojing [Beijing Key Laboratory of Energy Conversion and Storage Materials and College of Chemistry, Beijing Normal University, Beijing 100875 (China)

    2016-09-05

    FeNi{sub 3} nanocrystals as an ideal candidate for EM-wave-absorption material have a great advantage due to their excellent magnetic properties. However, its large permittivity and poor chemical stability confine its application. A strategy to improve electromagnetic performance of FeNi{sub 3}via phase-controlled synthesis of FeNi{sub 3} nanostructures grown on graphene networks has been employed in this work. The phases, structures, sizes and morphologies of FeNi{sub 3} nanocomposites were in-depth characterized by using scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), powder X-ray diffraction (XRD), Fourier transform infrared spectra (FT-IR), and Raman spectroscopy. The results of electromagnetic performance tests for the as-synthesized FeNi{sub 3} nanocomposites showed excellent microwave absorbability in comparison with the corresponding FeNi{sub 3} nanocrystals, especially in the low (2–6 GHz) and middle (6–12 GHz) frequencies. The one-pot method we utilized is simple and effective, and because of its versatility, it may be extended to prepare some magnetic metal or alloy materials via this route. - Highlights: • Monodispersed FeNi{sub 3} alloy nanocrystals have been successfully assembled on 2D graphene via a one-pot strategy. • The process ensures different crystal phase and controlled morphology and size in the monodispersed particles. • The nanocomposites exhibit excellent microwave absorbability, which is stronger than the corresponding alloy monomer.

  16. Synthesis and characterization of hydrotalcite-hydroxyapatite material doped with carbon nanotubes and its application in catalysis of transesterification reaction

    International Nuclear Information System (INIS)

    Rodrigues, E.; Barros, T.; Pereira, C.; Almeida, O.; Brasil, H.; Reis, M.A L. dos

    2018-01-01

    The aim of this study was to synthesize and characterize hydrotalcite-hydroxyapatite (HTHAp) material doped with three different proportions (1, 5 and 15% w/w) of carbon nanotubes (NTC) in order to evaluate its potential as a heterogeneous catalyst in the soybean oil methanolysis reaction. The synthesis of the HTHAp material was performed by the co-precipitation method (10≤pH≤ 11) with ultrasonic homogenization and hydrothermal treatment at 80 °C. XRD, SEM/EDS, FT-IR, Raman, N 2 physisorption and TG/DTA were the characterization techniques performed. The sample HTHAp1NTC, doped at 1% w/w, was tested as a catalyst under two temperature conditions (180 and 240 °C), 4 h reaction time, 2.5% catalyst loading and alcohol:oil ratio of 12:1. Doping contributed to improve structural, morphological and thermal stability properties of HTHAp material. The yield results achieved 35.2% (180 °C) and 40.5% (240 °C) qualifying the HTHAp material doped with CNT as a potential catalyst in the transesterification reaction. (author)

  17. Graphene–Gold Nanoparticles Hybrid—Synthesis, Functionalization, and Application in a Electrochemical and Surface-Enhanced Raman Scattering Biosensor

    Directory of Open Access Journals (Sweden)

    Ibrahim Khalil

    2016-05-01

    Full Text Available Graphene is a single-atom-thick two-dimensional carbon nanosheet with outstanding chemical, electrical, material, optical, and physical properties due to its large surface area, high electron mobility, thermal conductivity, and stability. These extraordinary features of graphene make it a key component for different applications in the biosensing and imaging arena. However, the use of graphene alone is correlated with certain limitations, such as irreversible self-agglomerations, less colloidal stability, poor reliability/repeatability, and non-specificity. The addition of gold nanostructures (AuNS with graphene produces the graphene–AuNS hybrid nanocomposite which minimizes the limitations as well as providing additional synergistic properties, that is, higher effective surface area, catalytic activity, electrical conductivity, water solubility, and biocompatibility. This review focuses on the fundamental features of graphene, the multidimensional synthesis, and multipurpose applications of graphene–Au nanocomposites. The paper highlights the graphene–gold nanoparticle (AuNP as the platform substrate for the fabrication of electrochemical and surface-enhanced Raman scattering (SERS-based biosensors in diverse applications as well as SERS-directed bio-imaging, which is considered as an emerging sector for monitoring stem cell differentiation, and detection and treatment of cancer.

  18. Design and synthesis of nanomaterials for surface-enhanced Raman scattering, fuel cell technology, and photonics

    Science.gov (United States)

    Camargo, Pedro Henrique Cury

    In the first part of my dissertation, I developed two approaches for selectively probing the SERS activities of individual hot spots, i.e., experimentally detect the SERS signals only for the molecules that are trapped within the hot-spot region in individual Ag nanoparticle dimers. Then, I performed a systematic investigation on the SERS activity of individual dimers composed of two closed spaced Ag nanoparticles. By utilizing Ag nanoparticles displaying a variety of well-defined shapes, sizes and orientations to construct the dimers, I were able to precisely correlate the detected SERS signals to the specific geometry of individual hot spots. In the second part of this dissertation, I performed a systematic investigation on the galvanic replacement reaction between PtCl62- and Pd nanocrystals with well-defined shapes including octahedra, nanocubes, and nanorods. The resultant hollow Pd-Pt bimetallic nanostructures were employed as electrocatalysts for the oxygen reduction reaction (ORR). Our results demonstrated that the nanostructures derived from Pd octahedra displayed the highest ORR activity, being 1.7 times more active based on equivalent Pt mass than the commercial Pt/C. I also conducted a mechanistic study on the galvanic replacement reaction between AuCl4- and Pd nanorods. Differently from the Pd-Pt system, a new type of hybrid nanostructure in the tadpole shape consisting of a Au head and a Pd tail was obtained due to a localized galvanic replacement mechanism. As an extension of my work to develop new electrocatalysts for the ORR, a templateengaged reaction was utilized for the synthesis of RuSe2+delta nanotubes. The RuSe2+delta nanotubes were active towards the ORR and displayed no loss in activity in the presence of methanol, as opposed to commercial Pt/C. Finally, the template-engaged reaction was applied to the synthesis of Se MSe (M = Zn, Cd or Pb) colloidal spheres having similar sizes but different compositions. They were utilized as building

  19. Aplicação de análise multivariada aos dados de espectroscopia no infravermelho obtidos na polimerização in situ de adesivo à base de cianoacrilato Multivariate analyses on FT-IR data of polymerization in situ of cyanoacrylate adhesive

    Directory of Open Access Journals (Sweden)

    Francisco A. A. Miranda

    1998-06-01

    Full Text Available A polimerização de adesivo à base de cianoacrilato foi acompanhada por FT-IR durante 30 minutos. A aplicação das técnicas de estatística multivariada (análise de agrupamento hierárquico e a análise dos componentes principais aos espectros de infravermelho, permitiram uma melhor identificação das diferenças espectrais entre monômero e polímero e possibilitou, também, inferir que a quantidade de monômero e do mero no polímero se eqüivalem com seis minutos de polimerização. A técnica de infravermelho mostrou-se uma ferramenta adequada para o acompanhamento da cinética de reação de adesivo à base de cianoacrilato, que torna-se ainda mais eficiente quando associada às técnicas de estatística multivariada.The polymerization of a cyanoacrylate adhesive was accompanied by FT-IR during 30 minutes. The application of multivariate statistics techniques (Hierarchical Clusters Analyses and Principal Components on infrared spectra allowed a better identification of spectral differences between monomer and polymer and also permitted to infer that the quantity of monomer and of mer of the polymer are equal in six minutes polymerization (half-life. The infrared technique appeared as an apropriate tool for observing the kinetics of cyanoacrylate adhesive reaction, which becomes even more efficient when associated to multivariate statistics techniques.

  20. Quaternary Alkylammonium Conjugates of Steroids: Synthesis, Molecular Structure, and Biological Studies

    Directory of Open Access Journals (Sweden)

    Bogumił Brycki

    2015-11-01

    Full Text Available The methods of synthesis as well as physical, spectroscopic (1H-NMR, 13C-NMR, and FT-IR, ESI-MS, and biological properties of quaternary and dimeric quaternary alkylammonium conjugates of steroids are presented. The results were contrasted with theoretical calculations (PM5 methods and potential pharmacological properties (PASS. Alkylammonium sterols exhibit a broad spectrum of antimicrobial activity comparable to squalamine.

  1. Managing of gas sensing characteristic of a reduced graphene oxide based gas sensor by the change in synthesis condition: A new approach for electronic nose design

    Energy Technology Data Exchange (ETDEWEB)

    Alizadeh, Taher, E-mail: talizadeh@ut.ac.ir [Department of Analytical Chemistry, Faculty of Chemistry, University College of Science, University of Tehran, P.O. Box 14155-6455, Tehran (Iran, Islamic Republic of); Hamedsoltani, Leyla [Department of Applied Chemistry, Faculty of Science, University of Mohaghegh Ardabili, Ardabil (Iran, Islamic Republic of)

    2016-11-01

    Natural graphite was oxidized and exfoliated via two different methods, leading to two types of graphene oxide (GO) materials. The obtained materials were reduced by three different reducing agents including: hydrazine hydrate, ascorbic acid and sodium borohydride, giving thus six kinds of reduced graphene oxide (RGO) materials. The obtained materials were characterized using Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy. The RGOs were then used to fabricate different gas sensors and their electrical resistances were recorded upon exposing to various volatile organic compounds vapors (VOCs). Gas sensing selectivity of each RGO was significantly affected by the synthesis condition. The RGO-based sensor array was fabricated and its capability for discrimination of seven kinds of VOCs was evaluated, utilizing principal component analysis and cluster analysis methods. Loading plot indicated that the presence of five RGO-based sensors could effectively discriminate the aimed vapors. The electronic nose, containing five kinds of RGOs, was used for the classification of seven kinds of VOCs at their different concentrations. - Highlights: • Two oxidation procedures and three reducing agents were utilized to produce six kinds of RGOs. • The synthesized different RGOs exhibited significantly different sensing behaviors. • Seven kinds of organic vapors were chosen for the evaluation of discrimination power of EN. • Using PCA, it was found that seven of six RFGOs were appropriate number to use in final EN. • The developed EN was capable of properly discrimination of tested vapors.

  2. Eco-friendly synthesis of TiO2, Au and Pt doped TiO2 nanoparticles for dye sensitized solar cell applications and evaluation of toxicity

    Science.gov (United States)

    Gopinath, K.; Kumaraguru, S.; Bhakyaraj, K.; Thirumal, S.; Arumugam, A.

    2016-04-01

    Driven by the demand of pure TiO2, Au and Pt doped TiO2 NPs were successfully synthesized using Terminalia arjuna bark extract. The eco-friendly synthesized NPs were characterized by UV-Vis-DRS, ATR-FT-IR, PL, XRD, Raman, SEM with EDX and TEM analysis. The synthesized NPs were investigation for dye sensitized solar cell applications. UV-Vis-Diffused Reflectance Spectra clearly showed that the expected TiO2 inter band absorption below 306 nm, incorporation of gold shows surface plasma resonant (SPR) near 555 nm and platinum incorporated TiO2 NPs shows absorbance at 460 nm. The energy conversion efficiency for Au doped TiO2 NPs when compared to pure and Pt doped TiO2 NPs. In addition to that, Au noble metal present TiO2 matrix and an improve open-circuit voltage (Voc) of DSSC. Synthesized NPs was evaluated into antibacterial and antifungal activities by disk diffusion method. It is observed that NPs have not shown any activities in all tested bacterial and fungal strains. In this eco-friendly synthesis method to provide non toxic and environmental friendly nanomaterials can be used for solar energy device application.

  3. Synthesis of NiO–Al{sub 2}O{sub 3} nanocomposites by sol–gel process and their use as catalyst for the oxidation of styrene

    Energy Technology Data Exchange (ETDEWEB)

    Yadav, Sudheer Kumar; Jeevanandam, P., E-mail: jeevafcy@iitr.ac.in

    2014-10-15

    Highlights: • NiO–Al{sub 2}O{sub 3} nanocomposites have been synthesized by sol–gel method. • The synthesis takes shorter time (∼48 h) compared to reported methods. • The nanocomposites show high catalytic activity for the oxidation of styrene compared to NiO. - Abstract: NiO–Al{sub 2}O{sub 3} nanocomposites were prepared by sol–gel method. The synthesized nanocomposites were characterized by X-ray diffraction, FT-IR spectroscopy, Raman spectroscopy, field emission scanning electron microscopy coupled with energy dispersive X-ray analysis, transmission electron microscopy, diffuse reflectance spectroscopy and magnetic measurements. XRD results indicate that the NiO–Al{sub 2}O{sub 3} nanocomposites consist of small NiO crystallites (mean size ∼2.6 nm). TEM results indicate uniform distribution of NiO nanoparticles in the Al{sub 2}O{sub 3} matrix. Increase in the band gap of NiO in the nanocomposites compared to pure NiO nanoparticles is observed and the nanocomposites show superparamagnetic behaviour. The NiO–Al{sub 2}O{sub 3} nanocomposites show high catalytic activity for the oxidation of styrene using tert-butyl hydroperoxide as the oxidant and also show higher selectivity for styrene oxide with higher total conversion compared to pure NiO nanoparticles.

  4. Synthesis, structural, optical and Raman studies of pure and lanthanum doped ZnSe nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Pushpendra, E-mail: push.nac@gmail.com [Department of Physics, Faculty of Science, Banaras Hindu University, Varanasi 221005 (India); Institute of Atomic and Molecular Sciences, Academia Sinica, Taipei 11529, Taiwan (China); Singh, Jai [Department of Physics, Faculty of Science, Banaras Hindu University, Varanasi 221005 (India); Department of Materials Science and Engineering, Pusan National University, 30 Jangjeon-dong, Geumjeong-gu, Busan 609-735 (Korea, Republic of); Pandey, Mukesh Kumar [Institute of Atomic and Molecular Sciences, Academia Sinica, Taipei 11529, Taiwan (China); Jeyanthi, C.E. [Research and Development Centre, Bharathiar University, Coimbatore 641 046 (India); Siddheswaran, R. [Department of Materials Science and Engineering, University of Concepcion, Concepcion (Chile); Paulraj, M. [Department of Physics, Faculty of Physical sciences and Mathematics, University of Concepcion, Casilla 160, Concepcion (Chile); Hui, K.N. [Department of Materials Science and Engineering, Pusan National University, 30 Jangjeon-dong, Geumjeong-gu, Busan 609-735 (Korea, Republic of); Hui, K.S., E-mail: kshui@hanyang.ac.kr [Department of Mechanical Engineering, Hanyang University, 17 Haengdang-dong, Seongdong-gu, Seoul 133-791 (Korea, Republic of)

    2014-01-01

    Graphical abstract: - Highlights: • Template-free synthesis of ZnSe and ZnSe:La nanoparticles was developed at low temperature 100 °C. • Cubic ZnSe and ZnSe:La nanoparticles were obtained by chemical route. • As-synthesized ZnSe:La nanoparticles showed higher emission intensity than ZnSe nanoparticles. • Band gap (E{sub g}) of ZnSe nanoparticles was bigger than ZnSe nanoparticles due to nanosized effect. - Abstract: In this work, a simple, effective and reproducible chemical synthetic route for the production of high-quality, pure ZnSe nanoparticles (NPs), and lanthanum-doped ZnSe (ZnSe:La) NPs is presented. The wide bandgap, luminescent pure ZnSe and ZnSe:La NPs has been synthesized at a low temperature (100 °C) in a single template-free step. The size and optical bandgap of the NPs was analyzed from powder X-ray diffraction (XRD), UV–visible (UV–vis) spectroscopy, transmission electron microscopy (TEM), and high resolution transmission electron microscopy (HRTEM). A broad photoluminescence (PL) emission across the visible spectrum has been demonstrated by a systematic blue-shift in emission due to the formation of small nanoparticles. Here, contribution to emission intensity from surface states of NPs increases with La doping. TEM data revealed that the average size of ZnSe and ZnSe:La NPs is 14 and 8 nm, respectively. On the other hand, band gap energy E{sub g} of ZnSe and ZnSe:La NPs were found to be 3.59 eV and 3.65 eV, respectively. Results showed that hydrazine hydrate played multiple roles in the formation of ZnSe and ZnSe:La NPs. A possible reaction mechanism for the growth of NPs is also discussed.

  5. Sci—Fri AM: Mountain — 04: Label-free Raman spectroscopy of single tumour cells detects early radiation-induced glycogen synthesis associated with increased radiation resistance

    International Nuclear Information System (INIS)

    Matthews, Q; Lum, JJ; Isabelle, M; Harder, S; Jirasek, A; Brolo, AG

    2014-01-01

    Purpose: To use label-free Raman spectroscopy (RS) for early treatment monitoring of tumour cell radioresistance. Methods: Three human tumour cell lines, two radioresistant (H460, SF 2 = 0.57 and MCF7, SF 2 = 0.70) and one radiosensitive (LNCaP, SF 2 = 0.36), were irradiated with single fractions of 2, 4, 6, 8 or 10 Gy. In additional experiments, H460 and MCF7 cells were irradiated under co-treatment with the anti-diabetic drug metformin, a known radiosensitizing agent. Treated and control cultures were analyzed with RS daily for 3 days post-treatment. Single-cell Raman spectra were acquired from 20 live cells per sample, and experiments were repeated in triplicate. The combined data sets were analyzed with principal component analysis using standard algorithms. Cells from each culture were also subjected to standard assays for viability, proliferation, cell cycle, and radiation clonogenic survival. Results: The radioresistant cells (H460, MCF7) exhibited a RS molecular radiation response signature, detectable as early as 1 day post-treatment, of which radiation-induced glycogen synthesis is a significant contributor. The radiosensitive cells (LNCaP) exhibited negligible glycogen synthesis. Co-treatment with metformin in MCF7 cells blocked glycogen synthesis, reduced viability and proliferation, and increased radiosensitivity. Conversely, metformin co-treatment in H460 cells did not produce these same effects; importantly, both radiation-induced synthesis of glycogen and radiosensitivity were unaffected. Conclusions: Label-free RS can detect early glycogen synthesis post-irradiation, a previously undocumented metabolic mechanism associated with tumour cell radioresistance that can be targeted to increase radiosensitivity. RS monitoring of intratumoral glycogen may provide new opportunities for personalized combined modality radiotherapy treatments

  6. Sci—Fri AM: Mountain — 04: Label-free Raman spectroscopy of single tumour cells detects early radiation-induced glycogen synthesis associated with increased radiation resistance

    Energy Technology Data Exchange (ETDEWEB)

    Matthews, Q; Lum, JJ [BC Cancer Agency — Vancouver Island Centre (Canada); Isabelle, M; Harder, S; Jirasek, A [Physics and Astronomy, University of Victoria (Australia); Brolo, AG [Chemistry, University of Victoria (Australia)

    2014-08-15

    Purpose: To use label-free Raman spectroscopy (RS) for early treatment monitoring of tumour cell radioresistance. Methods: Three human tumour cell lines, two radioresistant (H460, SF{sub 2} = 0.57 and MCF7, SF{sub 2} = 0.70) and one radiosensitive (LNCaP, SF{sub 2} = 0.36), were irradiated with single fractions of 2, 4, 6, 8 or 10 Gy. In additional experiments, H460 and MCF7 cells were irradiated under co-treatment with the anti-diabetic drug metformin, a known radiosensitizing agent. Treated and control cultures were analyzed with RS daily for 3 days post-treatment. Single-cell Raman spectra were acquired from 20 live cells per sample, and experiments were repeated in triplicate. The combined data sets were analyzed with principal component analysis using standard algorithms. Cells from each culture were also subjected to standard assays for viability, proliferation, cell cycle, and radiation clonogenic survival. Results: The radioresistant cells (H460, MCF7) exhibited a RS molecular radiation response signature, detectable as early as 1 day post-treatment, of which radiation-induced glycogen synthesis is a significant contributor. The radiosensitive cells (LNCaP) exhibited negligible glycogen synthesis. Co-treatment with metformin in MCF7 cells blocked glycogen synthesis, reduced viability and proliferation, and increased radiosensitivity. Conversely, metformin co-treatment in H460 cells did not produce these same effects; importantly, both radiation-induced synthesis of glycogen and radiosensitivity were unaffected. Conclusions: Label-free RS can detect early glycogen synthesis post-irradiation, a previously undocumented metabolic mechanism associated with tumour cell radioresistance that can be targeted to increase radiosensitivity. RS monitoring of intratumoral glycogen may provide new opportunities for personalized combined modality radiotherapy treatments.

  7. The synthesis of four-layer gold-silver-polymer-silver core-shell nanomushroom with inbuilt Raman molecule for surface-enhanced Raman scattering

    Science.gov (United States)

    Jiang, Tao; Wang, Xiaolong; Zhou, Jun

    2017-12-01

    A facial two-step reduction method was proposed to synthesize four-layer gold-silver-polymer-silver (Au@Ag@PSPAA@Ag) core-shell nanomushrooms (NMs) with inbuilt Raman molecule. The surface-enhanced Raman scattering (SERS) intensity of 4MBA adhered on the surface of Au core gradually increased with the modification of middle Ag shell and then Ag mushroom cap due to the formation of two kinds of ultra-small interior nanogap. Compared with the initial Au nanoparticles, the SERS enhancement ratio of the Au@Ag@PSPAA@Ag NMs approached to nearly 40. The novel core-shell NMs also exhibited homogeneous SERS signals for only one sample and reproducible signals for 10 different samples, certified by the low relative standard deviation values of less than 10% and 15% for the character peaks of 4-mercaptobenzoic acid, respectively. Such a novel four-layer core-shell nanostructure with reliable SERS performance has great potential application in quantitative SERS-based immunoassay.

  8. Synthesis and characterization of MCM-41-supported nano zirconia catalysts

    Directory of Open Access Journals (Sweden)

    Mohamed S. Abdel Salam

    2015-03-01

    Full Text Available Series of MCM-41 supported sulfated Zirconia (SZ catalysts with different loadings (2.5–7.5% wt. were prepared using direct impregnation method. The acquired solid catalysts were characterized structurally and chemically using X-RD, HRTEM, BET, FT-IR, Raman spectroscopy and TPD analysis. The acidity of the solid catalysts was investigated through cumene cracking and isopropanol dehydration at different temperatures. As the SZ loading increases, the surface acidity of the mesoporous catalysts was enhanced, this was reflected by the higher catalytic activity toward cumene cracking and isopropanol dehydration.

  9. Piper betle-mediated green synthesis of biocompatible gold nanoparticles

    Science.gov (United States)

    Punuri, Jayasekhar Babu; Sharma, Pragya; Sibyala, Saranya; Tamuli, Ranjan; Bora, Utpal

    2012-08-01

    Here, we report the novel use of the ethonolic leaf extract of Piper betle for gold nanoparticle (AuNP) synthesis. The successful formation of AuNPs was confirmed by UV-visible spectroscopy, and different parameters such as leaf extract concentration (2%), gold salt concentration (0.5 mM), and time (18 s) were optimized. The synthesized AuNPs were characterized with different biophysical techniques such as transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), and energy-dispersive X-ray spectroscopy (EDX). TEM experiments showed that nanoparticles were of various shapes and sizes ranging from 10 to 35 nm. FT-IR spectroscopy revealed that AuNPs were functionalized with biomolecules that have primary amine group -NH2, carbonyl group, -OH groups, and other stabilizing functional groups. EDX showed the presence of the elements on the surface of the AuNPs. FT-IR and EDX together confirmed the presence of biomolecules bounded on the AuNPs. Cytotoxicity of the AuNPs was tested on HeLa and MCF-7 cancer cell lines, and they were found to be nontoxic, indicating their biocompatibility. Thus, synthesized AuNPs have potential for use in various biomedical applications.

  10. Synthesis of Ag nanobars in the presence of single-crystal seeds and a bromide compound, and their surface-enhanced Raman scattering (SERS) properties.

    Science.gov (United States)

    Zhang, Qiang; Moran, Christine H; Xia, Xiaohu; Rycenga, Matthew; Li, Naixu; Xia, Younan

    2012-06-19

    This Article describes the synthesis of Ag nanobars with different aspect ratios using a seed-mediated method and evaluation of their use for surface-enhanced Raman scattering (SERS). The formation of Ag nanobars was found to critically depend on the introduction of a bromide compound into the reaction system, with ionic salts being more effective than covalent molecules. We examined single-crystal seeds with both spherical and cubic shapes and found that Ag nanobars grown from spherical seeds had much higher aspect ratios than those grown from cubic seeds. The typical product of a synthesis contained nanocrystals with three different morphologies: nanocubes, nanobars with a square cross section, and nanobars with a rectangular cross section. Their formation can be attributed to the difference in growth rates along the three orthogonal directions. The SERS enhancement factor of the Ag nanobar was found to depend on its aspect ratio, its orientation relative to the laser polarization, and the wavelength of excitation.

  11. Sol-gel synthesis and characterizations of crystalline NaGd(WO4)2 powder for anisotropic transparent ceramic laser application

    Science.gov (United States)

    Durairajan, A.; Thangaraju, D.; Balaji, D.; Moorthy Babu, S.

    2013-02-01

    NaGd(WO4)2 powders were synthesized at different pH (3.5, 4.5, 5.5, 6.5 and 7.5) values by conventional Pechini method. Sodium and gadolinium nitrate salts and ammonium paratungstate are used as starting precursors. Metal cations were chelated by citric acid and individual citrates were bound together with ethylene glycol. Synthesized gel was analyzed using differential thermal analysis (DTA), thermo gravimetric (TG) and FT-IR spectroscopy to understand the degradation of gel and formation of metal citrates. Calcined powders (250, 600, 700 and 800 °C) were characterized by powder XRD, FT-IR, Raman and FE-SEM analysis. The temperature dependent phase formation was examined by powder XRD. The morphological changes at different pH derived powders were observed with FE-SEM micrographs. Stepwise organic liberation with respect to temperature and presence of carbon content in the pre-fired powder were analyzed using FT-IR analysis. Raman spectrum reveals disordered tungstate vibrations in the NGW matrix.

  12. Synthesis of anti-aggregation silver nanoparticles based on inositol hexakisphosphoric micelles for a stable surface enhanced Raman scattering substrate

    International Nuclear Information System (INIS)

    Wang Na; Yang Haifeng; Zhu Xuan; Zhang Rui; Wang Yao; Huang Guanfeng; Zhang Zongrang

    2009-01-01

    We report a novel method of synthesizing a kind of silver nanoparticles aided by the inositol hexakisphosphoric micelle as a soft template and stabilizer. By controlling the reaction time, UV-vis and TEM observations of the size growth of the nanoparticles are performed. Careful examinations of surface enhanced Raman scattering (SERS) spectra of 2-mercaptopyridine (2-Mpy) on the as-produced silver nanoparticles exhibit very stable and reproducible Raman signals within about 4 months.

  13. Synthesis and Characterization of New ‎Condensation Polymers Based on New ‎Aromatic di-ethers

    Directory of Open Access Journals (Sweden)

    Saadon Abdulla Aowda

    2017-11-01

    Full Text Available This research includes synthesis and identification of new polymers that are expected having industrial applications in paint ships and dyes. These polymers were prepared from cheap and available materials such as glycerol and catechol, hydroquinone and resorcinol and using cheap catalyst in good yields.       The resulting compounds were identified by FT-IR, 1H-NMR, 13C-NMR, CHN, and DSC techniques. Some physical properties of these compounds were studied

  14. Green synthesis of highly fluorescent carbon quantum dots from sugarcane bagasse pulp

    Energy Technology Data Exchange (ETDEWEB)

    Thambiraj, S. [Nano-Bio Materials and Sensors Laboratory, PSG Institute of Advanced Studies, Coimbatore, 641 004, Tamil Nadu (India); Ravi Shankaran, D., E-mail: dravishankaran@hotmail.com [Nano-Bio Materials and Sensors Laboratory, PSG Institute of Advanced Studies, Coimbatore, 641 004, Tamil Nadu (India); National Centre for Nanoscience and Nanotechnology, University of Madras, Guindy Campus, Chennai, 600 025, Tamil Nadu (India)

    2016-12-30

    Graphical abstract: Schematic representation of CQDs from sugarcane bagasse carbon. - Highlights: • CQDs were synthesised from sugarcane bagasse waste with top down approaches. • Synthesis method is green, simple and efficient process. • CQDs possess high quantum yield, good stability and highly fluorescent in nature. • The morphological and topographical study of CQDs was done by HR-TEM and AFM and was observed that the average size is 4.1 ± 0.17 nm and surface thickness is 5 nm. - Abstract: Carbon quantum dots (CQDs) have great potential due to its advantageous characteristics of highly fluorescent nature and good stability. In this study, we aimed to develop a simple and efficient method for the green synthesis of fluorescent CQDs from sugarcane bagasse, a renewable and sustainable resource. The process involves the top down approach of chemical oxidation followed by exfoliation of sugarcane carbon. The synthesized CQDs was characterized by UV–vis absorption spectroscopy, Spectrofluorophotometry, Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Raman spectroscopy, X-ray photon spectroscopy (XPS), Atomic force microscopy (AFM) and High-resolution transmission electron microscopy (HR-TEM). The synthesized CQDs possess stable fluorescent properties, good bio-compatibility and high quantum yield. The CQDs are highly crystalline with longitudinal dimensions of 4.1 ± 0.17 nm with an average roughness of around 5 nm. The XRD and TEM analysis indicates that the synthesized CQDs possess face centred cubic crystal structure. The results suggest that the proposed CQDs could be utilized for bio-sensor, bio-imaging and drug delivery applications.

  15. Synthesis of cerium oxide nanoparticles using Gloriosa superba L. leaf extract and their structural, optical and antibacterial properties

    Energy Technology Data Exchange (ETDEWEB)

    Arumugam, Ayyakannu, E-mail: sixmuga@yahoo.com [Department of Nanoscience and Technology, Alagappa University, Karaikudi 630 004, Tamil Nadu (India); Karthikeyan, Chandrasekaran; Haja Hameed, Abdulrahman Syedahamed [PG and Research Department of Physics, Jamal Mohamed College, Tiruchirappalli 620 020, Tamil Nadu (India); Gopinath, Kasi; Gowri, Shanmugam; Karthika, Viswanathan [Department of Nanoscience and Technology, Alagappa University, Karaikudi 630 004, Tamil Nadu (India)

    2015-04-01

    CeO{sub 2} nanoparticles (NPs) were green synthesized using Gloriosa superba L. leaf extract. The synthesized nanoparticles retained the cubic structure, which was confirmed by X-ray diffraction studies. The oxidation states of the elements (C (1s), O (1s) and Ce (3d)) were confirmed by XPS studies. TEM images showed that the NPs possessed spherical shape and particle size of 5 nm. The Ce–O stretching bands were observed at 451 cm{sup −1} and 457 cm{sup −1} from the FT-IR and Raman spectra respectively. The band gap of the CeO{sub 2} NPs was estimated as 3.78 eV from the UV–visible spectrum. From the photoluminescence measurements, the broad emission composed of eight different bands were found. The antibacterial studies performed against a set of bacterial strains showed that Gram positive (G +) bacteria were relatively more susceptible to the NPs than Gram negative (G −) bacteria. The toxicological behavior of CeO{sub 2} NPs was found due to the synthesized NPs with uneven ridges and oxygen defects in CeO{sub 2} NPs. - Highlights: • Phytosynthesis of CeO{sub 2} NPs using Gloriosa superba leaf extract • Single step synthesis • Characterized by XRD, XPS, TEM, FTIR, Raman, UV–vis, PL and TG/DTA analyses • CeO{sub 2} NPs were of spherical shape with an average size of 5 nm. • CeO{sub 2} NPs showed highly potent antibacterial activity.

  16. Single-source-precursor synthesis of dense SiC/HfC(x)N(1-x)-based ultrahigh-temperature ceramic nanocomposites.

    Science.gov (United States)

    Wen, Qingbo; Xu, Yeping; Xu, Binbin; Fasel, Claudia; Guillon, Olivier; Buntkowsky, Gerd; Yu, Zhaoju; Riedel, Ralf; Ionescu, Emanuel

    2014-11-21

    A novel single-source precursor was synthesized by the reaction of an allyl hydrido polycarbosilane (SMP10) and tetrakis(dimethylamido)hafnium(iv) (TDMAH) for the purpose of preparing dense monolithic SiC/HfC(x)N(1-x)-based ultrahigh temperature ceramic nanocomposites. The materials obtained at different stages of the synthesis process were characterized via Fourier transform infrared (FT-IR) as well as nuclear magnetic resonance (NMR) spectroscopy. The polymer-to-ceramic transformation was investigated by means of MAS NMR and FT-IR spectroscopy as well as thermogravimetric analysis (TGA) coupled with in situ mass spectrometry. Moreover, the microstructural evolution of the synthesized SiHfCN-based ceramics annealed at different temperatures ranging from 1300 °C to 1800 °C was characterized by elemental analysis, X-ray diffraction, Raman spectroscopy and transmission electron microscopy (TEM). Based on its high temperature behavior, the amorphous SiHfCN-based ceramic powder was used to prepare monolithic SiC/HfC(x)N(1-x)-based nanocomposites using the spark plasma sintering (SPS) technique. The results showed that dense monolithic SiC/HfC(x)N(1-x)-based nanocomposites with low open porosity (0.74 vol%) can be prepared successfully from single-source precursors. The average grain size of both HfC0.83N0.17 and SiC phases was found to be less than 100 nm after SPS processing owing to a unique microstructure: HfC0.83N0.17 grains were embedded homogeneously in a β-SiC matrix and encapsulated by in situ formed carbon layers which acted as a diffusion barrier to suppress grain growth. The segregated Hf-carbonitride grains significantly influenced the electrical conductivity of the SPS processed monolithic samples. While Hf-free polymer-derived SiC showed an electrical conductivity of ca. 1.8 S cm(-1), the electrical conductivity of the Hf-containing material was analyzed to be ca. 136.2 S cm(-1).

  17. Synthesis and temperature dependent Raman studies of large crystalline faces topological GeBi4Te7 single crystal

    Science.gov (United States)

    Mal, Priyanath; Bera, G.; Turpu, G. R.; Srivastava, Sunil K.; Das, Pradip

    2018-05-01

    We present a study of structural and vibrational properties of topological insulator GeBi4Te7. Modified Bridgeman technique is employed to synthesize the single crystal with relatively large crystalline faces. Sharp (0 0 l) reflection confirms the high crystallinity of the single crystal. We have performed temperature dependent Raman measurement for both parallel and perpendicular to crystallographic c axis geometry. In parallel configuration we have observed seven Raman modes whereas in perpendicular geometry only four of these are identified. Appearance and disappearance of Raman modes having different intensities for parallel and perpendicular to c measurement attribute to the mode polarization. Progressive blue shift is observed with lowering temperature, reflects the increase in internal stress.

  18. Environment-dependent conformation investigation of 3-amino-1,2,4-triazole (3-AT): Raman Spectroscopy and density functional theory

    Science.gov (United States)

    Meng, Shuang; Zhao, Yanying; Xue, Jiadan; Zheng, Xuming

    2018-02-01

    In the paper, diverse tautomers of 3-amino-1,2,4-triazole (3AT) in solid and polar solvent have been explored by FT-IR, FT-Raman and 488 nm Raman experiments combing with quantum chemical theoretical calculation using PCM solvent model and normal mode analysis. The vibrational spectra prefer the 3-amino-1,2,4-2H-triazole (2H-3AT) dimer in solid, while in a polar solvent 3AT is apt to the 3-amino-1,2,4-2H-triazole (2H-3AT) monomer. The significant wavenumber difference and Raman intensity patterns in solid and different solvents are induced by hydrogen bond perturbation along > NH ⋯ N ≤ hydrogen bonds on five-membered N-heterocyclic ring. The ground state proton transfer reaction mechanism along the five-membered N-heterocyclic ring is supported by intermolecular hydrogen bonding between 3AT and protonic solvent molecules.

  19. X-ray structure determination, Hirshfeld surface analysis, spectroscopic (FT-IR, NMR, UV-Vis, fluorescence), non-linear optical properties, Fukui function and chemical activity of 4‧-(2,4-dimethoxyphenyl)-2,2‧:6‧,2″-terpyridine

    Science.gov (United States)

    Demircioğlu, Zeynep; Yeşil, Ahmet Emin; Altun, Mehmet; Bal-Demirci, Tülay; Özdemir, Namık

    2018-06-01

    The compound 4‧-(2,4-dimethoxyphenyl)-2,2‧:6‧,2″-terpyridine (Mtpyr) was synthesized and investigated using X-ray single crystal structure determination, combined with Hirshfeld topology analysis of the molecular packing. In addition, Mtpyr was characterized by experimental and theoretical FT-IR, UV-Vis, 1H NMR, 13C NMR and fluorescence emission spectra. The optimized molecular geometry (bond length, bond angle, torsion angle), the complete vibrational frequency and all other theoretical computations were calculated by using density functional theory (DFT) B3LYP method with the help of 6-311++G(d,p) basis set. From the recorded UV-Vis spectrum, the electronic properties such as excitation energies, wavelength and oscillator strength are evaluated by TD-DFT in chloroform solution. The 1H and 13C nuclear magnetic resonance (NMR) chemical shifts of the molecule were calculated by the gauge-independent atomic orbital (GIAO) method and compared with experimental results. The calculated HOMO-LUMO band gap energies confirmed that charge transfer and chemical stability within the molecule. The hyperconjugative interaction energy E(2) and electron densities of donor (i) and acceptor (j) bonds were calculated using natural bond orbital (NBO) analysis. Besides Mulliken and natural population charges (NPA), non-linear optic properties (NLO), Fukui Function analysis, molecular electrostatic potential (MEP) were also computed which helps to identifying the electrophilic/nucleophilic nature.

  20. Sol-gel synthesis and characterization of SiO{sub 2}/PEG hybrid materials containing quercetin as implants with antioxidant properties

    Energy Technology Data Exchange (ETDEWEB)

    Catauro, Michelina; Bollino, Flavia [Department of Industrial and Information Engineering, Second University of Naples, Via Roma 21, 81031 Aversa (Italy); Gloria, Antonio [Institute of Polymers, Composites and Biomaterials - National Research Council of Italy, V.le J. F. Kennedy 54 - Mostra d’Oltremare Pad. 20, 80125 Naples (Italy)

    2016-05-18

    In the present work, Silica/Polyethylene glycol (PEG) hybrid nanocomposites containing an antioxidant agent, the quercetin, were synthesized via sol-gel to be used as implants with antioxidant properties. Fourier transform infrared (FT-IR) analysis proved that a modification of both polymer and quercetin occurs due to synthesis process. Scanning electron microscope (SEM) showed that the proposed materials were hybrid nanocomposites. The bioactivity was ascertained by soaking the samples in a simulated body fluid (SBF).

  1. Biological sensing with surface-enhanced Raman spectroscopy (SERS) using a facile and rapid silver colloid-based synthesis technique

    Science.gov (United States)

    Smyth, C.; Mehigan, S.; Rakovich, Y. P.; Bell, S. E. J.; McCabe, E. M.

    2011-03-01

    Optical techniques towards the realisation of sensitive and selective biosensing platforms have received a considerable amount of attention in recent times. Techniques based on interferometry, surface plasmon resonance, field-effect transistors and waveguides have all proved popular, and in particular, spectroscopy offers a large range of options. Raman spectroscopy has always been viewed as an information rich technique in which the vibrational frequencies reveal a lot about the structure of a compound. The issue with Raman spectroscopy has traditionally been that its rather low cross section leads to poor limits-of-detection. In response to this problem, Surface-enhanced Raman Scattering (SERS), which increases sensitivity by bringing the sample in contact with many types of enhanceing substrates, has been developed. Here we discuss a facile and rapid technique for the detection of pterins using colloidal silver suspensions. Pteridine compounds are a family of biochemicals, heterocyclic in structure, and employed in nature as components of colour pigmentation and also as facilitators for many metabolic pathways, particularly those relating to the amino acid hydroxylases. In this work, xanthopterin, isoxanthopterin and 7,8- dihydrobiopterin have been examined whilst absorbed to SERS-active silver colloids. SERS, while far more sensitive than regular Raman spectroscopy, has its own issues relating to the reproducibility of substrates. In order to obtain quantitative data for the pteridine compounds mentioned above, exploratory studies of methods for introducing an internal standard for normalisation of the signals have been carried out.e

  2. Synthesis, structural, optical and morphological characterization of hematite through the precipitation method: Effect of varying the nature of the base

    Science.gov (United States)

    Lassoued, Abdelmajid; Lassoued, Mohamed Saber; Dkhil, Brahim; Gadri, Abdellatif; Ammar, Salah

    2017-08-01

    Iron oxide (α-Fe2O3) nanoparticles were synthesized using the precipitation synthesis method focusing only on (FeCl3, 6H2O), NaOH, KOH and NH4OH as raw materials. The impact of varying the nature of the base on the crystalline phase, size and morphology of α-Fe2O3 products was explored. XRD spectra revealed that samples crystallize in the rhombohedral (hexagonal) system at 800 °C.The Transmission Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM) were used to detect the morphology of synthesized nanoparticles and specify their sizes. However, the Fourier Transform Infra-Red (FT-IR) spectroscopy has permitted the observation of vibration band Fe-O. Raman spectroscopy was used not only to prove that we have synthesized hematite but also to identify their phonon modes. The Thermo Gravimetric Analysis (TGA) findings allow the thermal cycle determination of samples whereas Differential Thermal Analysis (DTA) findings allow the phase transition temperature identification. Besides, the optical investigation revealed that samples have an optical gap of about 2.1 eV. Findings highlight that the nature of the agent precipitant plays a significant role in the morphology of the products and the formation of the crystalline phase. Hematite synthesis with the base NH4OH brought about much stronger, sharper and wider diffraction peaks of α-Fe2O3. The morphology of samples are spherical with a size of about 61 nm while the size of the nanoparticles of hematite which we have synthesized with NaOH and KOH is respectively of the order of 82 and 79 nm.

  3. Single-source-precursor synthesis of dense SiC/HfCxN1-x-based ultrahigh-temperature ceramic nanocomposites

    Science.gov (United States)

    Wen, Qingbo; Xu, Yeping; Xu, Binbin; Fasel, Claudia; Guillon, Olivier; Buntkowsky, Gerd; Yu, Zhaoju; Riedel, Ralf; Ionescu, Emanuel

    2014-10-01

    A novel single-source precursor was synthesized by the reaction of an allyl hydrido polycarbosilane (SMP10) and tetrakis(dimethylamido)hafnium(iv) (TDMAH) for the purpose of preparing dense monolithic SiC/HfCxN1-x-based ultrahigh temperature ceramic nanocomposites. The materials obtained at different stages of the synthesis process were characterized via Fourier transform infrared (FT-IR) as well as nuclear magnetic resonance (NMR) spectroscopy. The polymer-to-ceramic transformation was investigated by means of MAS NMR and FT-IR spectroscopy as well as thermogravimetric analysis (TGA) coupled with in situ mass spectrometry. Moreover, the microstructural evolution of the synthesized SiHfCN-based ceramics annealed at different temperatures ranging from 1300 °C to 1800 °C was characterized by elemental analysis, X-ray diffraction, Raman spectroscopy and transmission electron microscopy (TEM). Based on its high temperature behavior, the amorphous SiHfCN-based ceramic powder was used to prepare monolithic SiC/HfCxN1-x-based nanocomposites using the spark plasma sintering (SPS) technique. The results showed that dense monolithic SiC/HfCxN1-x-based nanocomposites with low open porosity (0.74 vol%) can be prepared successfully from single-source precursors. The average grain size of both HfC0.83N0.17 and SiC phases was found to be less than 100 nm after SPS processing owing to a unique microstructure: HfC0.83N0.17 grains were embedded homogeneously in a β-SiC matrix and encapsulated by in situ formed carbon layers which acted as a diffusion barrier to suppress grain growth. The segregated Hf-carbonitride grains significantly influenced the electrical conductivity of the SPS processed monolithic samples. While Hf-free polymer-derived SiC showed an electrical conductivity of ca. 1.8 S cm-1, the electrical conductivity of the Hf-containing material was analyzed to be ca. 136.2 S cm-1.A novel single-source precursor was synthesized by the reaction of an allyl hydrido

  4. Analysis of skin oil by FT-IR spectroscopy

    Science.gov (United States)

    Dasarathy, Keshava B.; Chittur, Krishnan K.; Dasarathy, Belur V.

    1996-11-01

    Secreted skin oil is a complex mixture of lipids, cholesterol, fatty acids, and a large number of other components. Its composition varies among individuals and with changes in physiology. In this paper, the feasibility of obtaining reproducible spectra of skin oils from individuals with a very simple, noninvasive technique is reported. Using pattern recognition algorithms, spectra could be classified on the basis of ethnicity and gender. Differences in spectra between individuals were larger than those between replicate samples taken from the same individual. While there are easier techniques for gender and ethnic identification, our purpose in this paper is to show that information of some value exists in skin-oil spectra. We believe that this approach could be used for such practical discrimination problems such as the determination of high and low cholesterol levels if confirmatory information for training such classifiers were available.

  5. Preliminary Discrimination of Cheese Adulteration by FT-IR Spectroscopy

    Directory of Open Access Journals (Sweden)

    Lucian Cuibus

    2014-11-01

    Full Text Available The present work describes a preliminary study to compare some traditional Romanian cheeses and adulterated cheeses using Attenuated Total Reflectance-Fourier transform infrared spectroscopy (ATR-FTIR. For PLS model calibration (6 concentration levels and validation (5 concentration levels sets were prepared from commercial Dalia Cheese from different manufacturers by spiking it with palm oil at concentrations ranging 2-50 % and 5-40 %, respectively. Fifteen Dalia Cheese were evaluated as external set. The spectra of each sample, after homogenization, were acquired in triplicate using a FTIR Shimatsu Prestige 21 Spectrophotometer, with a horizontal diamond ATR accessory in the MIR region 4000-600 cm-1. Statistical methods as PLS were applied using MVC1 routines written for Matlab R2010a. As first step the optimal condition for PLS model were obtained using cross-validation on the Calibration set. Spectral region in 3873-652 cm-1, and 3 PLS-factors were stated as the best conditions and showed an R2 value of 0.9338 and a relative error in the calibration of 17.2%. Then validation set was evaluated, obtaining good recovery rates (108% and acceptable dispersion of the data (20%. The curve of actual vs. predicted values shows slope near to 1 and origin close to 0, with an R2 of 0.9695. When the external sample set was evaluated, samples F19, F21, F22 and F24, showed detectable levels of palm fats. The results proved that FTIR-PLS is a reliable non-destructive technique for a rapid quantification the level of adulteration in cheese.  The spectroscopic methods could assist the quality control authority, traders and the producers to discriminate the adulterated cheeses with palm oil.

  6. FT-IR, NMR SPECTROSCOPIC and QUANTUM MECHANICAL ...

    African Journals Online (AJOL)

    frequencies, potential energy distribution (PED) data, 1H and 13C NMR chemical shifts of Fc- .... Due to electronegative oxygen atom, C11 appears at the highest frequency field region. The most intense singlet appearing at 69.73 ppm arises.

  7. Raman spectroscopy

    Science.gov (United States)

    Raman spectroscopy has gained increased use and importance in recent years for accurate and precise detection of physical and chemical properties of food materials, due to the greater specificity and sensitivity of Raman techniques over other analytical techniques. This book chapter presents Raman s...

  8. Hydrothermal synthesis of porous triphasic hydroxyapatite/(alpha and beta) tricalcium phosphate.

    Science.gov (United States)

    Vani, R; Girija, E K; Elayaraja, K; Prakash Parthiban, S; Kesavamoorthy, R; Narayana Kalkura, S

    2009-12-01

    A novel, porous triphasic calcium phosphate composed of nonresorbable hydroxyapatite (HAp) and resorbable tricalcium phosphate (alpha- and beta-TCP) has been synthesized hydrothermally at a relatively low temperature. The calcium phosphate precursor for hydrothermal treatment was prepared by gel method in the presence of ascorbic acid. XRD, FT-IR, Raman analyses confirmed the presence of HAp/TCP. The surface area and average pore size of the samples were found to be 28 m2/g and 20 nm, respectively. The samples were found to be bioactive in simulated body fluid (SBF).

  9. Raman spectroscopic study of ancient South African domestic clay pottery

    Science.gov (United States)

    Legodi, M. A.; de Waal, D.

    2007-01-01

    The technique of Raman spectroscopy was used to examine the composition of ancient African domestic clay pottery of South African origin. One sample from each of four archaeological sites including Rooiwal, Lydenburg, Makahane and Graskop was studied. Normal dispersive Raman spectroscopy was found to be the most effective analytical technique in this study. XRF, XRD and FT-IR spectroscopy were used as complementary techniques. All representative samples contained common features, which were characterised by kaolin (Al 2Si 2O 5(OH) 5), illite (KAl 4(Si 7AlO 20)(OH) 4), feldspar (K- and NaAlSi 3O 8), quartz (α-SiO 2), hematite (α-Fe 2O 3), montmorillonite (Mg 3(Si,Al) 4(OH) 2·4.5H 2O[Mg] 0.35), and calcium silicate (CaSiO 3). Gypsum (CaSO 4·2H 2O) and calcium carbonates (most likely calcite, CaCO 3) were detected by Raman spectroscopy in Lydenburg, Makahane and Graskop shards. Amorphous carbon (with accompanying phosphates) was observed in the Raman spectra of Lydenburg, Rooiwal and Makahane shards, while rutile (TiO 2) appeared only in Makahane shard. The Raman spectra of Lydenburg and Rooiwal shards further showed the presence of anhydrite (CaSO 4). The results showed that South African potters used a mixture of clays as raw materials. The firing temperature for most samples did not exceed 800 °C, which suggests the use of open fire. The reddish brown and grayish black colours were likely due to hematite and amorphous carbon, respectively.

  10. Chemical synthesis of highly stable PVA/PANI films for supercapacitor application

    Energy Technology Data Exchange (ETDEWEB)

    Patil, D.S.; Shaikh, J.S.; Dalavi, D.S.; Kalagi, S.S. [Thin Films Materials laboratory, Department of Physics, Shivaji University, Kolhapur 416004, M.S. (India); Patil, P.S., E-mail: psp_phy@unishivaji.ac.in [Thin Films Materials laboratory, Department of Physics, Shivaji University, Kolhapur 416004, M.S. (India)

    2011-08-15

    Highlights: {yields} Chemical synthesis of PVA/PANI films by spin and dip coating at room temperature. {yields} Thickness dependent supercapacitor behavior of PVA/PANI film. {yields} The synthesized film are highly stable up to 20,000 cycles. - Abstract: Polyvinyl alcohol (PVA)/polyaniline (PANI) thin films were chemically synthesized by adopting two step process: initially a thin layer (200 nm) of PVA was spin coated by using an aqueous PVA solution onto fluorine doped tin oxide (FTO) coated glass substrate, afterwards PANI was chemically polymerized from aniline monomer and dip coated onto the precoated substrate. The thickness of PANI layer was varied from 293 nm to 2367 nm by varying deposition cycles onto the precoated PVA thin film. The resultant PVA/PANI films were characterized for their optical, morphological and electrochemical properties. The FT-IR and Raman spectra revealed characteristic features of the PANI phase. The SEM study showed porous spongy structure. Electrochemical properties were studied by electrochemical impedance measurement and cyclic voltammetry. The electrochemical performance of PVA/PANI thin films was investigated in 1 M H{sub 2}SO{sub 4} aqueous electrolyte. The highest specific capacitance of 571 Fg{sup -1} was observed for the optimized thickness of 880 nm. The film was found to be stable for more than 20,000 cycles. The samples degraded slightly (25% decrement in specific capacitance) for the first 10,000 cycles. The degradation becomes much slower (10.8% decrement in specific capacitance) beyond 10,000 cycles. This dramatic improvement in the electrochemical stability of the PANI samples, without sacrificing specific capacitance was attributed to the optimized PVA layer.

  11. The synthesis of Ag/polypyrrole coaxial nanocables via ion adsorption method using different oxidants

    Science.gov (United States)

    Qiu, Teng; Xie, Huxiao; Zhang, Jiangru; Zahoor, Amad; Li, Xiaoyu

    2011-03-01

    Ag/polypyrrole (PPy) coaxial nanocables (NCs) were synthesized by an ion adsorption method. In this method, the pre-made Ag nanowires (NWs) were dispersed in the aqueous solution of copper acetate (Cu(Ac)2), and the Cu2+ ions adsorbed onto the surface of Ag NWs can oxidize pyrrole monomers to polymerize into uniform PPy sheath outside Ag NWs after the Cu(Ac)2-treated Ag NWs were re-dispersed in the aqueous solution of pyrrole. The morphology of NCs was characterized by transmission electron microscope (TEM) and scanning electron microscope (SEM). The relationship between the thickness of polymer sheath and the concentration of Cu(Ac)2 was established. As Cu(Ac)2 which served as the oxidant can also be replaced by AgNO3 in this synthesis, the differences on the structure of polymer sheath caused by different oxidants were studied by surface-enhanced Raman scattering (SERS), high-resolution transmission electron microscope (HR-TEM), Fourier transform infrared spectroscopy (FT-IR), and X-ray photoelectron spectroscopy (XPS). Comparing with the characterization results of Ag/PPy NCs synthesized using AgNO3 as the oxidant which indicates the random arrangement of PPy chains at the interface between polymer sheath and Ag NWs, PPy chain oxidized by Cu2+ tends to show a relatively ordered conformation at the interface with the pyrrole rings identically taking the plane vertical to the surface of Ag NWs. In addition, although the main part of the polymer sheath was composed of PPy whatever kind of oxidant was used, the sheath of the NCs oxidized by Cu2+ is typical for the existence of Cu(I)-pyrrole coordinate structures with strong Cu(I)-N bond signal shown in XPS characterization.

  12. The synthesis of Ag/polypyrrole coaxial nanocables via ion adsorption method using different oxidants

    International Nuclear Information System (INIS)

    Qiu Teng; Xie Huxiao; Zhang Jiangru; Zahoor, Amad; Li Xiaoyu

    2011-01-01

    Ag/polypyrrole (PPy) coaxial nanocables (NCs) were synthesized by an ion adsorption method. In this method, the pre-made Ag nanowires (NWs) were dispersed in the aqueous solution of copper acetate (Cu(Ac) 2 ), and the Cu 2+ ions adsorbed onto the surface of Ag NWs can oxidize pyrrole monomers to polymerize into uniform PPy sheath outside Ag NWs after the Cu(Ac) 2 -treated Ag NWs were re-dispersed in the aqueous solution of pyrrole. The morphology of NCs was characterized by transmission electron microscope (TEM) and scanning electron microscope (SEM). The relationship between the thickness of polymer sheath and the concentration of Cu(Ac) 2 was established. As Cu(Ac) 2 which served as the oxidant can also be replaced by AgNO 3 in this synthesis, the differences on the structure of polymer sheath caused by different oxidants were studied by surface-enhanced Raman scattering (SERS), high-resolution transmission electron microscope (HR-TEM), Fourier transform infrared spectroscopy (FT-IR), and X-ray photoelectron spectroscopy (XPS). Comparing with the characterization results of Ag/PPy NCs synthesized using AgNO 3 as the oxidant which indicates the random arrangement of PPy chains at the interface between polymer sheath and Ag NWs, PPy chain oxidized by Cu 2+ tends to show a relatively ordered conformation at the interface with the pyrrole rings identically taking the plane vertical to the surface of Ag NWs. In addition, although the main part of the polymer sheath was composed of PPy whatever kind of oxidant was used, the sheath of the NCs oxidized by Cu 2+ is typical for the existence of Cu(I)–pyrrole coordinate structures with strong Cu(I)–N bond signal shown in XPS characterization.

  13. Solvent effect in implicit/explicit model on FT-IR, 1H, 13C and 19F NMR, UV-vis and fluorescence spectra, linear, second- and third-nonlinear optical parameters of 2-(trifluoromethyl)benzoic acid: Experimental and computational study

    Science.gov (United States)

    Avcı, Davut; Altürk, Sümeyye; Tamer, Ömer; Kuşbazoğlu, Mustafa; Atalay, Yusuf

    2017-09-01

    FT-IR, 1H, 13C and 19F NMR, UV-vis and fluorescence spectra for 2-(trifluoromethyl)benzoic acid (2-TFMBA) were recorded. DFT//B3LYP/6-31++G(d,p) calculations were used to determine the optimized molecular geometry, vibrational frequencies, 1H, 13C and 19F GIAO-NMR chemical shifts of 2-TFMBA. The detailed assignments of vibrational frequencies were carried out on the basis of potential energy distribution (PED) by using VEDA program. TD-DFT/B3LYP/6-31++G(d,p) calculations with the PCM (polarizable continuum model) in ethanol and DMSO solvents based on implicit/explicit model and gas phase in the excited state were employed to investigate UV-vis absorption and fluorescence emission wavelengths. The UV-vis and emission spectra were given in ethanol and DMSO solvents, and the major contributions to the electronic transitions were obtained. In addition, the NLO parameters (β, γ and χ(3)) and frontier molecular orbital energies of 2-TFMBA were calculated by using B3LYP/6-31++G(d,p) level. The NLO parameters of 2-TFMBA were compared with that of para-Nitroaniline (pNA) and urea which are the typical NLO materials. The refractive index (n) is calculated by using the Lorentz-Lorenz equation to observe polarization behavior of 2-TFMBA in DMSO and ethanol solvents. In order to investigate intramolecular and hydrogen bonding interactions, NBO calculations were also performed by the same level. To sum up, considering the well-known biological role, photochemical properties of 2-TFMBA were discussed.

  14. Application potential of ATR-FT/IR molecular spectroscopy in animal nutrition: revelation of protein molecular structures of canola meal and presscake, as affected by heat-processing methods, in relationship with their protein digestive behavior and utilization for dairy cattle.

    Science.gov (United States)

    Theodoridou, Katerina; Yu, Peiqiang

    2013-06-12

    Protein quality relies not only on total protein but also on protein inherent structures. The most commonly occurring protein secondary structures (α-helix and β-sheet) may influence protein quality, nutrient utilization, and digestive behavior. The objectives of this study were to reveal the protein molecular structures of canola meal (yellow and brown) and presscake as affected by the heat-processing methods and to investigate the relationship between structure changes and protein rumen degradations kinetics, estimated protein intestinal digestibility, degraded protein balance, and metabolizable protein. Heat-processing conditions resulted in a higher value for α-helix and β-sheet for brown canola presscake compared to brown canola meal. The multivariate molecular spectral analyses (PCA, CLA) showed that there were significant molecular structural differences in the protein amide I and II fingerprint region (ca. 1700-1480 cm(-1)) between the brown canola meal and presscake. The in situ degradation parameters, amide I and II, and α-helix to β-sheet ratio (R_a_β) were positively correlated with the degradable fraction and the degradation rate. Modeling results showed that α-helix was positively correlated with the truly absorbed rumen synthesized microbial protein in the small intestine when using both the Dutch DVE/OEB system and the NRC-2001 model. Concerning the protein profiles, R_a_β was a better predictor for crude protein (79%) and for neutral detergent insoluble crude protein (68%). In conclusion, ATR-FT/IR molecular spectroscopy may be used to rapidly characterize feed structures at the molecular level and also as a potential predictor of feed functionality, digestive behavior, and nutrient utilization of canola feed.

  15. Synthesis and characterization of "1"3C_3-tristearin

    International Nuclear Information System (INIS)

    Wu Hangyu; Lin Lin; Li Lei; Chen Dazhou

    2011-01-01

    A highly efficient synthesis of "1"3C_3 labeled triglycerides of stearic acids from "1"3C_3-glycerol and stearic acids, by immobilized lipase-catalyzed in solvent-free medium was described. The structure of the product were characterized by fourier transform infrared spectrum (FT-IR), nuclear magnetic resonance (NMR), mass spectra (MS). The results showed that triglycerides of stearic acids contained three "1"3C atoms. The isotope abundance of "1"3C_3-tristearin was more than 99% and the yield was 80% of "1"3C_3-tristearin through calculation. Chemical purity (> 98%) was obtained by differential scanning calorimetry (DSC). (authors)

  16. Casein mediated green synthesis and decoration of reduced graphene oxide

    Science.gov (United States)

    Maddinedi, Sireesh Babu; Mandal, Badal Kumar; Vankayala, Raviraj; Kalluru, Poliraju; Tammina, Sai Kumar; Kiran Kumar, H. A.

    This research is mainly focusing on one-step biosynthesis of graphene from graphene oxide and its stabilization using naturally occurring milk protein, casein. The synthesis of casein reduced graphene oxide (CRGO) was completed within 7 h under reflux at 90 °C with the formation of few layered fine graphene nanosheets. UV-Vis, XRD, XPS analysis data revealed the reduction process of the graphene oxide. Results of FT-IR, HPLC and TEM analysis have shown that the ensuing material consists of graphene decorated with casein molecules. Aspartic acid and glutamic acid residue present in casein molecules are responsible for the reduction of graphene oxide.

  17. Microwave-assisted phenytoine synthesis: proposed practical class for undergraduate students

    International Nuclear Information System (INIS)

    Konrath, Eduardo L.; Piedade, Maristela; Eifler-Lima, Vera Lucia

    2012-01-01

    Microwave synthesis is considered a breakthrough in the field of chemistry due to its benefits over conventional heating methods. We describe, for the first time, the total synthesis of phenytoine adapted for a microwave reactor, proposed as an experiment for undergraduate courses. When carried out with microwaves, the synthetic route provided phenytoine in 6 min and 30 s, while for conventional heating the total time was 170 min. The experiment also involves rapid identification of compounds by TLC, 1 H NMR, FT-IR and melting points determination. (author)

  18. Polyethylenimine-assisted seed-mediated synthesis of gold nanoparticles for surface-enhanced Raman scattering studies

    Science.gov (United States)

    Philip, Anish; Ankudze, Bright; Pakkanen, Tuula T.

    2018-06-01

    Large-sized gold nanoparticles (AuNPs) were synthesized with a new polyethylenimine - assisted seed - mediated method for surface-enhanced Raman scattering (SERS) studies. The size and polydispersity of gold nanoparticles are controlled in the growth step with the amounts of polyethylenimine (PEI) and seeds. Influence of three silicon oxide supports having different surface morphologies, namely halloysite (Hal) nanotubes, glass plates and inverse opal films of SiO2, on the performance of gold nanoparticles in Raman scattering of a 4-aminothiophenol (4-ATP) analyte was investigated. Electrostatic interaction between positively charged polyethylenimine-capped AuNPs and negatively charged surfaces of silicon oxide supports was utilized in fabrication of the SERS substrates using deposition and infiltration methods. The Au-photonic crystal of the three SERS substrate groups is the most active one as it showed the highest analytical enhancement factor (AEF) and the lowest detection limit of 1x10-8 M for 4-ATP. Coupling of the optical properties of photonic crystals with the plasmonic properties of AuNPs provided Au-photonic crystals with the high SERS activity. The AuNPs clusters formed both in the photonic crystal and on the glass plate are capable of forming more hot spots as compared to sparsely distributed AuNPs on Hal nanotubes and thereby increasing the SERS enhancement.

  19. Facile synthesis of AgCl/polydopamine/Ag nanoparticles with in-situ laser improving Raman scattering effect

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Yan; Zhang, Wenqi; Wang, Lin; Wang, Feng, E-mail: wangfeng@shnu.edu.cn; Yang, Haifeng

    2017-01-15

    Highlights: • AgCl/PDA/AgNPs (polydopamine (PDA) adlayer covered cubic AgCl core inlaid with Ag nanoparticles (AgNPs)) was fabricated for in-situ SERS detection. • Such SERS substrate shows in-situ laser improving Raman scattering effect due to the generation of more AgNPs. • Enhancement factor could reach 10{sup 7}. • Such SERS substrate shows good reproducibility and long term stability. - Abstract: We reported a simple and fast method to prepare a composite material of polydopamine (PDA) adlayer covered cubic AgCl core, which was inlaid with Ag nanoparticles (NPs), shortly named as AgCl/PDA/AgNPs. The resultant AgCl/PDA/AgNPs could be employed as surface-enhanced Raman scattering (SERS) substrate for in-situ detection and the SERS activity could be further greatly improved due to the production of more AgNPs upon laser irradiation. With 4-mercaptopyridine (4-Mpy) as the probe molecule, the enhancement factor could reach 10{sup 7}. Additionally, such SERS substrate shows good reproducibility with relative standard deviation of 7.32% and long term stability (after storage for 100 days under ambient condition, SERS intensity decay is less than 25%). In-situ elevating SERS activity of AgCl/PDA/AgNPs induced by laser may be beneficial to sensitive analysis in practical fields.

  20. Microwave Assisted Synthesis of Osmium Electrocatalysts for the Oxygen Reduction Reaction in the Absence and Presence of Aqueous Methanol

    Directory of Open Access Journals (Sweden)

    Edgar Borja-Arco

    2011-01-01

    Full Text Available Osmium electrocatalysts for the oxygen reduction reaction (ORR were prepared by microwave irradiation of Os3(CO12 at different experimental conditions. The materials obtained were structurally characterized by FT-IR, micro-Raman spectroscopy and X-ray diffraction. Their chemical compositions were obtained by EDS. The electrocatalytic properties for the oxygen reduction reaction were evaluated by rotating disk electrode measurements in 0.5 mol L-1 H2SO4, in the absence and presence of aqueous methanol. The kinetic parameters, such as Tafel slope, exchange current density, and charge transfer coefficient are reported.

  1. Optical and structural properties of undoped and Mn{sup 2+} doped Ca–Li hydroxyapatite nanopowders using mechanochemical synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Ravindranadh, K. [Department of Physics, Andhra Loyola College, Vijayawada 520008 (India); Department of Physics, Acharya Nagarjuna University, Guntur 522510 (India); Babu, B.; Pushpa Manjari, V.; Thirumala Rao, G. [Department of Physics, Acharya Nagarjuna University, Guntur 522510 (India); Rao, M.C. [Department of Physics, Andhra Loyola College, Vijayawada 520008 (India); Ravikumar, R.V.S.S.N., E-mail: rvssn@yahoo.co.in [Department of Physics, Acharya Nagarjuna University, Guntur 522510 (India)

    2015-03-15

    Undoped and Mn{sup 2+} doped calcium–lithium hydroxyapatite (CLHA) nanopowders were prepared by mechanochemical synthesis. The prepared samples were characterized by powder X-ray diffraction, scanning electron microscope, transmission electron microscope, optical absorption, photoluminescence, electron paramagnetic resonance and FT-IR spectroscopy techniques. From powder XRD pattern, lattice cell parameters and average crystallite sizes were evaluated. The morphologies of prepared samples were analyzed by using SEM and TEM studies. Optical and EPR data confirmed that the doped Mn{sup 2+} enter into the host material as distorted octahedral site. Photoluminescence spectra of undoped and Mn{sup 2+} doped CLHA nanopowders exhibited blue, blue-green emission bands at 425, 443, 468 nm and green, strong orange emission bands at 534, 577 nm respectively under the excitation wavelength of 365 nm. The CIE chromaticity coordinates were also calculated from emission spectra for undoped and Mn{sup 2+} doped CLHA nanopowders. Vibrational bands related to phosphate molecules, P–O–H and hydroxyl ions are observed in FT-IR spectra. - Highlights: • PXRD pattern of prepared undoped and Mn{sup 2+} doped CLHA nanopowders are in nanosize. • Optical and EPR studies reveal site symmetry of Mn{sup 2+} doped CLHA nanopowders are distorted octahedral symmetry. • FT-IR spectra exhibits the various vibrational modes of phosphate ions, P–O–H and water molecules.

  2. Optical and structural properties of undoped and Mn2+ doped Ca–Li hydroxyapatite nanopowders using mechanochemical synthesis

    International Nuclear Information System (INIS)

    Ravindranadh, K.; Babu, B.; Pushpa Manjari, V.; Thirumala Rao, G.; Rao, M.C.; Ravikumar, R.V.S.S.N.

    2015-01-01

    Undoped and Mn 2+ doped calcium–lithium hydroxyapatite (CLHA) nanopowders were prepared by mechanochemical synthesis. The prepared samples were characterized by powder X-ray diffraction, scanning electron microscope, transmission electron microscope, optical absorption, photoluminescence, electron paramagnetic resonance and FT-IR spectroscopy techniques. From powder XRD pattern, lattice cell parameters and average crystallite sizes were evaluated. The morphologies of prepared samples were analyzed by using SEM and TEM studies. Optical and EPR data confirmed that the doped Mn 2+ enter into the host material as distorted octahedral site. Photoluminescence spectra of undoped and Mn 2+ doped CLHA nanopowders exhibited blue, blue-green emission bands at 425, 443, 468 nm and green, strong orange emission bands at 534, 577 nm respectively under the excitation wavelength of 365 nm. The CIE chromaticity coordinates were also calculated from emission spectra for undoped and Mn 2+ doped CLHA nanopowders. Vibrational bands related to phosphate molecules, P–O–H and hydroxyl ions are observed in FT-IR spectra. - Highlights: • PXRD pattern of prepared undoped and Mn 2+ doped CLHA nanopowders are in nanosize. • Optical and EPR studies reveal site symmetry of Mn 2+ doped CLHA nanopowders are distorted octahedral symmetry. • FT-IR spectra exhibits the various vibrational modes of phosphate ions, P–O–H and water molecules

  3. Raman facility

    Data.gov (United States)

    Federal Laboratory Consortium — Raman scattering is a powerful light scattering technique used to diagnose the internal structure of molecules and crystals. In a light scattering experiment, light...

  4. Novel and facile microwave-assisted synthesis of Mo-doped hydroxyapatite nanorods: Characterization, gamma absorption coefficient, and bioactivity.

    Science.gov (United States)

    Abutalib, M M; Yahia, I S

    2017-09-01

    In the current work, the authors report the microwave-assisted synthesis Molybdenum-doped (from 0.05 to 5wt%) hydroxyapatite (HAp) for the first time. The morphology of Mo-doped HAp is nanorods of diameter in the range of 25-70nm and length in the range of 25nm to 200nm. The good crystalline nature was confirmed from X-ray diffraction patterns and also lattice parameters, grain size, strain and dislocation density were determined. The crystallite size was found to be in the range 16 to 30nm and crystallinity was found to be enhanced from 0.5 to 0.7 with doping. The field emission SEM micrographs show that the morphology of the synthesized nanostructures of pure and Mo-doped HAp are nanorods of few nanometers. The vibrational modes were identified using the FT-Raman and FT-IR spectroscopy. The dielectric properties were studied and the AC electrical conductivity was found to be increased with increasing the concentration of Mo ions doping in HAp. Moreover, antimicrobial studies were also carried out to understand the anti-bacterial and anti-fungi properties. The results suggest that it may be a good bio-ceramics material for bio-medical applications. Mo-doped HAp was subjected to the gamma irradiation produced from Cs-137 (662keV) and its related parameters such as linear absorption coefficient, the half-value layer (HVL) and the tenth value layer TVL were calculated and analyzed. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Facile synthesis of gold-capped TiO2 nanocomposites for surface-enhanced Raman scattering

    International Nuclear Information System (INIS)

    Han, Di; Huang, Hao; Du, Deyang; Lang, Xianzhong; Long, Kailin; Hao, Qi; Qiu, Teng

    2015-01-01

    A convenient technique was developed to fabricate gold-capped TiO 2 nanocomposites as robust, cost-efficient and recyclable surface-enhanced Raman scattering (SERS) substrates. The morphologies of obtained nanocomposites exhibit nanotube, nanolace, and nanopore nanostructures by adjusting TiO 2 anodization parameters. As an illustration, dramatic enhancement is achieved using Rhodamine 6G as a molecular probe. Owing to activation by the incident laser beam, the localized electromagnetic field on the nanocomposite surface can be enhanced subsequently amplifying the Raman signal. The topography can be further tuned to optimize the enhancement factor by adjusting the time of gold evaporation. Finite-difference time-domain calculations indicate the nanopore structure may possess excellent SERS characteristic due to the high density of hot spots. In addition, the substrate can be self-cleaned under ultraviolet irradiation due to the superior photocatalytic capacity of the Au–TiO 2 nanocomposites. Our Au–TiO 2 nanocomposites with highly SERS-active properties and recyclability shows promising applications in the detection and treatment of pollutants. - Highlights: • Au–TiO 2 nanocomposites with different morphologies were fabricated. • Au–TiO 2 nanopore shows pronounced SERS compared with nanotube and nanolace. • The size of the gold nanocaps on Au–TiO 2 nanopore was tailored to optimize the SERS. • FDTD simulations indicate excellent SERS attributes to the high density of hot spots. • Au–TiO 2 nanocomposites prove to be recyclable substrates for SERS detection

  6. Synthesis of silver/silver chloride/graphene oxide composite and its surface-enhanced Raman scattering activity and self-cleaning property

    Science.gov (United States)

    Zhao, Nan; Fei, Xiao; Cheng, Xiaonong; Yang, Juan

    2017-09-01

    Recently, silver nanoparticles decorated with graphene and graphene oxide (GO) sheets can be employed as surface-enhanced Raman scattering (SERS) substrates. However, their SERS activity on macromolecular compound detection is all one-time process. In order to solve this issue and decrease the cost of routine SERS detection, silver/silver chloride (Ag/AgCl) with photocatalytic activity under visible light was introduced. In this study, a novel, simple and clean approach is carried out for synthesis of the Ag/AgCl/GO composite. The Ag/AgCl colloidal solution is obtained by hydrothermal method and then mixed with GO solution to obtain the Ag/AgCl/GO composite using a facile electrostatic self-assembly method. Results showed that the Ag/AgCl/GO composite has the optimized SERS activity to Rhodamine 6G molecules with the maximum enhancement factor value of 3.8×107. Furthermore, the Ag/AgCl particles with high efficient and stable photocatalytic activity under visible light lead to an outstanding self-cleaning property of the Ag/AgCl/GO composite.

  7. Facile Synthesis of Micron-Sized Hollow Silver Spheres as Substrates for Surface-Enhanced Raman Scattering

    Directory of Open Access Journals (Sweden)

    Lixin Xia

    2014-01-01

    Full Text Available A well-designed type of micron-sized hollow silver sphere was successfully synthesized by a simple hard-template method to be used as substrates for surface-enhanced Raman scattering. 4 Å molecular sieves were employed as a removable solid template. [Ag(NH32]+ was absorbed as the precursor on the surface of the molecular sieve. Formaldehyde was selected as a reducing agent to reduce [Ag(NH32]+, resulting in the formation of a micron-sized silver shell on the surface of the 4 Å molecular sieves. The micron-sized hollow silver spheres were obtained by removing the molecular sieve template. SEM and XRD were used to characterize the structure of the micron-sized hollow silver spheres. The as-prepared micro-silver spheres exhibited robust SERS activity in the presence of adsorbed 4-mercaptobenzoic acid (4-MBA with excitation at 632.8 nm, and the enhancement factor reached ~1.5 × 106. This synthetic process represents a promising method for preparing various hollow metal nanoparticles.

  8. Ag Nanorods-Oxide Hybrid Array Substrates: Synthesis, Characterization, and Applications in Surface-Enhanced Raman Scattering

    Directory of Open Access Journals (Sweden)

    Lingwei Ma

    2017-08-01

    Full Text Available Over the last few decades, benefitting from the sufficient sensitivity, high specificity, nondestructive, and rapid detection capability of the surface-enhanced Raman scattering (SERS technique, numerous nanostructures have been elaborately designed and successfully synthesized as high-performance SERS substrates, which have been extensively exploited for the identification of chemical and biological analytes. Among these, Ag nanorods coated with thin metal oxide layers (AgNRs-oxide hybrid array substrates featuring many outstanding advantages have been proposed as fascinating SERS substrates, and are of particular research interest. The present review provides a systematic overview towards the representative achievements of AgNRs-oxide hybrid array substrates for SERS applications from diverse perspectives, so as to promote the realization of real-world SERS sensors. First, various fabrication approaches of AgNRs-oxide nanostructures are introduced, which are followed by a discussion on the novel merits of AgNRs-oxide arrays, such as superior SERS sensitivity and reproducibility, high thermal stability, long-term activity in air, corrosion resistivity, and intense chemisorption of target molecules. Next, we present recent advances of AgNRs-oxide substrates in terms of practical applications. Intriguingly, the recyclability, qualitative and quantitative analyses, as well as vapor-phase molecule sensing have been achieved on these nanocomposites. We further discuss the major challenges and prospects of AgNRs-oxide substrates for future SERS developments, aiming to expand the versatility of SERS technique.

  9. Large-scale, rapid synthesis and application in surface-enhanced Raman spectroscopy of sub-micrometer polyhedral gold nanocrystals

    International Nuclear Information System (INIS)

    Guo Shaojun; Wang Yuling; Wang Erkang

    2007-01-01

    Macromolecule-protected sub-micrometer polyhedral gold nanocrystals have been facilely prepared by heating an aqueous solution containing poly (N-vinyl-2-pyrrolidone) (PVP) and HAuCl 4 without adding other reducing agents. Scanning electron microscopy (SEM), energy-dispersive x-ray spectroscopy (EDX), ultraviolet-visible-near-infrared spectroscopy (UV-vis-NIR), and x-ray diffraction (XRD) were employed to characterize the obtained polyhedral gold nanocrystals. It is found that the 10:1 molar ratio of PVP to gold is a key factor for obtaining quasi-monodisperse polyhedral gold nanocrystals. Furthermore, the application of polyhedral gold nanocrystals in surface-enhanced Raman scattering (SERS) was investigated by using 4-aminothiophenol (4-ATP) as a probe molecule. The results indicated that the sub-micrometer polyhedral gold nanocrystals modified on the ITO substrate exhibited higher SERS activity compared to the traditional gold nanoparticle modified film. The enhancement factor (EF) on polyhedral gold nanocrystals was about six times larger than that obtained on aggregated gold nanoparticles (∼25 nm)

  10. Synthesis and characterization of arsenic-doped cysteine-capped thoria-based nanoparticles

    International Nuclear Information System (INIS)

    Pereira, F. J.; Díez, M. T.; Aller, A. J.

    2013-01-01

    Thoria materials have been largely used in the nuclear industry. Nonetheless, fluorescent thoria-based nanoparticles provide additional properties to be applied in other fields. Thoria-based nanoparticles, with and without arsenic and cysteine, were prepared in 1,2-ethanediol aqueous solutions by a simple precipitation procedure. The synthesized thoria-based nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (ED-XRS), Raman spectroscopy, Fourier transform infrared (FT-IR) spectroscopy and fluorescence microscopy. The presence of arsenic and cysteine, as well as the use of a thermal treatment facilitated fluorescence emission of the thoria-based nanoparticles. Arsenic-doped and cysteine-capped thoria-based nanoparticles prepared in 2.5 M 1,2-ethanediol solutions and treated at 348 K showed small crystallite sizes and strong fluorescence. However, thoria nanoparticles subjected to a thermal treatment at 873 K also produced strong fluorescence with a very narrow size distribution and much smaller crystallite sizes, 5 nm being the average size as shown by XRD and TEM. The XRD data indicated that, even after doping of arsenic in the crystal lattice of ThO 2 , the samples treated at 873 K were phase pure with the fluorite cubic structure. The Raman and FT-IR spectra shown the most characteristics vibrational peaks of cysteine together with other peaks related to the bonds of this molecule to thoria and arsenic when present

  11. FT-Raman and FT-Infrared investigations of archaeological artefacts from Foeni Neolithic site (Banat, Romania

    Directory of Open Access Journals (Sweden)

    Simona Cîntă Pînzaru

    2008-08-01

    Full Text Available An impressive collection of chert artefacts from the Foeni Neolithic archaeological site (Timiş County, Banat region, Romania is hosted by the Banat Museum in Timişoara. A representative set of seven specimens was non-destructively investigated using FT-Raman and ATR-FT-IR spectroscopy. The research was carried out for checking if these readily-available, non-destructive, fast, and cheap methods, which do not require preliminary sample preparation could provide significant information for characterizing the mineral composition of chert artefacts. Based on vibrational data, it was confirmed that the raw material was represented by microcrystalline quartz and moganite, with local concentrations of accessory minerals (calcite, dolomite, and clay minerals. In spite of their wide macroscopic heterogeneity (colour, transparency, based on single point FT-Raman measurements the chert artefacts could not be assigned to distinctive groups of raw silica materials, in order to provide specific arguments for provenance studies. However, the presence of specific accessory minerals (dolomite, illite pointed to distinctive genetic conditions in the case of one lithic material. Sets of measurements (mapping are required for statistically characterizing each artefact specimen. IR data were less significant, due to the rough surface texture of the specimens in contact with the ZnSe crystal of the ATR-FT-IR module. However, illite was identified based solely on its contribution to the IR spectrum. This pioneering study on chert artefacts from Romania based on optical spectroscopic methods shows that there are good premises for a systematic investigation of highly-valuable museum collections, in particular in terms of chert geology.

  12. Green synthesis of silver nanoparticles using tannins

    Science.gov (United States)

    Raja, Pandian Bothi; Rahim, Afidah Abdul; Qureshi, Ahmad Kaleem; Awang, Khalijah

    2014-09-01

    Colloidal silver nanoparticles were prepared by rapid green synthesis using different tannin sources as reducing agent viz. chestnut (CN), mangrove (MG) and quebracho (QB). The aqueous silver ions when exposed to CN, MG and QB tannins were reduced which resulted in formation of silver nanoparticles. The resultant silver nanoparticles were characterized using UV-Visible, X-ray diffraction (XRD), scanning electron microscopy (SEM/EDX), and transmission electron microscopy (TEM) techniques. Furthermore, the possible mechanism of nanoparticles synthesis was also derived using FT-IR analysis. Spectroscopy analysis revealed that the synthesized nanoparticles were within 30 to 75 nm in size, while XRD results showed that nanoparticles formed were crystalline with face centered cubic geometry.

  13. Microwave-assisted synthesis of Mn{sub 3}O{sub 4} nanoparticles@reduced graphene oxide nanocomposites for high performance supercapacitors

    Energy Technology Data Exchange (ETDEWEB)

    She, Xiao; Zhang, Xinmin; Liu, Jingya [School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan 430073 (China); Li, Liang, E-mail: msell08@163.com [School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan 430073 (China); Yu, Xianghua; Huang, Zhiliang [School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan 430073 (China); Shang, Songmin, E-mail: shang.songmin@polyu.edu.hk [Institute of Textiles and Clothing, The Hong Kong Polytechnic University, Hong Kong (China)

    2015-10-15

    Highlights: • Mn{sub 3}O{sub 4}@rGO nanocomposites were prepared by one-step microwave-assisted method. • The growth of Mn{sub 3}O{sub 4} and the reduction of graphene oxide occurred simultaneously. • Specific capacitance of the nanocomposite is higher than those of rGO and Mn{sub 3}O{sub 4}. • The nanocomposites have good rate capability and cycling stability. - ABSTRACT: One-step microwave-assisted synthetic route for the fabrication of Mn{sub 3}O{sub 4} nanoparticles@reduced graphene oxide (Mn{sub 3}O{sub 4}@rGO) nanocomposites has been demonstrated. The morphological structures of the nanocomposites are characterized by Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, X-ray diffraction (XRD), thermogravimetric analyses (TGA), and scanning electron microscopy (SEM), respectively. All of the results indicate that the microwave-assisted synthesis results in the growth of Mn{sub 3}O{sub 4} and the reduction of graphene oxide simultaneously in ethylene glycol-water system. The specific capacitance of the as-prepared Mn{sub 3}O{sub 4}@rGO nanocomposite is higher than those of rGO and pure Mn{sub 3}O{sub 4}, which indicates the synergetic interaction between rGO and Mn{sub 3}O{sub 4}. The nanocomposites also have good rate capability and cycling stability in electrochemical experiments. This facile technique may be extended to the large scale and cost effective production of other composites based on graphene and metal oxide for many applications.

  14. Synthesis and application of bismuth ferrite nanosheets supported functionalized carbon nanofiber for enhanced electrochemical detection of toxic organic compound in water samples.

    Science.gov (United States)

    Ramaraj, Sukanya; Mani, Sakthivel; Chen, Shen-Ming; Kokulnathan, Thangavelu; Lou, Bih-Show; Ali, M Ajmal; Hatamleh, A A; Al-Hemaid, Fahad M A

    2018-03-15

    Recently, the multiferroic material has fabulous attention in numerous applications owing to its excellent electronic conductivity, unique mechanical property, and higher electrocatalytic activity, etc. In this paper, we reported that the synthesis of bismuth ferrite (BiFeO 3 ) nanosheets integrated functionalized carbon nanofiber (BiFeO 3 NS/F-CNF) nanocomposite using a simple hydrothermal technique. Herein, the structural changes and crystalline property of prepared BiFeO 3 NS/F-CNF nanocomposite were characterized using Scanning electron microscopy (SEM), Transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). From this detailed structural evolution, the formation of nanosheets like BiFeO 3 and its nanocomposite with F-CNF were scrutinized and reported. Furthermore, the as-prepared BiFeO 3 NS/F-CNF nanocomposite modified glassy carbon electrode (GCE) was applied for electrochemical detection of catechol (CC). As expected, BiFeO 3 NS/F-CNF/GCE shows excellent electrocatalytic activity as well as 3.44 (F-CNF/GCE) and 7.92 (BiFeO 3 NS/GCE) fold higher electrochemical redox response for CC sensing. Moreover, the proposed sensor displays a wide linear range from 0.003 to 78.02 µM with a very low detection limit of 0.0015 µM. In addition, we have validated the real-time application of our developed CC sensor in different water samples. Copyright © 2017 Elsevier Inc. All rights reserved.

  15. Experimental and theoretical studies on IR, Raman, and UV-Vis spectra of quinoline-7-carboxaldehyde.

    Science.gov (United States)

    Kumru, M; Küçük, V; Kocademir, M; Alfanda, H M; Altun, A; Sarı, L

    2015-01-05

    Spectroscopic properties of quinoline-7-carboxaldehyde (Q7C) have been studied in detail both experimentally and theoretically. The FT-IR (4000-50 cm(-1)), FT-Raman (4000-50 cm(-1)), dispersive-Raman (3500-50 cm(-1)), and UV-Vis (200-400 nm) spectra of Q7C were recorded at room temperature (25 °C). Geometry parameters, potential energy surface about CCH(O) bond, harmonic vibrational frequencies, IR and Raman intensities, UV-Vis spectrum, and thermodynamic characteristics (at 298.15K) of Q7C were computed at Hartree-Fock (HF) and density functional B3LYP levels employing the 6-311++G(d,p) basis set. Frontier molecular orbitals, molecular electrostatic potential, and Mulliken charge analyses of Q7C have also been performed. Q7C has two stable conformers that are energetically very close to each other with slight preference to the conformer that has oxygen atom of the aldehyde away from the nitrogen atom of the quinoline. Copyright © 2014 Elsevier B.V. All rights reserved.

  16. One-pot multi-component green synthesis of highly substituted piperidines

    Directory of Open Access Journals (Sweden)

    Ravi Bansal

    2017-05-01

    Full Text Available An effective and expeditious method of the synthesis of a highly functionalized piperidines, catalyzed by nontoxic, recyclable and environment friendly sodium lauryl sulfate (SLS, via one-pot multi-component condensation of aldehydes, amines and β-ketoesters in water at room temperature, has been developed. This new protocol has advantages such as moderate to high yields of products obtained after simple post reaction workup. Structure of the synthesized compounds 4a–4j have been elucidated based on the 1H NMR, 13C NMR, FT-IR spectroscopy and elemental analysis.

  17. Biological evaluation and simple method for the synthesis of tetrahydrobenzo[a]xanthenes-11-one derivatives

    Directory of Open Access Journals (Sweden)

    Ali Akbari

    2017-01-01

    Full Text Available A simple method for the synthesis of Tetrahydrobenzo[a]xanthenes-11-one derivatives in the presence of BF3.SiO2, and its antibacterial activity was assessed against Pseudomonas syringae, Xanthomonas citi and Pectobacterium carotovorum. The structure of the isolated compounds has been determined by means of 1H/13C NMR and FT-IR spectroscopy. The reactions were carried out in water at room temperature for 5 h. This method has some advantages such as good to excellent yield, mild reaction condition, ease of operation and workup, high product purity and green process.

  18. Microwave Synthesis and Characterization of Waste Soybean Oil-Based Gemini Imidazolinium Surfactants with Carbonate Linkage

    Science.gov (United States)

    Tripathy, Divya Bajpai; Mishra, Anuradha

    Gemini surfactants are presently gaining attention due to their unusual self-assembling characteristics and incomparable interfacial activity. Current research work involves the cost-effective microwave (MW) synthesis of waste soybean oil-based gemini imidazolinium surfactants (GIS) having a carbonate linkage in its spacer moiety. Structural characterizations of the materials have been done using FT-IR, 1H-NMR and 13C-NMR. Using indigenous and natural material as base and MW as energy source for synthesizing the GIS with easily degradable chemical moiety make them to be labeled as green surfactants.

  19. Microwave-assisted phenytoine synthesis: proposed practical class for undergraduate students; Sintese da fenitoina assistida por micro-ondas: proposta de aula pratica para alunos de graduacao

    Energy Technology Data Exchange (ETDEWEB)

    Konrath, Eduardo L; Piedade, Maristela; Eifler-Lima, Vera Lucia, E-mail: edukonrath@yahoo.com.br [Universidade Federal do Rio Grande do Sul (UFRGS), Porto Alegre, RS (Brazil). Fac. de Farmacia. Dept. de Producao de Materia-Prima

    2012-07-01

    Microwave synthesis is considered a breakthrough in the field of chemistry due to its benefits over conventional heating methods. We describe, for the first time, the total synthesis of phenytoine adapted for a microwave reactor, proposed as an experiment for undergraduate courses. When carried out with microwaves, the synthetic route provided phenytoine in 6 min and 30 s, while for conventional heating the total time was 170 min. The experiment also involves rapid identification of compounds by TLC, {sup 1}H NMR, FT-IR and melting points determination. (author)

  20. Facile synthesis of terminal-alkyne bioorthogonal molecules for live -cell surface-enhanced Raman scattering imaging through Au-core and silver/dopamine-shell nanotags.

    Science.gov (United States)

    Chen, Meng; Zhang, Ling; Yang, Bo; Gao, Mingxia; Zhang, Xiangmin

    2018-03-01

    Alkyne is unique, specific and biocompatible in the Raman-silent region of the cell, but there still remains a challenge to achieve ultrasensitive detection in living systems due to its weak Raman scattering. Herein, a terminal alkyne ((E)-2-[4-(ethynylbenzylidene)amino]ethane-1-thiol (EBAE)) with surface-enhanced Raman scattering is synthesized. The EBAE molecule possesses S- and C-termini, which can be directly bonded to gold nanoparticles and dopamine/silver by forming the Au-S chemical bond and the carbon-metal bond, respectively. The distance between Raman reporter and AuNPs/AgNPs can be reduced, contributing to forming hot-spot-based SERS substrate. The alkyne functionalized nanoparticles are based on Au core and encapsulating polydopamine shell, defined as Au-core and dopamine/Ag-shell (ACDS). The bimetallic ACDS induce strong SERS signals for molecular imaging that arise from the strong electromagnetic field. Furthermore, the EBAE provides a distinct peak in the cellular Raman-silent region with nearly zero background interference. The EBAE Raman signals could be tremendously enhanced when the Raman reporter is located at the middle of the Au-core and dopamine/Ag-shell. Therefore, this work could have huge potential benefits for the highly sensitive detection of intercellular information delivery by connecting the recognition molecules in biomedical diagnostics. Graphical abstract Terminal-alkyne-functionalized Au-core and silver/dopamine-shell nanotags for live-cell surface-enhanced Raman scattering imaging.

  1. Green Synthesis and Characterization of Palladium Nanoparticles Using Origanum vulgare L. Extract and Their Catalytic Activity

    Directory of Open Access Journals (Sweden)

    Mohammed Rafi Shaik

    2017-01-01

    Full Text Available The synthesis of Palladium (Pd nanoparticles by green methods has attracted remarkable attention in recent years because of its superiority above chemical approaches, owing to its low cost and ecological compatibility. In this present work, we describe a facile and environmentally friendly synthesis of Pd nanoparticles (Pd NPs using an aqueous extract of aerial parts of Origanum vulgare L. (OV as a bioreductant. This plant is available in many parts of the world as well as in Saudi Arabia and is known to be a rich source of phenolic components, a feature we fruitfully utilized in the synthesis of Pd NPs, using various concentrations of plant extracts. Moreover, the OV extract phytomolecules are not only accountable for the reduction and progression of nanoparticles, but they also act as stabilizing agents, which was confirmed by several characterization methods. The as-synthesized Pd nanoparticles (Pd NPs were analyzed using ultraviolet-visible spectroscopy (UV-Vis, Fourier-transform infrared spectroscopy (FT-IR, X-ray diffraction (XRD, transmission electron microscopy (TEM, energy-dispersive X-ray spectroscopy (EDX, and thermal gravimetric analysis (TGA. Further, FT-IR study has proven that the OV not merely represents a bioreductant but also functionalizes the nanoparticles. Furthermore, the green synthesized metallic Pd NPs were successfully applied as catalysts for selective oxidation of alcohols.

  2. Effect of concentration of imperata cylindrica L leaf extraction synthesis process of gold nanoparticles

    International Nuclear Information System (INIS)

    Iwan Syahjoko Saputra; Yoki Yulizar; Sudirman

    2018-01-01

    Gold Nanoparticles (Gold NPs) successful was performed using HAuCl 4 precursor as Au 3+ ion source with 7 x 10 -4 M concentration. There search aims to knows effect of concentration variation of Imperata cylindrica L leaf extract on synthesis process of gold nanoparticles. There search used of green synthesis method. Colloid of nanoparticles which is formed in analyzed using UV - Vis Spectrophotometer, FT-IR Spectroscopy, PSA, PZC, XRD and TEM. The results of synthesis showed the best concentration of Imperata cilyndrica L leaf extract at 3.46 %, happen a shift of wave length at UV-Vis from 216 nm to 530 nm with 1.779 absorbance value. The PSA analysis showed a particle size of 51.87 nm and a PZC value of -19.2 mV. The result of FT - IR indicated a shift of wave number in the hydroxyl group from 3354 cm -1 to 3390 cm -1 and showed a interaction of hydroxyl group at imperata cylindrica L leaf extract with Au 3+ ion. TEM analysis shows the morphology of Gold NPs that spherical shape with a particle size of 20 nm. XRD calculation results show crystallite size of gold nano particles is 15.47 nm. (author)

  3. CV Raman

    Indian Academy of Sciences (India)

    formatted to take advantage of the changes in publishing methods in the past thirty ..... This work would not have been possible without the support and en- couragement of ..... in which Raman made his decision, have a deeper significance than .... Light in Water and the Colour of the Sea within a month of his return to India ...

  4. Raman Chandrasekar

    Indian Academy of Sciences (India)

    Home; Journals; Resonance – Journal of Science Education. Raman Chandrasekar. Articles written in Resonance – Journal of Science Education. Volume 13 Issue 5 May 2008 pp 430-439 General Article. How Children Learn to Use Language - An Overview of R. Narasimhan's Ideas on Child Language Acquisition.

  5. Facile preparation of water dispersible polypyrrole nanotube-supported silver nanoparticles for hydrogen peroxide reduction and surface-enhanced Raman scattering

    International Nuclear Information System (INIS)

    Peng Yingjing; Qiu Lihua; Pan Congtao; Wang Cancan; Shang Songmin; Yan Feng

    2012-01-01

    Water dispersible polypyrrole nanotube/silver nanoparticle hybrids (PPyNT-COOAgNP) were synthesized via a cation-exchange method. The approach involves the surface functionalization of PPyNTs with carboxylic acid groups (-COOH), and cation-exchange with silver ions (Ag + ) and followed by the reduction of metal ions. The morphology and optical properties of the produced PPyNT-COOAgNP nanohybrids were characterized by transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectrometer, and UV–vis spectroscopy. The as-prepared PPyNT-COOAgNP nanohybrids exhibited well-defined response to the reduction of hydrogen peroxide, and as extremely suitable substrates for surface-enhanced Raman spectroscopy (SERS) with a high enhancement factor of 6.0 × 10 7 , and enabling the detection of 10 −12 M Rhodamine 6G solution.

  6. Raman and infrared spectroscopy of carbohydrates: A review

    Science.gov (United States)

    Wiercigroch, Ewelina; Szafraniec, Ewelina; Czamara, Krzysztof; Pacia, Marta Z.; Majzner, Katarzyna; Kochan, Kamila; Kaczor, Agnieszka; Baranska, Malgorzata; Malek, Kamilla

    2017-10-01

    Carbohydrates are widespread and naturally occurring compounds, and essential constituents for living organisms. They are quite often reported when biological systems are studied and their role is discussed. However surprisingly, up till now there is no database collecting vibrational spectra of carbohydrates and their assignment, as has been done already for other biomolecules. So, this paper serves as a comprehensive review, where for selected 14 carbohydrates in the solid state both FT-Raman and ATR FT-IR spectra were collected and assigned. Carbohydrates can be divided into four chemical groups and in the same way is organized this review. First, the smallest molecules are discussed, i.e. monosaccharides (D-(-)-ribose, 2-deoxy-D-ribose, L-(-)-arabinose, D-(+)-xylose, D-(+)-glucose, D-(+)-galactose and D-(-)-fructose) and disaccharides (D-(+)-sucrose, D-(+)-maltose and D-(+)-lactose), and then more complex ones, i.e. trisaccharides (D-(+)-raffinose) and polysaccharides (amylopectin, amylose, glycogen). Both Raman and IR spectra were collected in the whole spectral range and discussed looking at the specific regions, i.e. region V (3600-3050 cm- 1), IV (3050-2800 cm- 1) and II (1200-800 cm- 1) assigned to the stretching vibrations of the OH, CH/CH2 and C-O/C-C groups, respectively, and region III (1500-1200 cm- 1) and I (800-100 cm- 1) dominated by deformational modes of the CH/CH2 and CCO groups, respectively. In spite of the fact that vibrational spectra of saccharides are significantly less specific than spectra of other biomolecules (e.g. lipids or proteins), marker bands of the studied molecules can be identified and correlated with their structure.

  7. Synthesis of adenine-modified reduced graphene oxide nanosheets.

    Science.gov (United States)

    Cao, Huaqiang; Wu, Xiaoming; Yin, Gui; Warner, Jamie H

    2012-03-05

    We report here a facile strategy to synthesize the nanocomposite of adenine-modified reduced graphene oxide (AMG) via reaction between adenine and GOCl which is generated from SOCl(2) reacted with graphite oxide (GO). The as-synthesized AMG was characterized by transmission electron microscopy (TEM), atomic force microscopy (AFM), UV-vis absorption spectroscopy, Fourier transform infrared (FT-IR) spectroscopy, Raman spectroscopy, thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV), and galvanostatic discharge analysis. The AMG owns about one adenine group per 53 carbon atoms on a graphene sheet, which improves electronic conductivity compared with reduced graphene oxide (RGO). The AMG displays enhanced supercapacitor performance compared with RGO accompanying good stability and good cycling behavior in the supercapacitor.

  8. Magnesium Borate Synthesis by Microwave Energy: A New Method

    Directory of Open Access Journals (Sweden)

    Azmi Seyhun Kipcak

    2013-01-01

    Full Text Available Magnesium borates are one of the major groups of boron minerals that have important properties such as high heat and corrosion resistances and high coefficients of elasticity. In this study, magnesium borate minerals are synthesized using boric acid and magnesium oxide with a new method of microwave, and the synthesized minerals are characterized by various analysis techniques. The results show that pure, “magnesium borate hydrate” minerals are obtained at the end of various steps. The characterization of the products is determined with the techniques of X-Ray Diffraction (XRD, Fourier Transform Infrared Spectroscopy (FT-IR, Raman Spectroscopy, and Scanning Electron Microscopy (SEM. Additionally, overall “magnesium borate hydrate” yields are calculated and found about 67% at 270 W, 8 minutes and 360 W, 3 minutes of reaction times, respectively.

  9. Synthesis and characterization of a new porphyrin-polyoxometalate hybrid material and investigation of its catalytic activity.

    Science.gov (United States)

    Araghi, Mehdi; Mirkhani, Valiollah; Moghadam, Majid; Tangestaninejad, Shahram; Mohammdpoor-Baltork, Iraj

    2012-03-14

    In the present work, the preparation of a new organic-inorganic hybrid material in which tetrakis(p-aminophenylporphyrin) is covalently linked to a Lindqvist structure of polyoxometalate, is reported. This new porphyrin-polyoxometalate hybrid material was characterized by (1)H NMR, FT-IR and UV-Vis spectroscopic methods and cyclic voltammetry. These spectro- and electrochemical studies provided spectral data of the synthesis of this compound. Cyclic voltammetry showed the influence of the porphyrin on the redox process of the polyoxometalate. The catalytic activity of this hybrid material was investigated in the alkene epoxidation with NaIO(4).

  10. Synthesis, characterization, photophysical, and photochemical properties of novel zinc(II) and indium(III) phthalocyanines containing 2-phenylphenoxy units

    International Nuclear Information System (INIS)

    Ali, Haytham Elzien Alamin; Pişkin, Mehmet; Altun, Selçuk; Durmuş, Mahmut; Odabaş, Zafer

    2016-01-01

    The synthesis of highly soluble and non-aggregated peripherally/non-peripherally Zn and In(OAc) phthalocyanines was achieved by 3-/ and 4-(2-phenylphenoxy)phthalonitrile as starting materials. The novel compounds were characterized by elemental analyses, FT-IR, 1 H-NMR (for phthalonitriles), UV–vis and MALDI-TOF mass (for Pcs) spectroscopic techniques. Additionally, photophysical, photochemical and spectral properties of the phthalocyanines were reported. Especially, the indium(OAc) phthalocyanines showed good singlet oxygen quantum yields in DMSO and they can be appropriate candidates as Type II photosensitizers in photodynamic therapy (PDT) applications.

  11. Synthesis, characterization, photophysical, and photochemical properties of novel zinc(II) and indium(III) phthalocyanines containing 2-phenylphenoxy units

    Energy Technology Data Exchange (ETDEWEB)

    Ali, Haytham Elzien Alamin [Department of Chemistry, Marmara University, Istanbul 34722 (Turkey); University of Khartoum, Department of Chemistry, Faculty of Science, P.O. Box 321, Khartoum, 11115 (Sudan); Pişkin, Mehmet [Çanakkale Onsekiz Mart University, Vocational School of Technical Sciences, Department of Food Technology, Çanakkale 17100 (Turkey); Altun, Selçuk [Department of Chemistry, Marmara University, Istanbul 34722 (Turkey); Durmuş, Mahmut [Gebze Technical University, Department of Chemistry, P.O. Box 141, Gebze, Kocaeli 41400 (Turkey); Odabaş, Zafer, E-mail: zodabas@marmara.edu.tr [Department of Chemistry, Marmara University, Istanbul 34722 (Turkey)

    2016-05-15

    The synthesis of highly soluble and non-aggregated peripherally/non-peripherally Zn and In(OAc) phthalocyanines was achieved by 3-/ and 4-(2-phenylphenoxy)phthalonitrile as starting materials. The novel compounds were characterized by elemental analyses, FT-IR, {sup 1}H-NMR (for phthalonitriles), UV–vis and MALDI-TOF mass (for Pcs) spectroscopic techniques. Additionally, photophysical, photochemical and spectral properties of the phthalocyanines were reported. Especially, the indium(OAc) phthalocyanines showed good singlet oxygen quantum yields in DMSO and they can be appropriate candidates as Type II photosensitizers in photodynamic therapy (PDT) applications.

  12. Radiation synthesis and characterization of new hydrogels based on acrylamide copolymers cross-linked with 1-allyl-2-thiourea

    Energy Technology Data Exchange (ETDEWEB)

    Sahiner, Nurettin [Department of Chemistry, Faculty of Science, Hacettepe University, Beytepe Campus, 0653 Ankara (Turkey); Malci, Savas [Department of Chemistry, Faculty of Science, Hacettepe University, Beytepe Campus, 0653 Ankara (Turkey); Celikbicak, Oemuer [Department of Chemistry, Faculty of Science, Hacettepe University, Beytepe Campus, 0653 Ankara (Turkey); Kantoglu, Oemer [Ankara Nuclear Research Center, Turkish Atomic Energy Authority, 06983 Ankara (Turkey); Salih, Bekir [Department of Chemistry, Faculty of Science, Hacettepe University, Beytepe Campus, 0653 Ankara (Turkey)]. E-mail: bekir@hacettepe.edu.tr

    2005-10-01

    Poly(acrylamide-1-allyl-2-thiourea) hydrogels, Poly(AA-AT), were synthesized by gamma irradiation using {sup 60}Co {gamma} source in different irradiation dose and at different 1-allyl-2-thiourea content in the monomer mixture. For the characterization of the hydrogels, Fourier transform infrared spectrometer (FT-IR), thermogravimetric analyzer (TGA), elemental analyzer and the swellability of the hydrogels were used. It was noted that 1-allyl-2-thiourea in the synthesized hydrogels was increased by the increasing the content of the 1-allyl-2-thiourea in the irradiation monomer mixture and increasing the radiation dose for the hydrogel synthesis. sis.

  13. Mechanochemical synthesis and structural characterization of three novel cocrystals of dimethylglyoxime with N-heterocyclic aromatic compounds and acetamide

    Science.gov (United States)

    Abidi, Syed Sibte Asghar; Azim, Yasser; Gupta, Abhishek Kumar; Pradeep, Chullikkattil P.

    2017-12-01

    With an aim to explore the interactions of (RR'Cdbnd Nsbnd OH) oxime moiety of dimethylglyoxime (DMG) with pyridyl ring of N-heterocyclic aromatic compounds and acetamide, three novel cocrystals of dimethylglyoxime with acridine (ACR), 1,10-phenanthroline monohydrate (PT) and acetamide (ACT) are reported. These three cocrystals were obtained with a mechanochemical synthesis approach and were characterized by single crystal X-ray diffraction (SCXRD), powder X-ray diffraction (PXRD), fourier transform-infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Additionally, Hirshfeld surface analysis is used to investigate the intermolecular interaction and the crystal packing of cocrystals.

  14. Polyol synthesis of silver nanoplates: The crystal growth mechanism based on a rivalrous adsorption

    International Nuclear Information System (INIS)

    Luo Xiaolin; Li Zongxiao; Yuan Chunlan; Chen Yashao

    2011-01-01

    Highlights: → Silver nanoplates have been successfully synthesized by polyol reduction in the presence of poly (vinylpyrrolidone) (PVP) and HNO 3 . → Due to the discovery of CN - ions in the solution, a mechanism for the anisotropic growth of silver nanoplates is systematically discussed. → TG, FT-IR and SERS were used to provide some direct evidences of rivalrous adsorption between PVP and CN - ions on the surface of the silver crystals. - Abstract: A polyol reducing approach has been applied to synthesize silver nanoplates with an average thickness of 50 nm and edge length of 3 μm in the presence of poly (vinylpyrrolidone) (PVP) and HNO 3 . X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscropy (TEM), and electron diffraction are used to characterize these silver nanoplates. Findings indicate that the nanoplates are single crystals and with their basal plane as (1 1 1) lattice plane. On the basis of the results from thermogravimetric analysis (TG), Fourier transform infrared spectroscopy (FT-IR) and Raman spectroscopy, a crystal growth mechanism based on the rivalrous adsorption between PVP and CN - ions on the surface of silver nanoplates is supposed to explain the crystal anisotropic growth.

  15. Synthesis, characterization, computational studies and biological evaluation of S-benzyl-β-N-[3-(4-hydroxy-3-methoxy-phenylallylidene)]dithiocarbazate

    Science.gov (United States)

    Bhat, Rayees A.; Kumar, D.; Malla, Manzoor A.; Bhat, Sami U.; Khan, Md Shahzad; Manzoor, Ovais; Srivastava, Anurag; Naikoo, Rawoof A.; Mohsin, Mohd; Mir, Muzzaffar A.

    2018-03-01

    S-Benzyl-β-N-[3-(4-hydroxy-3-methoxy-phenylallylidene)]dithiocarbazate (HL1), Schiff base of S-benzyl dithiocarbazate, was synthesized by 1:1 condensation between S-benzyl dithiocarbazate and 4-hydroxy-3-methoxy cinnamaldehyde. The nitrogen-sulfur Schiff base (HL1) was characterized by Mass, FT-IR, H1-NMR, Raman, and UV-VIS spectroscopic techniques. Theoretical quantum chemical calculations were performed using DFT in combination with B3LYP exchange correlation functional and 6-311++ G (d, p) basis sets level. The calculated values of chemical potential (μ), HOMO-LUMO energy gap, chemical hardness, softness (S), ionization energy (IE), electron affinity (EA), dipole moment (D) and relative stabilization energy of the compound were 0.14881 eV, 0.12542 eV, 0.06271 eV, 3.37299 eV, -0.21152 eV, -0.08610 eV, 4.4090 Debye and -1753.350 eV respectively. Theoretically calculated parameters like H1-NMR, FT-IR, UV-VIS, Raman, electrostatic potential and HOMO-LUMO energy gap are in good agreement with experimental results. Also, in-vitro cytotoxicity studies were done against two habitually infection causing bacteria strains including gram-positive (S. aureus) and gram-negative (E. coli) for antibacterial activity. The results showed appreciable biological activity and the activity increased with increase in dose.

  16. FTIR, FT-Raman, FT-NMR, UV-visible and quantum chemical investigations of 2-amino-4-methylbenzothiazole.

    Science.gov (United States)

    Arjunan, V; Sakiladevi, S; Rani, T; Mythili, C V; Mohan, S

    2012-03-01

    The FT-IR (4000-400 cm(-1)) and FT-Raman (4000-100 cm(-1)) spectral measurements and complete assignments of the observed spectra of 2-amino-4-methylbenzothiazole (2A4MBT) have been proposed. Ab initio and DFT calculations have been performed and the structural parameters of the compound were determined from the optimised geometry with 6-31G(d,p), 6-311++G(d,p) and cc-pVDZ basis sets and giving energies, harmonic vibrational frequencies, depolarisation ratios, IR intensities and Raman activities. (1)H and (13)C NMR spectra were recorded and (1)H and (13)C nuclear magnetic resonance chemical shifts of the molecule were calculated using the gauge independent atomic orbital (GIAO) method. UV-visible spectrum of the compound was also recorded and the electronic properties, such as HOMO, LUMO and band gap energies were measured by time-dependent DFT (TD-DFT) approach. The geometric parameters, energies, harmonic vibrational frequencies, IR intensities, Raman activities chemical shifts and absorption wavelengths were compared with the available experimental data of the molecule. The influences of methyl and amino groups on the skeletal modes and on the proton chemical shifts have been investigated. Copyright © 2011 Elsevier B.V. All rights reserved.

  17. Graphene Dendrimer-stabilized silver nanoparticles for detection of methimazole using Surface-enhanced Raman scattering with computational assignment

    Science.gov (United States)

    Saleh, Tawfik A.; Al-Shalalfeh, Mutasem M.; Al-Saadi, Abdulaziz A.

    2016-08-01

    Graphene functionalized with polyamidoamine dendrimer, decorated with silver nanoparticles (G-D-Ag), was synthesized and evaluated as a substrate with surface-enhanced Raman scattering (SERS) for methimazole (MTZ) detection. Sodium borohydride was used as a reducing agent to cultivate silver nanoparticles on the dendrimer. The obtained G-D-Ag was characterized by using UV-vis spectroscopy, scanning electron microscope (SEM), high-resolution transmission electron microscope (TEM), Fourier-transformed infrared (FT-IR) and Raman spectroscopy. The SEM image indicated the successful formation of the G-D-Ag. The behavior of MTZ on the G-D-Ag as a reliable and robust substrate was investigated by SERS, which indicated mostly a chemical interaction between G-D-Ag and MTZ. The bands of the MTZ normal spectra at 1538, 1463, 1342, 1278, 1156, 1092, 1016, 600, 525 and 410 cm-1 were enhanced due to the SERS effect. Correlations between the logarithmical scale of MTZ concentrations and SERS signal intensities were established, and a low detection limit of 1.43 × 10-12 M was successfully obtained. The density functional theory (DFT) approach was utilized to provide reliable assignment of the key Raman bands.

  18. Synthesis, crystal structure, vibrational spectra and theoretical calculations of quantum chemistry of a potential antimicrobial Meldrum's acid derivative

    Science.gov (United States)

    Campelo, M. J. M.; Freire, P. T. C.; Mendes Filho, J.; de Toledo, T. A.; Teixeira, A. M. R.; da Silva, L. E.; Bento, R. R. F.; Faria, J. L. B.; Pizani, P. S.; Gusmão, G. O. M.; Coutinho, H. D. M.; Oliveira, M. T. A.

    2017-10-01

    A new derivative of Meldrum's acid 5-((5-chloropyridin-2-ylamino)methylene)-2,2-dimethyl-1,3-dioxane-4,6-dione (CYMM) of molecular formula C12H11ClN2O4 was synthesized and structurally characterized using single crystal X-ray diffraction technique. The vibrational properties of the crystal were studied by Fourier Transform infrared (FT-IR), Fourier Transform Raman (FT-Raman) techniques and theoretical calculations of quantum chemistry using Density functional theory (DFT) and Density functional perturbation theory (DFPT). A comparison with experimental spectra allowed the assignment of all the normal modes. The descriptions of the normal modes were carried by means of potential energy distribution (PED). Additionally, analysis of the antimicrobial activity and antibiotic resistance modulatory activity was carried out to evaluate the antibacterial potential of the CYMM.

  19. Facile synthesis, single crystal analysis, and computational studies of sulfanilamide derivatives

    Science.gov (United States)

    Tahir, Muhammad Nawaz; Khalid, Muhammad; Islam, Ayesha; Ali Mashhadi, Syed Muddassir; Braga, Ataualpa A. C.

    2017-01-01

    Antibacterial resistance is a worldwide problem. Sulfanilamide is widely used antibacterial. For the first time, we report here a simple method for the derivative synthesis of the title drugs, single crystal XRD and density functional theory (DFT) studies. The optimized molecular structure, natural bond orbital (NBO), frontier molecular orbitals (FMOs) molecular electrostatic potential studies (MEP) and Mulliken population analysis (MPA) have been performed using M06-2X/6-31G(d, p). The FT-IR spectra and thermodynamic parameters were calculated at M06-2X/6-311 + G(2d,p) and B3LYP/6-31G(d, p) levels respectively, while, the UV-Vis analysis was performed using TD-DFT/B3LYP/6-31G(d, p) method. The experimental FT-IR spectra of both compounds were also carried out to reconfirm sbnd H⋯Osbnd hydrogen bonds. The DFT optimized parameters exhibiting good agreement with the experimental data. NBO analysis explored the hyper conjugative interaction and stability of title crystals, especially, reconfirmed the existence of sbnd H⋯Osbnd hydrogen bonds between the dimers. The FT-IR, thermodynamic parameters, MEP and MPA also revealed the hydrogen bonding detail is harmonious to XRD data. As a matter of the fact, the hydrogen bonding is a significant parameter for the understanding and design of molecular crystals, subsequently; it can also play a vital role in the supramolecular chemistry. Moreover, the global reactivity descriptors suggest that title compounds might be bioactive.

  20. Green synthesis of gold nanoparticles using Stevia rebaudiana leaf extracts: Characterization and their stability.

    Science.gov (United States)

    Sadeghi, Babak; Mohammadzadeh, M; Babakhani, B

    2015-07-01

    Various methods invented and developed for the synthesis of gold nanoparticles that increases daily consumed. According to this method, including potential environmental pollution problems and the complexity of the synthesis, in this study, the feasibility of using the leaves extract of Stevia rebaudiana (SR) for the reduction of gold ions to nanoparticles form have been studied. Stevia leaves were used to prepare the aqueous extract for this study. Gold nanoparticles were characterized with different techniques such as UV-vis spectroscopy, FT-IR spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Transmission electron microscopy experiments showed that these nanoparticles are spherical and uniformly distributed and its size is from 5 to 20 nm. FT-IR spectroscopy revealed that gold nanoparticles were functionalized with biomolecules that have primary amine group (NH2), carbonyl group, OH groups and other stabilizing functional groups. X-ray diffraction pattern showed high purity and face centered cubic structure of gold nanoparticles with size of 17 nm. The scanning electron microscopy (SEM) implies the right of forming gold nanoparticles. The results, confirm that gold nanoparticles have synthesized by the leaves extract of S. rebaudiana (SR). Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Synthesis and Characterization of C-Cinnamal Calix [4] Resorsinarena from Cinnamon Oil Waste West Sumatra

    Science.gov (United States)

    Etika, S. B.; Nasra, E.; Rilaztika, I.

    2018-04-01

    Synthesis and characterization of compound C-Cinnamal Calix [4] Resorsinarena (CCCR) of cinnamon oil waste have been done. This study was aimed to synthesis and characterize C-Cinnamal Calix [4] Resorsinarena from cinnamaldehyde violated cinnamon oil waste. C-Cinnamal Calix [4] Resorsinarena was synthesized by electrophilic substitution reaction of cinnamaldehyde isolated by the acid and resorcinol at 77oC temperature for 2 hour. The data analysis spectrum UV-VIS and FT-IR showed that the compound isolated cinnamaldehyde same as pure cinnamaldehyde compound. The characterization of C-Cinnamal Calix [4] Resorsinarena in the form of reddish-colored solids with melting point 3580C by using UV-VIS showed the presence of double bond, FT-IR showed the absorption at the wave number 3323,94 cm-1 indicating the ‑OH group, the wave number 1610,94 cm-1 showed the vibration C=C, the strong region absorption of 1500,86 cm-1 indicating the presence of an aromatic ring, the at 1442,88 cm-1 wave number indicating the presence of CH3.

  2. Influence of synthesis procedure on the formation and properties of zinc oxide

    International Nuclear Information System (INIS)

    Music, S.; Popovic, S.; Maljkovic, M.; Dragcevic, D.

    2002-01-01

    Formation and properties of zinc oxide were investigated in dependence on the synthesis procedure. Zinc oxide did not crystallize upon hydrothermal treatment of Zn(NO 3 ) 2 aqueous solutions containing urea, up to 160 deg. C. Hydrozincite was formed instead. Changes in the X-ray diffraction patterns and Fourier transform infrared (FT-IR) spectra were interpreted in terms of stacking disorder in hydrozincite crystals. Zinc oxide powder was obtained by thermal treatment in air of precipitated hydrozincite. The conditions for instantaneous synthesis of very fine zinc oxide particles were found. This procedure is based on addition of TMAH (tetramethylammonium hydroxide) solution to an ethanolic solution of zinc acetate dihydrate, up to pH∼14. On the other hand, addition of an equivalent volume of water to the ethanolic solution of zinc acetate dihydrate, prior to the addition of TMAH solution up to pH∼14, yielded ZnO flakes without any specific shape. All zinc oxide particles produced upon heating at 600 deg. C in air showed similar morphology and tendency to aggregation due to the sintering effect. The features of the FT-IR spectra of zinc oxide particles were related to their shapes

  3. Synthesis and Characterization of Fluoro- and Chlorobimetallic Alkoxides as Precursors for Luminescent Metal Oxide Materials via Sol-Gel Technique

    Institute of Scientific and Technical Information of China (English)

    ATHAR, Taimur; SEOK, Sang II; KWON, Jeong Oh

    2007-01-01

    Heterobimetallic alkoxides are broadly recognized as versatile precursors for luminescence materials, and efforts are being made to develop novel routes by applying the concept of geometrical molecular design, for their synthesis and to design a single source precursor suited to photoluminescent materials. Novel and new series of bimetallic alkoxides has been prepared by metathesis route. They exhibit a lower sensitivity towards hydrolysis and so they are easier to handle as compared to other alkoxides. All the compounds were characterized by elemental analysis, FT-IR and multinuclear NMR spectroscopies. FT-IR revealed that the molecular structure of these metal spectroscopy provided useful information about chemical shifts for better understanding the likely structure based on interactions with their coordinate metals. The mass spectra show similar types of fragmentation pattern.SEM-EDS analyses showed consistency with the formulation. XRD patterns show an enhanced homogeneity at high temperature. TGA measurements show that thermal decomposition occured in steps that depended entirely on the chemical compositions and the synthesis routes. SEM observation reveals that the morphology and particle size strongly depend on synthesis routes for their precursors.

  4. Plant Extract Mediated Eco-Friendly Synthesis of Pd@Graphene Nanocatalyst: An Efficient and Reusable Catalyst for the Suzuki-Miyaura Coupling

    Directory of Open Access Journals (Sweden)

    Mujeeb Khan

    2017-01-01

    Full Text Available Suzuki-Miyaura coupling reaction catalyzed by the palladium (Pd-based nanomaterials is one of the most versatile methods for the preparation of biaryls. However, use of organic solvents as reaction medium causes a big threat to environment due to the generation of toxic byproducts as waste during the work up of these reactions. Therefore, the use of water as reaction media has attracted tremendous attention due to its environmental, economic, and safety benefits. In this study, we report on the synthesis of green Pd@graphene nanocatalyst based on an in situ functionalization approach which exhibited excellent catalytic activity towards the Suzuki–Miyaura cross-coupling reactions of phenyl halides with phenyl boronic acids under facile conditions in water. The green and environmentally friendly synthesis of Pd@graphene nanocatalyst (PG-HRG-Pd is carried out by simultaneous reduction of graphene oxide (GRO and PdCl2 using Pulicaria glutinosa extract (PGE as reducing and stabilizing agent. The phytomolecules present in the plant extract (PE not only facilitated the reduction of PdCl2, but also helped to stabilize the surface of PG-HRG-Pd nanocatalyst, which significantly enhanced the dispersibility of nanocatalyst in water. The identification of PG-HRG-Pd was established by various spectroscopic and microscopic techniques, including, high-resolution transmission electron microscopy (HRTEM, X-ray diffraction (XRD, ultraviolet–visible spectroscopy (UV-Vis, Fourier transform infrared spectroscopy (FT-IR, and Raman spectroscopy. The as-prepared PG-HRG-Pd nanocatalyst demonstrated excellent catalytic activity towards the Suzuki-Miyaura cross coupling reactions under aqueous, ligand free, and aerobic conditions. Apart from this the reusability of the catalyst was also evaluated and the catalyst yielded excellent results upon reuse for several times with marginal loss of its catalytic performance. Therefore, the method developed for the green

  5. CuI nanoparticles as a remarkable catalyst in the synthesis of benzo[b][1,5]diazepines: an eco-friendly approach.

    Science.gov (United States)

    Ghasemzadeh, Mohammad Ali; Safaei-Ghomi, Javad

    2015-01-01

    Highly efficient CuI nanoparticles catalyzed one-pot synthesis of some benzo[b][1,5]diazepine derivatives via multi-component condensation of aromatic diamines, Meldrum's acid and isocyanides. The present approach creates a variety of benzo[b][1,5]diazepines as pharmaceutical and biologically active heterocyclic compounds in excellent yields and short reaction times. The salient features of the copper iodide nanoparticles are: easy preparation, cost-effective, high stability, low loading and reusability of the catalyst. The prepared copper iodide nanoparticles were fully characterized by XRD, EDX, FT-IR, SEM and TEM analysis.

  6. Synthesis, characterization, and 3D-FDTD simulation of Ag@SiO2 nanoparticles for shell-isolated nanoparticle-enhanced Raman spectroscopy.

    Science.gov (United States)

    Uzayisenga, Viviane; Lin, Xiao-Dong; Li, Li-Mei; Anema, Jason R; Yang, Zhi-Lin; Huang, Yi-Fan; Lin, Hai-Xin; Li, Song-Bo; Li, Jian-Feng; Tian, Zhong-Qun

    2012-06-19

    Au-seed Ag-growth nanoparticles of controllable diameter (50-100 nm), and having an ultrathin SiO(2) shell of controllable thickness (2-3 nm), were prepared for shell-isolated nanoparticle-enhanced Raman spectroscopy (SHINERS). Their morphological, optical, and material properties were characterized; and their potential for use as a versatile Raman signal amplifier was investigated experimentally using pyridine as a probe molecule and theoretically by the three-dimensional finite-difference time-domain (3D-FDTD) method. We show that a SiO(2) shell as thin as 2 nm can be synthesized pinhole-free on the Ag surface of a nanoparticle, which then becomes the core. The dielectric SiO(2) shell serves to isolate the Raman-signal enhancing core and prevent it from interfering with the system under study. The SiO(2) shell also hinders oxidation of the Ag surface and nanoparticle aggregation. It significantly improves the stability and reproducibility of surface-enhanced Raman scattering (SERS) signal intensity, which is essential for SERS applications. Our 3D-FDTD simulations show that Ag-core SHINERS nanoparticles yield at least 2 orders of magnitude greater enhancement than Au-core ones when excited with green light on a smooth Ag surface, and thus add to the versatility of our SHINERS method.

  7. On the use of spectra from portable Raman and ATR-IR instruments in synthesis route attribution of a chemical warfare agent by multivariate modeling.

    Science.gov (United States)

    Wiktelius, Daniel; Ahlinder, Linnea; Larsson, Andreas; Höjer Holmgren, Karin; Norlin, Rikard; Andersson, Per Ola

    2018-08-15

    Collecting data under field conditions for forensic investigations of chemical warfare agents calls for the use of portable instruments. In this study, a set of aged, crude preparations of sulfur mustard were characterized spectroscopically without any sample preparation using handheld Raman and portable IR instruments. The spectral data was used to construct Random Forest multivariate models for the attribution of test set samples to the synthetic method used for their production. Colored and fluorescent samples were included in the study, which made Raman spectroscopy challenging although fluorescence was diminished by using an excitation wavelength of 1064 nm. The predictive power of models constructed with IR or Raman data alone, as well as with combined data was investigated. Both techniques gave useful data for attribution. Model performance was enhanced when Raman and IR spectra were combined, allowing correct classification of 19/23 (83%) of test set spectra. The results demonstrate that data obtained with spectroscopy instruments amenable for field deployment can be useful in forensic studies of chemical warfare agents. Copyright © 2018 Elsevier B.V. All rights reserved.

  8. The synthesis and the spectroscopic, thermal, and structural properties of the M2[(fumarate)Ni(CN)4]·2(1,4-Dioxane) clathrate (M = Co, Ni, Cd and Hg)

    Science.gov (United States)

    Kartal, Zeki; Yavuz, Abdülkerim

    2018-03-01

    In this study, the clathrates of fumarate-tetracyanonickel-dioxane, given by the formula M2[(fumarate)Ni(CN)4]·2(1,4-Dioxane) (M = Co, Ni, Cd and Hg), have been obtained for the first time through chemical methods. These clathrates have been characterized by elemental, thermal, FT-IR, and FT-Raman spectroscopies. The parameters of structures of clathrates have been determined by X-ray powder diffraction. The thermal behaviors of these clathrates have been also investigated by thermo-gravimetric analysis (TGA), differential thermal analysis (DTA), and derivative thermal gravimetric analysis (DTG) in the range of 20-900 °C. X-ray powder diffraction data have been recorded at ambient temperature in the 2θ range 5-50°. The FT-IR and FT-Raman spectra of clathrates have been recorded in the region of 4000-400 cm-1 and 4000-100 cm-1, respectively. The results of the spectral and thermal analyses of the newly synthesized clathrates of fumarate-tetracyanonickel-dioxane suggest that these clathrates are new examples of the Hofmann-type dioxane clathrates. In our study, the Hofmann-type dioxane clathrates, which are formed by bounding electrons of oxygen-donor atoms of fumarate ion ligand molecule to transition metal atoms, consist of the corrugated |M-Ni(CN)4|∞ polymeric layers, which are held in parallel through the chain of (-M-fumarate-M-).

  9. Synthesis and photocatalytic degradation study of methylene blue dye under visible light irradiation by Fe1-xBixVO4 solid solutions (0 ≤ x ≤ 1.0)

    Science.gov (United States)

    Bera, Ganesh; Reddy, V. R.; Mal, Priyanath; Das, Pradip; Turpu, G. R.

    2018-05-01

    The novel hetero-structures Fe1-xBixVO4 solid solutions (0 ≤ x ≤ 1.0) with the two dissimilar end member of FeVO4 - BiVO4, were successfully synthesized by the standard solid state reaction method. The structural and chemical properties of as prepared photo-catalyst samples were characterized by X-ray diffraction (XRD), Raman spectroscopy, Fourier transform infrared spectroscopy (FT-IR) and UV-visible absorption spectroscopy techniques. It is confirmed from the results of XRD, Raman and FT-IR that FeVO4 and BiVO4 are in triclinic (space group P-1 (2)) and monoclinic (space group I2/b (15)) phases respectively. The Bi incorporation into Fe site of FeVO4 emerges as hetero-structures of both the end members of the solid solutions. In addition, the photocatalytic activity in the degradation of methylene blue (MB) dye under visible light irradiation was carried out through UV-visible spectroscopy measurement of photo-catalysts FeVO4, BiVO4 and mixed phases of both photo-catalyst. The results indicate that under visible light irradiation the photocatalytic activity of mixed phases were very effective and higher than the both single phases of the solid solutions. The composition x= 0.25 exhibits an excellent photocatalytic property for the degradation of MB solution under visible light irradiation rather than other.

  10. Pseudo template synthesis of poly (1-naphthylamine): effect of environment on nanostructured morphology

    International Nuclear Information System (INIS)

    Riaz, Ufana; Ahmad, Sharif; Ashraf, S. M.

    2008-01-01

    A template free approach was adopted to explore the effect of polymerization environment on the synthesis of nanostructured poly (1-naphthylamine) (PNA) using cupric chloride as oxidant and methyl alcohol as medium. The polymerization environment was varied by carrying out the synthesis in the presence of nitrogen and oxygen. The morphology of the synthesized nanostructured PNA was investigated using scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-vis and FT-IR spectroscopies. PNA nanorods of sizes varying between 50-100 nm were obtained in presence of nitrogen while in presence of oxygen, it formed aggregated globular particles of sizes varying between 80-100 nm. The results provide valuable information on controlling the synthesis of one-dimensional nanostructured conducting polymers that exhibit superior processibility as compared to the conventional conducting polymers.

  11. Study of the influence in crystallization period in MCM-22 zeolite synthesis

    International Nuclear Information System (INIS)

    Barbosa, A.S.; Santos, E.R.F.; Rodrigues, M.G.F.

    2011-01-01

    The synthesis of MCM-22 is accomplished by hydrothermal treatment and long periods needed for crystallization, with the gradual growth of crystals of 10-14 days. MCM-22 catalyst is studied intensively as promising, with high thermal stability. As part of a line of research focused on the development of zeolite with lowest cost, this study aimed to examine the effect in decreasing the period of crystallization in the synthesis of zeolite MCM-22. The materials were characterized by X-ray diffraction (XRD) spectroscopy, X-ray Energy Dispersive (EDX) and Fourier transform infrared spectroscopy and Fourier transform (FT-IR). By XRD it was observed that the hydrothermal treatment used in the synthesis was effective during periods of crystallization and EDX was observed that the samples have a high percentage of silica and low alumina content, which gives them a high ratio SiO 2 /Al 2 O 3 characteristic of the MWW structure. (author)

  12. Colloidal synthesis and characterization of Bi2S3 nanoparticles for photovoltaic applications

    International Nuclear Information System (INIS)

    Piras, R; Aresti, M; Saba, M; Marongiu, D; Mula, G; Quochi, F; Mura, A; Bongiovanni, G; Cannas, C; Mureddu, M; Ardu, A; Ennas, G; Musinu, A; Calzia, V; Mattoni, A

    2014-01-01

    Bismuth sulfide is a promising n-type semiconductor for solar energy conversion. We have explored the colloidal synthesis of Bi 2 S 3 nanocrystals, with the aim of employing them in the fabrication of solution-processable solar cells and to replace toxic heavy metals chalcogenides like PbS or CdS, that are currently employed in such devices. We compare different methods to obtain Bi 2 S 3 colloidal quantum dots, including the use of environmentally benign reactants, through organometallic synthesis. Different sizes and shapes were obtained according to the synthesis parameters and the growth process has been rationalized by comparing the predicted morphology with systematic physical-chemistry characterization of nanocrystals by X-ray diffraction, FT-IR spectroscopy, Transmission Electron Microscopy (TEM)

  13. Progress in the synthesis and characterization of magnetite nanoparticles with amino groups on the surface

    Science.gov (United States)

    Durdureanu-Angheluta, A.; Dascalu, A.; Fifere, A.; Coroaba, A.; Pricop, L.; Chiriac, H.; Tura, V.; Pinteala, M.; Simionescu, B. C.

    2012-05-01

    This manuscript deals with the synthesis of new hydrophilic magnetite particles by employing a two-step method: in the first step magnetite particles with hydrophobic shell formed in presence of oleic acid-oleylamine complex through a synthesis in mass, without solvent, in a mortar with pestle were obtained; while in the second step the hydrophobic shell was interchanged with an aminosilane monomer. The influence of the Fe2+/Fe3+ molar ratio on the dimension of the particles of high importance for their potential applications was carefully investigated. This paper, also presents an alternative method of synthesis of new core-shell magnetite particles and the complete study of their structure and morphology by FT-IR, XPS, TGA, ESEM and TEM techniques. The rheological properties and magnetization analysis of high importance for magnetic particles were also investigated.

  14. Synthesis, structure characterization and catalytic activity of nickel tungstate nanoparticles

    International Nuclear Information System (INIS)

    Pourmortazavi, Seied Mahdi; Rahimi-Nasrabadi, Mehdi; Khalilian-Shalamzari, Morteza; Zahedi, Mir Mahdi; Hajimirsadeghi, Seiedeh Somayyeh; Omrani, Ismail

    2012-01-01

    Graphical abstract: NiWO 4 nanoparticles were prepared via precipitation technique. Experimental parameters of procedure were optimized statistically. Highlights: ► NiWO 4 spherical nanoparticles were synthesized via direct precipitation method. ► Taguchi robust design was used for optimization of synthesis reaction parameters. ► Composition and structural properties of NiWO 4 nanoparticles were characterized. ► EDAX, XRD, SEM, FT-IR, UV–vis and photoluminescence techniques were employed. ► Catalytic activity of the product in a cyclo-addition reaction was investigated. - Abstract: Taguchi robust design was applied to optimize experimental parameters for controllable, simple and fast synthesis of nickel tungstate nanoparticles. NiWO 4 nanoparticles were synthesized by precipitation reaction involving addition of nickel ion solution to the tungstate aqueous reagent and then formation of nickel tungstate nucleolus which are insoluble in aqueous media. Effects of various parameters such as nickel and tungstate concentrations, flow rate of reagent addition and reactor temperature on diameter of synthesized nickel tungstate nanoparticles were investigated experimentally by the aid of orthogonal array design. The results for analysis of variance (ANOVA) showed that particle size of nickel tungstate can be effectively tuned by controlling significant variables involving nickel and tungstate concentrations and flow rate; while, temperature of the reactor has a no considerable effect on the size of NiWO 4 particles. The ANOVA results proposed the optimum conditions for synthesis of nickel tungstate nanoparticles via this technique. Also, under optimum condition nanoparticles of NiWO 4 were prepared and their structure and chemical composition were characterized by means of EDAX, XRD, SEM, FT-IR spectroscopy, UV–vis spectroscopy, and photoluminescence. Finally, catalytic activity of the nanoparticles in a cycloaddition reaction was examined.

  15. Synthesis, structure characterization and catalytic activity of nickel tungstate nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Pourmortazavi, Seied Mahdi, E-mail: pourmortazavi@yahoo.com [Faculty of Material and Manufacturing Technologies, Malek Ashtar University of Technology, Tehran (Iran, Islamic Republic of); Rahimi-Nasrabadi, Mehdi, E-mail: rahiminasrabadi@gmail.com [Department of Chemistry, Imam Hossein University, Tehran (Iran, Islamic Republic of); Khalilian-Shalamzari, Morteza [Department of Chemistry, Imam Hossein University, Tehran (Iran, Islamic Republic of); Zahedi, Mir Mahdi; Hajimirsadeghi, Seiedeh Somayyeh [Islamic Azad University, Varamin Pishva Branch, Varamin (Iran, Islamic Republic of); Omrani, Ismail [Department of Chemistry, Imam Hossein University, Tehran (Iran, Islamic Republic of)

    2012-12-15

    Graphical abstract: NiWO{sub 4} nanoparticles were prepared via precipitation technique. Experimental parameters of procedure were optimized statistically. Highlights: Black-Right-Pointing-Pointer NiWO{sub 4} spherical nanoparticles were synthesized via direct precipitation method. Black-Right-Pointing-Pointer Taguchi robust design was used for optimization of synthesis reaction parameters. Black-Right-Pointing-Pointer Composition and structural properties of NiWO{sub 4} nanoparticles were characterized. Black-Right-Pointing-Pointer EDAX, XRD, SEM, FT-IR, UV-vis and photoluminescence techniques were employed. Black-Right-Pointing-Pointer Catalytic activity of the product in a cyclo-addition reaction was investigated. - Abstract: Taguchi robust design was applied to optimize experimental parameters for controllable, simple and fast synthesis of nickel tungstate nanoparticles. NiWO{sub 4} nanoparticles were synthesized by precipitation reaction involving addition of nickel ion solution to the tungstate aqueous reagent and then formation of nickel tungstate nucleolus which are insoluble in aqueous media. Effects of various parameters such as nickel and tungstate concentrations, flow rate of reagent addition and reactor temperature on diameter of synthesized nickel tungstate nanoparticles were investigated experimentally by the aid of orthogonal array design. The results for analysis of variance (ANOVA) showed that particle size of nickel tungstate can be effectively tuned by controlling significant variables involving nickel and tungstate concentrations and flow rate; while, temperature of the reactor has a no considerable effect on the size of NiWO{sub 4} particles. The ANOVA results proposed the optimum conditions for synthesis of nickel tungstate nanoparticles via this technique. Also, under optimum condition nanoparticles of NiWO{sub 4} were prepared and their structure and chemical composition were characterized by means of EDAX, XRD, SEM, FT-IR spectroscopy, UV

  16. Synthesis of Siloxanes Directly from Amorphous Silica

    International Nuclear Information System (INIS)

    Myint Sandar Win

    2011-12-01

    A direct synthesis of oligomeric-siloxanes from amorphous silica has been achieved. The compound prepared was caedonal-siloxane. Cardonal is a mono hydroxyphenolic compound with a bulky group in the meta position. It was derived as a by-product from the renewable resources cashew nut shell liquid (CNSL). In the synthesis, one pot synthesis was carried out by using ethylene glycol (EG) as solvent. In the reaction ethylene glycol served as a primary precursor chelating ligand in the synthesised product. The one pot synthesis was enhanced by the strong base, triethylenetetramine (TETA) which served as the promoter catalyst. In the synthesis, optimal conditions were established on the basic of the yield percent of organo-siloxane compounds with respect to the variation of the weight fraction of TETA and to the variation of reaction time. Experimental runs were carried out at (ca 210 2c) which was nearly above the boiling point of the solvent. The substituted organo-silicon compounds obtained were characterized by FT- ir, Thermal analysis, XRD and SEM.

  17. H3PW12O40 Encapsulation by Nanoporous Metal Organic Framework HKUST-1: Synthesis, Characterization, Activity and Stability.

    Science.gov (United States)

    Rafiee, Ezzat; Nobakht, Narges

    2016-01-01

    Hybrid composite material was obtained through encapsulation of H3PW12O40 (PW) into HKUST-1 (Cu3(BTC)2, BTC = 1,3,5-benzenetricarboxylic acid), in molar composition of 5 Cu(NO3)2 · 3H2O/2.8 BTC/0.3 PW/0.6 CTAB by adding solutions of PW and copper salts to mixture of BTC and surfactant. The catalyst was characterized by various techniques including powder X-ray diffraction (XRD), Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), energy dispersive X-ray (EDX), laser particle size analyzer, Brunauer Emmett-Teller (BET). The acidity of the catalyst was measured by a potentiometric titration with n-butylamine and PW/HKUST-1 presented very strong acidic sites with Ei > 100 mV. This nano catalyst was successfully used for the synthesis of various β-keto enol ethers at 45 °C with 51-98% yield after 5-75 min. The catalyst was easily recycled and reused at least four times without significant loss of its activity (94% yield after forth run). The presence of the PW in PW/HKUST-1 and reused PW/HKUST-1 structure, eliminating any doubt about collapse of the HKUST-1 after catalytic reaction and can be followed by FT-IR, XRD and SEM techniques. Brönsted and Lewis acidity of the PW/HKUST-1 catalyst was distinguished by studying the FT-IR and determined by chemisorption of pyridine. The strength and dispersion of the protons on PW/HKUST-1 was considerably high and active surface protons became more available for reactant.

  18. Fe_3O_4@B-MCM-41: A new magnetically recoverable nanostructured catalyst for the synthesis of polyhydroquinolines

    International Nuclear Information System (INIS)

    Abdollahi-Alibeik, Mohammad; Rezaeipoor-Anari, Ali

    2016-01-01

    Boron modified MCM-41 with magnetite core (Fe_3O_4@B-MCM-41) as a new magnetically recoverable heterogeneous catalyst was prepared and characterized by SEM, TEM, BET, XRD, VSM and FT-IR techniques. The catalytic activity of Fe_3O_4@B-MCM-41 was investigated in the four-component reaction of aldehyde, dimedone, active methylene compounds and ammonium acetate for the synthesis of polyhydroquinolines. According to optimization and characterization results the catalyst with Si:B:Fe_3O_4 mole composition of 40:4:1 has the best activity. The catalyst could be recovered easily by external magnet and has excellent reusability many times without significant decrease of activity. - Highlights: • Core–shell Fe_3O_4@MCM-41 nanoparticles modified by boron (Fe_3O_4@B-MCM-41). • Fe_3O_4@B-MCM-41 as reusable catalyst for the synthesis of polyhydroquinolines. • Characterization of Fe_3O_4@B-MCM-41 using SEM, TEM, BET, XRD and FT-IR techniques.

  19. Facile synthesis of gold coated copper(II) hydroxide pine-needle-like micro/nanostructures for surface-enhanced Raman scattering

    Science.gov (United States)

    Long, Kailin; Du, Deyang; Luo, Xiaoguang; Zhao, Weiwei; Wu, Zhangting; Si, Lifang; Qiu, Teng

    2014-08-01

    This work reports a facile method to fabricate gold coated copper(II) hydroxide pine-needle-like micro/nanostructures for surface-enhanced Raman scattering (SERS) application. The effects of reaction parameters on the shape, size and surface morphology of the products are systematically investigated. The as-prepared 3D hierarchical structures have the advantage of a large surface area available for the formation of hot spots and the adsorption of target analytes, thus dramatically improving the Raman signals. The finite difference time domain calculations indicate that the pine-needle-like model pattern may demonstrate a high quality SERS property owing to the high density and abundant hot spot characteristic in closely spaced needle-like arms.

  20. Green Synthesis of Novel Polyaniline Nanofibers: Application in pH Sensing

    Directory of Open Access Journals (Sweden)

    Shivani Tanwar

    2015-10-01

    Full Text Available An optically active polyaniline nanomaterial (PANI-Nap, doped with (S-naproxen, was developed and evaluated as a potent pH sensor. We synthesized the material in one pot by the addition of the dopant, (S-naproxen, prior to polymerization, followed by the addition of the oxidizing agent (ammonium persulfate that causes polymerization of the aniline. This green chemistry approach allowed us to take only 1 h to produce a water-soluble and stable nanomaterial. UV-visible spectroscopy, fluorescence spectroscopy, FT-IR spectroscopy, Raman spectroscopy, scanning electron microscopy (SEM, transmission electron microscopy (TEM, and X-ray photoelectron spectroscopy (XPS were used to characterize the designed nanomaterial. This nanomaterial exhibited excellent pH sensing properties and showed long term stability (up to one month without loss of sensor performance.

  1. Synthesis of drug loaded magnetic nanoparticles and their uptake into immune cells

    International Nuclear Information System (INIS)

    Prinz, Eva-Marie; Hempelmann, Rolf; Eggers, Ruth; Lee, Hyeck-Hee; Steinfeld, Ute

    2010-01-01

    Ferrite nanoparticles (Mn 0,8 Zn 0,2 Fe 2 O 4 ) are synthesized by the co-precipitation method and characterized by X-ray diffraction, transmission electron microscopy and dynamic light scattering. The particles are functionalized with dextran which is activated via amino or carboxymethyl groups. The chemotherapeutic drug doxorubicin (DOX) is attached to these dextran derivates in different ways. One method is based on the attachment of DOX to amino dextran by its keto group; the other is a bond to the primary amino group of DOX. The characterization of drug loaded dextran derivates is performed by Raman, FT-IR-, UV/VIS-and fluorescence spectroscopy. The biofunctionalized particles are intended for use in adoptive cancer immunotherapy as a new approach, where immune cells (T lymphocytes) will be used as new autonomous highly target specific drug delivery systems. The uptake efficiency of these particles into T lymphocytes is investigated by fluorescence and convocal microscopy.

  2. Synthesis and spectral characterization of hydrazone derivative of furfural using experimental and DFT methods.

    Science.gov (United States)

    Babu, N Ramesh; Subashchandrabose, S; Ali Padusha, M Syed; Saleem, H; Erdoğdu, Y

    2014-01-01

    The Spectral Characterization of (E)-1-(Furan-2-yl) methylene)-2-(1-phenylvinyl) hydrazine (FMPVH) were carried out by using FT-IR, FT-Raman and UV-Vis., Spectrometry. The B3LYP/6-311++G(d,p) level of optimization has been performed on the title compound. The conformational analysis was performed for this molecule, in which the cis and trans conformers were studied for spectral characterization. The recorded spectral results were compared with calculated results. The optimized bond parameters of FMPVH molecule was compared with X-ray diffraction data of related molecule. To study the intra-molecular charge transfers within the molecule the Lewis (bonding) and Non-Lewis (anti-bonding) structural calculation was performed. The Non-linear optical behavior of the title compound was measured using first order hyperpolarizability calculation. The atomic charges were calculated and analyzed. Copyright © 2013 Elsevier B.V. All rights reserved.

  3. Synthesis and Characterization of Nanofibrous Polyaniline Thin Film Prepared by Novel Atmospheric Pressure Plasma Polymerization Technique.

    Science.gov (United States)

    Park, Choon-Sang; Kim, Dong Ha; Shin, Bhum Jae; Tae, Heung-Sik

    2016-01-11

    This work presents a study on the preparation of plasma-polymerized aniline (pPANI) nanofibers and nanoparticles by an intense plasma cloud type atmospheric pressure plasma jets (iPC-APPJ) device with a single bundle of three glass tubes. The nano size polymer was obtained at a sinusoidal wave with a peak value of 8 kV and a frequency of 26 kHz under ambient air. Discharge currents, photo-sensor amplifier, and optical emission spectrometer (OES) techniques were used to analyze the plasma produced from the iPC-APPJ device. Field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), gas chromatography-mass spectrometry (GC-MS), and gel permeation chromatography (GPC) techniques were used to analyze the pPANI. FE-SEM and TEM results show that pPANI has nanofibers, nanoparticles morphology, and polycrystalline characteristics. The FT-IR and GC-MS analysis show the characteristic polyaniline peaks with evidence that some quinone and benzene rings are broken by the discharge energy. GPC results show that pPANI has high molecular weight ( M w ), about 533 kDa with 1.9 polydispersity index (PDI). This study contributes to a better understanding on the novel growth process and synthesis of uniform polyaniline nanofibers and nanoparticles with high molecular weights using the simple atmospheric pressure plasma polymerization technique.

  4. Coriandrum sativum mediated synthesis of silver nanoparticles and evaluation of their biological characteristics

    Science.gov (United States)

    Senthilkumar, N.; Aravindhan, V.; Ruckmani, K.; Vetha Potheher, I.

    2018-05-01

    Silver (Ag) nanoparticles (NPs) were prepared by percolated green synthesis method using Coriandrum sativum leaf, root, seed and stem extracts and reported its antibacterial activity. The synthesized Ag NPs were confirmed by UV–visible Spectroscopy, Powder x-ray Diffraction (PXRD), Fourier Transform Infra Red (FT-IR) Spectroscopy analyzes. The Maximum absorbance observed around 400–450 nm reveal the characteristic absorbance of Ag NPs. The Dynamic Light Scattering (DLS) analysis shows the stability of synthesized NPs with average size varying from 35 to 53 nm and also zeta potential stability varying from ‑20 to ‑30 mV. The cubic structure, crystalline nature and purity of the material was confirmed by powder x-ray diffraction studies. FT-IR spectrum shows the presence of various functional groups in the resultant material. The Field Emission Scanning Electron Microscopy (FESEM) image shows the surface morphology of the synthesized NPs and the Energy Dispersive x-ray Analysis (EDAX) confirms the presence of silver metal ions. The Coriandrum sativum aqueous extract exhibited excellent antimicrobial activity against Klebsiella pneumoniae (Gram -ve) bacteria. Numerous studies have been made previously in our field of study but optimization has not been carried out by both extract (different parts like leaf, root, seed and stem) and without addition of any external source such as chemicals, heat etc.

  5. Synthesis, Characterization, and Self-Assembly of a Tetrathiafulvalene (TTF–Triglycyl Derivative

    Directory of Open Access Journals (Sweden)

    Sónia Pérez-Rentero

    2018-04-01

    Full Text Available In this work, we describe the synthesis, characterization, and self-assembly properties of a new tetrathiafulvalene (TTF–triglycyl low-molecular-weight (LMW gelator. Supramolecular organogels were obtained in various solvents via a heating–cooling cycle. Critical gelation concentrations (CGC (range ≈ 5–50 g/L and thermal gel-to-sol transition temperatures (Tgel (range ≈ 36–51 °C were determined for each gel. Fourier transform infrared (FT-IR spectroscopy suggested that the gelator is also aggregated in its solid state via a similar hydrogen-bonding pattern. The fibrillar microstructure and viscoelastic properties of selected gels were demonstrated by means of field-emission electron microscopy (FE-SEM and rheological measurements. As expected, exposure of a model xerogel to I2 vapor caused the oxidation of the TTF unit as confirmed by UV-vis-NIR analysis. However, FT-IR spectroscopy showed that the oxidation was accompanied with concurrent alteration of the hydrogen-bonded network.

  6. Synthesis and Characterization of Nanofibrous Polyaniline Thin Film Prepared by Novel Atmospheric Pressure Plasma Polymerization Technique

    Directory of Open Access Journals (Sweden)

    Choon-Sang Park

    2016-01-01

    Full Text Available This work presents a study on the preparation of plasma-polymerized aniline (pPANI nanofibers and nanoparticles by an intense plasma cloud type atmospheric pressure plasma jets (iPC-APPJ device with a single bundle of three glass tubes. The nano size polymer was obtained at a sinusoidal wave with a peak value of 8 kV and a frequency of 26 kHz under ambient air. Discharge currents, photo-sensor amplifier, and optical emission spectrometer (OES techniques were used to analyze the plasma produced from the iPC-APPJ device. Field emission scanning electron microscopy (FE-SEM, transmission electron microscopy (TEM, Fourier transform infrared spectroscopy (FT-IR, gas chromatography-mass spectrometry (GC-MS, and gel permeation chromatography (GPC techniques were used to analyze the pPANI. FE-SEM and TEM results show that pPANI has nanofibers, nanoparticles morphology, and polycrystalline characteristics. The FT-IR and GC-MS analysis show the characteristic polyaniline peaks with evidence that some quinone and benzene rings are broken by the discharge energy. GPC results show that pPANI has high molecular weight (Mw, about 533 kDa with 1.9 polydispersity index (PDI. This study contributes to a better understanding on the novel growth process and synthesis of uniform polyaniline nanofibers and nanoparticles with high molecular weights using the simple atmospheric pressure plasma polymerization technique.

  7. Synthesis and optical properties of Mg-Al layered double hydroxides precursor powders

    Directory of Open Access Journals (Sweden)

    Chia-Hsuan Lin

    2017-12-01

    Full Text Available The synthesis and optical properties of Mg-Al layered double hydroxide (LDH precursor powders were investigated using X-ray diffraction (XRD, Fourier transform-infrared (FT-IR spectroscopy, transmission electron microscopy (TEM, selected area electron diffraction (SAED, high-resolution TEM (HRTEM, UV-transmission spectrometer, and fluorescence spectrophotometer. The FT-IR results show that the intense absorption at around 1363–1377 cm-1 can be assigned to the antisymmetric ν3 mode of interlayer carbonate anions because the LDH phase contains some CO32-. The XRD results show that all of the Mg-Al LDH precursor powders contain only a single phase of [Mg0.833Al0.167(OH2](CO30.083·(H2O0.75 but have broad and weak intensities of peaks. All of Mg-Al LDHs precursor powders before calcination have the same photoluminescence (PL spectra. Moreover, these spectra were excited at λex = 235 nm, and the broad emission band was in the range 325-650 nm. In the range, there were relatively strong intensity at around 360, 407 and 510 nm, respectively.

  8. Synthesis, spectroscopic characterization, biological screenings, DNA binding study and POM analyses of transition metal carboxylates

    Science.gov (United States)

    Uddin, Noor; Sirajuddin, Muhammad; Uddin, Nizam; Tariq, Muhammad; Ullah, Hameed; Ali, Saqib; Tirmizi, Syed Ahmed; Khan, Abdur Rehman

    2015-04-01

    This article contains the synthesis of a novel carboxylic acid derivative, its transition metal complexes and evaluation of biological applications. Six carboxylate complexes of transition metals, Zn(II) and Hg(II), have been successfully synthesized and characterized by FT-IR and NMR (1H, 13C). The ligand, HL, (4-[(2,6-Diethylphenyl)amino]-4-oxobutanoic acid) was also characterized by single crystal X-ray analysis. The complexation occurs via oxygen atoms of the carboxylate moiety. FT-IR date show the bidentate nature of the carboxylate moiety of the ligand as the Δν value in all complexes is less than that of the free ligand. The ligand and its complexes were screened for antifungal and antileishmanial activities. The results showed that the ligand and its complexes are active with few exceptions. UV-visible spectroscopy and viscometry results reveal that the ligand and its complexes interact with the DNA via intercalative mode of interaction. A new and efficient strategy to identify the pharmacophores and anti-pharmacophores sites in carboxylate derivatives for the antibacterial/antifungal activity using Petra, Osiris and Molinspiration (POM) analyses was also carried out.

  9. One-pot green synthesis of zinc oxide nano rice and its application as sonocatalyst for degradation of organic dye and synthesis of 2-benzimidazole derivatives

    Science.gov (United States)

    Paul, Bappi; Vadivel, Sethumathavan; Dhar, Siddhartha Sankar; Debbarma, Shyama; Kumaravel, M.

    2017-05-01

    In this paper, we report novel and green approach for one-pot biosynthesis of zinc oxide (ZnO) nanoparticles (NPs). Highly stable and hexagonal phase ZnO nanoparticles were synthesized using seeds extract from the tender pods of Parkia roxburghii and characterized by XRD, FT-IR, EDX, TEM, and N2 adsorption-desorption (BET) studies. The present method of synthesis of ZnO NPs is very efficient and cost effective. The powder XRD pattern furnished evidence for the formation of hexagonal close packing structure of ZnO NPs having average crystallite size 25.6 nm. The TEM image reveals rice shapes ZnO NPs are with an average diameter of 40-60 nm. The as-synthesized ZnO NPs has proved to be an excellent sonocatalysts for degradation of organic dye and synthesis of 2-benzimidazole derivatives.

  10. Anchoring of Cu(II) onto surface of porous metal-organic framework through post-synthesis modification for the synthesis of benzimidazoles and benzothiazoles

    Science.gov (United States)

    Kardanpour, Reihaneh; Tangestaninejad, Shahram; Mirkhani, Valiollah; Moghadam, Majid; Mohammadpoor-Baltork, Iraj; Zadehahmadi, Farnaz

    2016-03-01

    Efficient synthesis of various benzimidazoles and benzothiazoles under mild conditions catalyzed by Cu(II) anchored onto UiO-66-NH2 metal organic framework is reported. In this manner, first, the aminated UiO-66 was modified with thiophene-2-carbaldehyde and then the prepared Schiff base was reacted with CuCl2. The prepared catalyst was characterized by FT-IR, UV-vis, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), N2 adsorption, inductively coupled plasma atomic emission spectroscopy (ICP-AES) and field emission scanning electron microscopy (FE-SEM). The UiO-66-NH2-TC-Cu was applied as a highly efficient catalyst for synthesis of benzimidazole and benzothiazole derivatives by the reaction of aldehydes with 1,2-diaminobenzene or 2-aminothiophenol. The Cu(II)-containing MOF was reused several times without any appreciable loss of its efficiency.

  11. Synthesis of p-Phenylenediamine (PPD) using Supercritical Ammonia

    International Nuclear Information System (INIS)

    Cho, Hang-Kyu; Lim, Jong Sung

    2015-01-01

    In this study, investigated the synthesis method of p-Phenylenediamine (PPD) by amination of p-Diiodobenzene (PDIB) under supercritical ammonia and CuI catalyst conditions. We examined the effects of various process variables (e.g., reaction temperature, pressure, amount of ammonia inserted, amount of catalyst inserted, and reaction time) on the production yield of PPD by analyzing the Gas Chromatography (GC). The experimental results demonstrated that PPD was not produced under non-catalyst conditions, and PPD production yield increased with increasing temperature, pressure, amount of catalyst inserted, and reaction time. However, for the reaction temperature case, it was found that 200 .deg. C was the optimal temperature, because thermal degradation of PPD occurred above 250 .deg. C. In addition, we confirmed the structure of PPD and the bonding characteristics of the amine group via FT-IR and H-NMR analysis

  12. Synthesis of p-Phenylenediamine (PPD) using Supercritical Ammonia

    Energy Technology Data Exchange (ETDEWEB)

    Cho, Hang-Kyu; Lim, Jong Sung [Sogang University, Seoul (Korea, Republic of)

    2015-02-15

    In this study, investigated the synthesis method of p-Phenylenediamine (PPD) by amination of p-Diiodobenzene (PDIB) under supercritical ammonia and CuI catalyst conditions. We examined the effects of various process variables (e.g., reaction temperature, pressure, amount of ammonia inserted, amount of catalyst inserted, and reaction time) on the production yield of PPD by analyzing the Gas Chromatography (GC). The experimental results demonstrated that PPD was not produced under non-catalyst conditions, and PPD production yield increased with increasing temperature, pressure, amount of catalyst inserted, and reaction time. However, for the reaction temperature case, it was found that 200 .deg. C was the optimal temperature, because thermal degradation of PPD occurred above 250 .deg. C. In addition, we confirmed the structure of PPD and the bonding characteristics of the amine group via FT-IR and H-NMR analysis.

  13. Synthesis and thermal degradation Kinetics of D - (+ - galactose containing polymers

    Directory of Open Access Journals (Sweden)

    Fehmi Saltan

    2013-01-01

    Full Text Available In this study, it is investigated the synthesis and characterizations of polymerizable vinyl sugars. Carbohydrate containing polymers were synthesized via free radical polymerization. Thermal behavior of polymer derivatives was analyzed by using DSC and TG. Molecular weight dispersion of polymer derivatives was also analyzed with GPC. Molecular structures were analyzed by FT-IR and 1H-NMR spectrophotometer. We found that molecular weight of copolymers could effect to the thermal stability. According to TG data related to the copolymers, molecular weight of polymers increased while the thermal stability decreased. Thermogravimetric analysis of polymers also investigated. The apparent activation energies for thermal degradation of carbohydrate containing polymers were obtained by integral methods (Flynn - Wall - Ozawa, Kissinger - Akahira - Sunose, and Tang.

  14. Synthesis and characterization of acrylate copolymer containing fluorescein functional group

    Energy Technology Data Exchange (ETDEWEB)

    Hui, Guodong; Huang, Weiyun; Song, Yunzhao; Chen, Deben; Zhong, Anyong [Sichuan University, Chengdu (China)

    2013-08-15

    We report a novel method to fabricate fluorescent polymer (F-CPA) based on the esterification between acrylate copolymer (CPA) and fluorescein using N, N-dicyclohexylcarbodiimide (DCC)/4-dimethylaminopyridine (DMAP) as catalyst. The resulting copolymer was characterized by Fourier transform-infrared spectroscopy (FT-IR), gel permeation chromatography (GPC), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), ultraviolet-visible spectroscopy (UV-Vis) and fluorescence spectroscopy. In addition, the influences of concentration, solvents, pH and metal cations (Cu{sup 2+}, Fe{sup 3+} and Zn{sup 2+}) on the fluorescent behaviors of F-CPA are discussed in detail. All those observations suggest that the synthesized F-CPA is an excellent luminescent macromolecular material with simple synthesis method and excellent solubility. Moreover, its sensitive fluorescence response behaviors to solvents, pH and metal cations make it to become a polymer-based probe.

  15. Synthesis and characterization of acrylate copolymer containing fluorescein functional group

    International Nuclear Information System (INIS)

    Hui, Guodong; Huang, Weiyun; Song, Yunzhao; Chen, Deben; Zhong, Anyong

    2013-01-01

    We report a novel method to fabricate fluorescent polymer (F-CPA) based on the esterification between acrylate copolymer (CPA) and fluorescein using N, N-dicyclohexylcarbodiimide (DCC)/4-dimethylaminopyridine (DMAP) as catalyst. The resulting copolymer was characterized by Fourier transform-infrared spectroscopy (FT-IR), gel permeation chromatography (GPC), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), ultraviolet-visible spectroscopy (UV-Vis) and fluorescence spectroscopy. In addition, the influences of concentration, solvents, pH and metal cations (Cu"2"+, Fe"3"+ and Zn"2"+) on the fluorescent behaviors of F-CPA are discussed in detail. All those observations suggest that the synthesized F-CPA is an excellent luminescent macromolecular material with simple synthesis method and excellent solubility. Moreover, its sensitive fluorescence response behaviors to solvents, pH and metal cations make it to become a polymer-based probe

  16. Hydroxyapatite-ciprofloxacin delivery system: Synthesis, characterisation and antibacterial activity

    Directory of Open Access Journals (Sweden)

    Ciocilteu Maria-Viorica

    2018-06-01

    Full Text Available The main objective of this study was to synthesize hydroxyapatite-ciprofloxacin composites using a chemical precipitation method and to evaluate the properties and in vitro release profile of the drug from the hydroxyapatite-ciprofloxacin composites. Composite characterization was achieved by FT-IR, XRD and DLS. Ciprofloxacin determination was accomplished by HPLC, resulting in good incorporation efficiency of the drug (18.13 %. The in vitro release study (Higuchi model C = K t1/2 and Ritger-Peppas model, C = K t0.6 showed a diffusion-controlled mechanism. The antibacterial activity showed that the bacterial growth inhibition zones were approximately equal for the synthesis composites and for the mechanical mixture on the Staphylococcus aureus germ.

  17. Molecular structure, vibrational analysis (IR and Raman) and quantum chemical investigations of 1-aminoisoquinoline

    Science.gov (United States)

    Sivaprakash, S.; Prakash, S.; Mohan, S.; Jose, Sujin P.

    2017-12-01

    Quantum chemical calculations of energy and geometrical parameters of 1-aminoisoquinoline [1-AIQ] were carried out by using DFT/B3LYP method using 6-311G (d,p), 6-311G++(d,p) and cc-pVTZ basis sets. The vibrational wavenumbers were computed for the energetically most stable, optimized geometry. The vibrational assignments were performed on the basis of potential energy distribution (PED) using VEDA program. The NBO analysis was done to investigate the intra molecular charge transfer of the molecule. The frontier molecular orbital (FMO) analysis was carried out and the chemical reactivity descriptors of the molecule were studied. The Mulliken charge analysis, molecular electrostatic potential (MEP), HOMO-LUMO energy gap and the related properties were also investigated at B3LYP level. The absorption spectrum of the molecule was studied from UV-Visible analysis by using time-dependent density functional theory (TD-DFT). Fourier Transform Infrared spectrum (FT-IR) and Raman spectrum of 1-AIQ compound were analyzed and recorded in the range 4000-400 cm-1 and 3500-100 cm-1 respectively. The experimentally determined wavenumbers were compared with those calculated theoretically and they complement each other.

  18. LIBS, Raman spectroscopy, and optical microscopy analyses of superficial encrustations on ancient tesserae in Lebanon

    Science.gov (United States)

    Tomkowska, Anna; Chmielewski, Krzysztof; Skrzyczanowski, Wojciech; Mularczyk-Oliwa, Monika; Ostrowski, Roman; Strzelec, Marek

    2017-07-01

    The aim of research was determination of composition and nature of superficial deposits, cumulated at the selected mosaic's tesserae from Lebanon. Selected were three series of objects from different locations, namely from the seaside and mountain archaeological sites as well as from the mosaics exposed in the city center. Analyzed were stone and ceramic tesserae. The selection of objects was dictated by wide diversification of factors influencing the state of preservation and composition of deposits in given location. Investigations were performed including LIBS, FT-IR, Raman spectroscopy and optical 3D microscopy. The experimental results included composition and kind of deposit at the tesserae surfaces, and composition of tesserae itself. Compounds in the superficial deposits were identified. Confirmed was occurrence of different encrustations in dependence on geographic localization of a given sample. The interpretation of results was supported by multivariate statistical techniques, especially by the factor analysis. Performed analyses constitute the pioneer realization in terms of determination of deposits composition at the surface of mosaics from the Lebanon territory.

  19. Synthesis, crystal structure, spectroscopic characterization and nonlinear optical properties of Co(II)- picolinate complex

    Energy Technology Data Exchange (ETDEWEB)

    Tamer, Ömer, E-mail: omertamer@sakarya.edu.tr; Avcı, Davut; Atalay, Yusuf

    2015-11-15

    A cobalt(II) complex of picolinate was synthesized, and its structure was fully characterized by the applying of X-ray diffraction method as well as FT-IR, FT-