WorldWideScience

Sample records for picrates

  1. Enrofloxacinium picrate

    Directory of Open Access Journals (Sweden)

    Jerry P. Jasinski

    2011-02-01

    Full Text Available There is one cation–anion pair in the asymmetric unit of the title compound [systematic name: 4-(3-carboxy-6-fluoro-4-oxo-1,4-dihydroquinolin-7-yl-1-ethylpiperazin-1-ium 2,4,6-trinitrophenolate], C19H23FN3O3+·C6H2N3O7−. The six-membered piperazine group in the cation adopts a slightly distorted chair conformation and contains a protonated N atom. The dihedral angles between the mean planes of the cyclopropyl and piperazine rings in the cation with the 10-atom ring system of the quinolone group are 48.1 (1 and 69.9 (5°, respectively. The picrate anion interacts with the protonated N atom of an adjacent cation through a bifurcated N—H...O three-center hydrogen bond, forming an R12(6 ring motif. Furthermore, there is an intramolecular O—H...O hydrogen bond. The dihedral angle between the mean planes of the anion benzene and cation piperizine, quinoline and cyclopropyl rings are 61.3 (6, 31.1 (4 and 70.4 (9°, respectively. The mean planes of the two o-NO2 and single p-NO2 groups in the picrate anion are twisted by 6.7 (6, 38.3 (9 and 12.8 (7° with respect to the mean plane of the benzene ring. Strong N—H...O and weak intermolecular C—H...O hydrogen bonds in concert with weak π–π stacking interactions [centroid–centroid distances = 3.5785 (13, 3.7451 (12 and 3.6587 (13 Å] dominate the crystal packing.

  2. Propiverinium picrate

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    Jerry P. Jasinski

    2009-08-01

    Full Text Available The title compound [systematic name: 4-(2,2-diphenyl-2-propoxyacetoxy-1-methylpiperidin-1-ium picrate], C23H30NO3+·C6H2N3O7−, crystallizes as a salt with one cation–anion (propiverinium picrate pair in the asymmetric unit. A significant number of conformational changes are observed between the crystalline environment of this cation–anion salt and that of a density functional theory (DFT calculation of the geometry-optimized structure. The angle between the dihedral planes of the two benzyl rings in the propiverinium cation increases by 14.4 (0° from that of the crystalline environment. The dihedral angles between the mean planes of each of the benzyl rings and the mean plane of the piperidine increase by 2.0 (8 and 12.3 (5°. The angles between the mean plane of the acetate group and the mean planes of the interconnected piperidine group and the two benzyl rings decrease by 0.2 (1, 7.4 (6 and 3.2 (2°, respectively. The mean plane of the phenolate group in the anion changes by +22.6 (9, +22.1 (1 and −2.8 (6° from the mean planes of the piperidine and benzyl rings in the cation, respectively. In the crystal, a bifurcated N—H...(O,O hydrogen bond and a weak C—H...π ring interaction help to establish the packing. The two O atoms of the p-NO2 group are disordered with occupancies 0.825 (10:0.175 (10.

  3. Study of the cerium(IV)-picrate system in acetonitrile.

    Science.gov (United States)

    Kratochvil, B; Tipler, M; McKay, B

    1966-07-01

    A potentiometric and spectrophotometric study has been made of the reaction between hexanitratocerate and picrate in dry acetonitrile. Several cerium(IV)-picrate complexes are formed; the formation constant for the first is estimated to be 4 from spectrophotometric measurements. The catalytic effect of picrate on hydroquinone oxidation by nitratocerate is postulated to be due to more rapid electron transfer by cerium picrate complexes.

  4. Structures of acetylcholine picrate and methoxycarbonylcholine picrate hemihydrate

    DEFF Research Database (Denmark)

    Frydenvang, Karla Andrea; Grønborg, L; Jensen, B

    1988-01-01

    Acetylcholine picrate, C7H16NO2+.C6H2N3-O7-, Mr = 374.3, orthorhombic, Pbca, at 105 K: a = 18.799 (4), b = 7.726 (2), c = 22.878 (4) A, V = 3323 (2) A3, Z = 8, Dm(295 K, flotation) = 1.44, D chi(105 K) = 1.496 Mg m-3, mu(Mo K alpha) = 0.120 mm-1, F(000) = 1568, m.p. (hot-stage microscope) 381-382...... neighbours a great number of oxygen atoms. Contacts to the quaternary ammonium group do not seem to be more important than contacts to the acetyl or methoxy-carbonyl moieties. No direct contacts between aromatic rings and quaternary ammonium groups are found....

  5. Synthesis and Characterization of some First Row Transition Metal Picrates

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    R. C. Aggarwal

    1975-10-01

    Full Text Available Transition metal picrates of the empirical compositions Ti(Picrate CI/Sub3, Ti (Picrate/Sub2CI/Sub2, Cr (OH (H/Sub2O/Sub6 (Pierate/Sub2 and M(H/Sub2Ox (Picrate/Sub2 (where M=Mn (II, Fe (II, Co(II, Ni(II, Cu(II and Zn(II and x=4for Cu(II, 8 for Fe(II & 6 for others have been prepared and characterized by elemental analysis, molar conductance, magnetic susceptibility measurements, infrared and electronic spectral studies. Molar conductances and molecular weights of the soluble metal picrates show that TiCI/Sub2 (Picrate/Sub2 is non electrolyte whereas others are 1:2 electrolytes. Magnetic susceptibility and electronic spectral I studies indicate that(II picrate is square planar, whereas those of Cr(III Mn(II0, Fe(II,Co(II and NI(II are spin free octahedral. The infrared spectral studies of the hydrated and anhydrous metal picrates show: (i that phenolic group of the picric acid is involved in bounding with the metals;(ii the water molecules in the hydrated metal picrates coordinated and (iii the-NO/Sub2 groups do not participate in bonding with the metals.

  6. Aquadipicrato(tetraethylene glycolgadolinium(III picrate methanol hemisolvate

    Directory of Open Access Journals (Sweden)

    Hoong-Kun Fun

    2008-09-01

    Full Text Available The asymmetric unit of the title compound [systematic name: aquabis(2,4,6-trinitrophenolato(3,6,9-trioxaundecane-1,11-diolgadolinium(III 2,4,6-trinitrophenolate methanol hemisolvate], [Gd(C6H2N3O72(C8H18O5(H2O](C6H2N3O7·0.5CH4O, contains two crystallographically independent GdIII complex cations with two uncoordinated picrate anions and one methanol molecule. Each GdIII atom has nine coordination sites occupied by five O atoms of tetraethylene glycol as a pentadentate ligand, one O atom of a water molecule and three O atoms of the two picrate anions as bidentate and monodentate ligands. The geometry is distorted tricapped trigonal prismatic. The mean planes of the two coordinated mono- and bidentate picrate ligands to the GdIII center are almost perpendicular to each other, as indicated by the dihedral angles of 89.92 (8 and 86.60 (8° in the two complex cations. The ions are arranged in a two-dimensional network parallel to the ac plane. Short O...O and N...O contacts between the nitro groups, intramolecular C—H...O hydrogen bonds, intermolecular O—H...O, O—H...N and C—H...O hydrogen bonds, and two π–π interactions between benzene rings [centroid–centroid distances = 3.8073 (10–3.9831 (10 Å] are observed. The methanol solvent molecule is disordered over two positions, with site-occupancy factors of ca 0.6 and 0.4.

  7. Effect of particle size on thermal decomposition of alkali metal picrates

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Rui; Zhang, Tonglai, E-mail: ztlbit@bit.edu.cn; Yang, Li; Zhou, Zunning

    2014-05-01

    Graphical abstract: The smaller-sized picrate has greater gas emission than do its larger counterpart. The small size effect reduces the thermal decomposition activation energy, accelerates the reaction rate, and promotes the reaction activity. - Highlights: • Picrates were prepared into three micron sizes by microemulsion synthesis. • Thermal decomposition kinetics and thermodynamics were studied by DPTA and DSC. • Smaller-sized picrate has higher activity and faster reaction rate. • Particle size effect on thermal decomposition kinetics and thermodynamics was revealed. - Abstract: Three alkali metal picrates, KPA, RbPA and CsPA, were prepared into three micron sizes by microemulsion synthesis, and their thermal decomposition behaviors were investigated by DPTA at different temperatures and by DSC at different heating rates. The smaller-sized picrate has greater gas emission and smaller kinetic and thermodynamic parameters than do its larger counterpart. It can be attributed to the decreasing particle size which leads to the high surface energy, the fast mass and heat transfer, and the increasing active sites on the reaction interface. The small size effect and surface effect cause the autocatalysis which reduces the activation energy and promotes the reaction activity. The particle size does not affect the reaction mechanism. However, the picrates with different central alkali metals exhibit different reaction mechanisms even though they are of the same size. This is because the central metal determines the bond energy and consequently affects the stability of picrate.

  8. The hydrothermolysis of the picrate anion: Kinetics and mechanism

    Science.gov (United States)

    Ross, D.S.; Jayaweera, I.

    2002-01-01

    The hydrothermolysis of the picrate anion in aqueous solution has been studied at 260-325??C in liquid water. At starting pH values above 12, the disappearance of picrate begins immediately and is first order in OH-. At lower pH, there is an induction period preceding the disappearance, and over the pH range 6.7-11.9 there is no pH dependence in the developed reaction phase. Added borate and silicate salts promote the reaction, suggesting their acting as nucleophiles at hydrothermal conditions. Nitrite is an initial product, while acetate is a final product and reflective of a vigorous oxidative sequence consuming the intermediate products. A reaction sequence consistent with the results at the lower pH includes initiation of a chain process by displacement of nitrite by water, followed by nucleophilic displacement of nitrite by nitrite such that a nitro group is replaced by an O-N=O group. The ester then rapidly hydrolyzes, and the net reaction is the production of an additional nitrite with each cycle. A simple modeling of this system satisfactorily fits the experimental findings. ?? 2002 Elsevier Science B.V. All rights reserved.

  9. Compounds of lanthanide picrates and 2-azacyclononanone (aza): synthesis, characterization and thermal study

    Energy Technology Data Exchange (ETDEWEB)

    Marinho, E.P.; Araujo Melo, D.M.; Zinner, L.B.; Zinner, K. [UFRN, Natal (Brazil). Dept. de Quimica; Xavier de Matos, J.E. [Departamento de Quimica Organica e Inorganica, UFC, Caixa Postal 12200, CEP 60001-970 Fortaleza CE (Brazil)

    1998-07-24

    Addition compounds between lanthanide(III) picrates and azacyclononanone(aza) were characterized by spectroscopic, microanalytical and X-ray data, with special emphasis on thermogravimetric techniques. (orig.) 10 refs.

  10. Structure and vibrational spectra of L-alanine L-alaninium picrate monohydrate

    Science.gov (United States)

    Ghazaryan, V. V.; Fleck, M.; Petrosyan, A. M.

    2012-05-01

    Preparation, crystal and molecular structure as well as vibrational spectra of the crystal L-alanine L-alaninium picrate monohydrate are described. The title crystal is monoclinic, space group P21. The asymmetric unit contains one dimeric (L-Ala⋯L-Ala+) cation, one picrate anion and a water molecule. The O⋯O distance in the dimeric cation is equal to 2.553(2) Å. The IR and Raman spectra are interpreted based on the structure.

  11. Crystal structure and hydrogen-bonding patterns in 5-fluorocytosinium picrate

    Directory of Open Access Journals (Sweden)

    Marimuthu Mohana

    2017-03-01

    Full Text Available In the crystal structure of the title compound, 5-fluorocytosinium picrate, C4H5FN3O+·C6H2N3O7−, one N heteroatom of the 5-fluorocytosine (5FC ring is protonated. The 5FC ring forms a dihedral angle of 19.97 (11° with the ring of the picrate (PA− anion. In the crystal, the 5FC+ cation interacts with the PA− anion through three-centre N—H...O hydrogen bonds, forming two conjoined rings having R21(6 and R12(6 motifs, and is extended by N—H...O hydrogen bonds and C—H...O interactions into a two-dimensional sheet structure lying parallel to (001. Also present in the crystal structure are weak C—F...π interactions.

  12. Vibrational and third-order nonlinear optical study on hydroxyethylammonium picrate (HEAP) single crystals

    Science.gov (United States)

    Sudharsana, N.; Nagalakshmi, R.; Krishnakumar, V.; Sharma, A.; Fausto, R.; Row, T. N. Guru; Pal, Rumpa

    2012-06-01

    Single crystals of hydroxyethylammonium picrate (C8 H10N4O8; HEAP) have been grown for the first time by slow evaporation solution growth technique at room temperature, using ethanol as solvent. FT-IR and Raman spectra were recorded for HEAP at room temperature. The main vibrational bands related to NH3+ and CO- (picrate) groups, involved in charge transfer, are discussed. Second-order hyperpolarizability(γ) for the single crystal was evaluated theoretically to be 3.48×10-28 e.s.u. A Z-scan study of HEAP showed that the relative third-order nonlinear refractive index is -9.2×10-5cm2/W. The measured third-order nonlinear properties confirm the suitability of the crystal for optical limiting and switching applications.

  13. Helical ternary complexes of alkaline earth picrates with open-chain crown ether

    Institute of Scientific and Technical Information of China (English)

    刘伟生; 温永红; 刘雪原; 谭民裕

    2003-01-01

    Four solid complexes of alkaline earth picrates with N,N,N′,N′-tetraphenyl-3,6,9-tri- oxaundecanediamide (TTD), M (Pic)2TTD (1, M = Mg; 2, M = Ca; 3, M = Sr; 4, M = Ba), have been prepared and characterized by elemental analysis, conductivity measurement, IR spectra, 1H NMR spectra and TG-DTA techniques. Crystal structure of complex 3 shows that the Sr(Ⅱ) ion is 9-coordinated by five oxygen atoms from TTD and four oxygen atoms from two bidentate picrates, and the coordination polyhedron is distorted tricapped trigonal prism. TTD as a pentadentate ligand forms a right-handed helical coordination structure. The chelating helical chain has a relative fixed radius and then shows a high coordination selectivity to metal ion. The high selectivity of TTD to alkaline earth ions is explained elementarily from the special coordination structures.

  14. Mutagenicity Evaluation of Ammonium Picrate in the Ames Salmonella/Microsome Plate Test. Segment Report,

    Science.gov (United States)

    1979-02-01

    Dicentric : A chromosome containing two centromeres. > = Greater than 10 aberrations: A cell which contains more than 10 aberrations. *Scored as "AP" on...Chromatid Deletion Ring Dicentric Chromosome Break Trans locati on Tr radial Quadri radial Translocation I Cong 1ex Rearrangenlent PROTOCOL 1...frequency and dose: SCE/ chromosome = 0.0006 D + 0.303, where D = dose in Pg/ ml, and the correlation factor (r) = 0.88. Therefore, ammonium picrate

  15. Growth and characterization of proficient second order nonlinear optical material: L-asparaginium picrate (LASP)

    Science.gov (United States)

    Saravanan, M.; Senthil, A.; Rajasekar, S. Abraham

    2016-09-01

    Good optical quality, potential second order nonlinear optical crystal L-asparaginium picrate (LASP) was grown by the slow cooling method. The solubility and metastable zone width of LASP specimen was studied. The LASP crystal belongs to monoclinic crystal system with noncentrosymmetric space group P21. UV-Visible-NIR transmittance spectrum determines the optical band gap of LASP. Excellence of the grown crystal is ascertained by the etching studies. Laser Damage Threshold and Photoluminescence studies designate that the grown crystal contains less imperfection. The mechanical behaviour of LASP sample was investigated at different temperatures. The piezoelectric nature, Photoconductive nature and the relative Second Harmonic Generation (for various particle sizes) of the material were also studied. Birefringence and ocular (optical) homogeneity of the crystal were assessed using modified channel spectrum method.

  16. Hydrogen bonding in the crystal structure of the molecular salt of pyrazole-pyrazolium picrate.

    Science.gov (United States)

    Su, Ping; Song, Xue-Gang; Sun, Ren-Qiang; Xu, Xing-Man

    2016-06-01

    The asymmetric unit of the title organic salt [systematic name: 1H-pyrazol-2-ium 2,4,6-tri-nitro-phenolate-1H-pyrazole (1/1)], H(C3H4N2)2 (+)·C6H2N3O7 (-), consists of one picrate anion and one hydrogen-bonded dimer of a pyrazolium monocation. The H atom involved in the dimer N-H⋯N hydrogen bond is disordered over both symmetry-unique pyrazole mol-ecules with occupancies of 0.52 (5) and 0.48 (5). In the crystal, the component ions are linked into chains along [100] by two different bifurcated N-H⋯(O,O) hydrogen bonds. In addition, weak C-H⋯O hydrogen bonds link inversion-related chains, forming columns along [100].

  17. Crystal structures of the complexes of rare earth picrates with N, N, N’, N’-tetraphenyl-3, 6-dioxaoctanediamide

    Institute of Scientific and Technical Information of China (English)

    刘伟生; 柳士霞; 谭民裕; 郁开北; 谭干祖

    1997-01-01

    The complexes of rare earth picrate with N,N,N’,N’-tetraphenyl-3,6-dioxaoctanediamide(TDD),Eu(picc(TDD)] 2CH3CN and [ Y(pic)3(TDD)],have been synthesized.The crystal structures reveal that TDD at is as n tetradentate ligand,forming a ring-like coordination structure with its oxygen atoms together with one oxygen atom of the bidentate pterate In the Eu(Ⅲ) complex,the europium ion with a larger ionic radius lies out of the ring,while in the Y(Ⅲ) complex,the yttrium ion with a smaller ionic radius enters the cavity of the ligand.The structures of the complexes are greatly affected by the ionic radii due to participation of the picrates in coordination.

  18. Crystal structure of a second triclinic polymorph of 2-methylpyridinium picrate

    Directory of Open Access Journals (Sweden)

    Jeganathan Gomathi

    2015-11-01

    Full Text Available The title molecular salt, C6H8N+·C6H2N3O7− (systematic name: 2-methylpyridinium 2,4,6-trinitrophenolate, crystallizes with two cations and two anions in the asymmetric unit. In the crystal, the cations are linked to the anions via bifurcated N—H...(O,O hydrogen bonds, generating R12(6 graph-set motifs. Numerous C—H...O hydrogen bonds are observed between these cation–anion pairs, which result in a three-dimensional network. In addition, weak aromatic π–π stacking between the 2-methylpyridinium rings [inter-centroid distance = 3.8334 (19 Å] and very weak stacking [inter-centroid distance = 4.0281 (16 Å] between inversion-related pairs of picrate anions is observed. The title salt is a second triclinic polymorph of the structure (also with Z′ = 2 reported earlier [Anita et al. (2006. Acta Cryst. C62, o567–o570; Chan et al. (2014. CrystEngComm, 16, 4508–4538]. In the title compound, the cations and anions display a chequerboard arrangement when viewed down [100], whereas in the first polymorph, (010 layers of alternating cations and anions are apparent in a [100] view. It is interesting that the unit-cell lengths are almost identical for the two polymorphs, although the inter-axial angles are quite different.

  19. Structural, thermal, optical and nonlinear optical properties of ethylenediaminium picrate single crystals

    Science.gov (United States)

    Indumathi, C.; T. C., Sabari Girisun; Anitha, K.; Alfred Cecil Raj, S.

    2017-07-01

    A new organic optical limiting material, ethylenediaminium picrate (EDAPA) was synthesized through acid base reaction and grown as single crystals by solvent evaporation method. Single crystal XRD analysis showed that EDAPA crystallizes in orthorhombic system with Cmca as space group. The formation of charge transfer complex during the reaction of ethylenediamine and picric acid was strongly evident through the recorded Fourier Transform Infra Red (FTIR), Raman and Nuclear Magnetic Resonance (NMR) spectrum. Thermal (TG-DTA and DSC) curves indicated that the material possesses high thermal stability with decomposition temperature at 243 °C. Optical (UV-Visible-NIR) analysis showed that the grown crystal was found to be transparent in the entire visible and NIR region. Z-scan studies with intense short pulse (532 nm, 5 ns, 100 μJ) excitations, revealed that EDAPA exhibited two photon absorption behaviour and the nonlinear absorption coefficient was found to be two orders of magnitude higher than some of the known optical limiter like Cu nano glasses. EDAPA exhibited a strong optical limiting action with low limiting threshold which make them a potential candidate for eye and photosensitive component protection against intense short pulse lasers.

  20. Growth and structural analysis of an organic NLO compound: L-lysinium picrate

    Science.gov (United States)

    Arthi, D.; Ilango, E.; Mercina, M.; Jayaraman, D.; Joseph, V.

    2017-01-01

    L-lysinium picrate (LLP), an organic material, has been synthesized and grown by solution growth method. The crystal structure of the grown material was solved by single crystal X-ray diffraction analysis and it was found that the material belongs to triclinic system with space group P1. The transmission range of the crystal was measured in the range of 470-1100 nm with lower cut off wavelength at 470 nm using UV-vis-NIR absorption spectrum. The optical band gap of the grown material was found to establish the dielectric behavior of the material. The main functional groups present in the material were identified using FTIR spectral analysis. Thermal stability and decomposition range were studied by means of TGA and DTA analyses. The microstructure of the grown crystal was studied using SEM analysis. The various chemical environments of the protons and carbons were studied by 1H and 13C NMR spectroscopy to confirm the molecular structure of the grown crystal. NLO behavior was confirmed by Kurtz and Perry technique and SHG efficiency was estimated as 1.4 times that of standard KDP.

  1. Investigation on growth and characterization of imidazolium picrate: An organic salt

    Science.gov (United States)

    Anandhi, S.; Shyju, T. S.; Srinivasan, T. P.; Gopalakrishnan, R.

    2011-11-01

    Organic crystal of imidazolium picrate (IP) was synthesized and successfully grown by the slow cooling solution growth method using ethanol and acetone as solvents. The structural, thermal, optical and mechanical properties were studied for the grown crystal. Cell parameters were determined using X-ray diffraction studies. HRXRD study shows the crystalline perfection. FT-IR and laser Raman studies confirm the functional groups present in the title material. The optical properties such as optical bandgap and refractive index of the title material were obtained from the UV-visible spectrum. The PL spectrum of the title compound shows green emission. The thermal stability of the crystal has been determined using TG/DTA studies. Vicker's microhardness studies were carried out to understand the mechanical properties of the grown crystal. The hardness of the title compound increases on increasing the load. Theoretical factor group analysis enumerates the possible modes of vibrations. The dielectric tensor, dielectric loss and conductivity over a range of frequencies and temperatures have been presented. Dielectric tensor components have been determined theoretically using the DFT theory.

  2. Growth, spectral, dielectric and antimicrobial studies on 4-piperidinium carboxylamide picrate crystals

    Science.gov (United States)

    Dhanabal, T.; Tharanitharan, V.; Amirthaganesan, G.; Dhandapani, M.

    2014-07-01

    Single crystal of 4-piperidinium carboxylamide picrate was grown by slow evaporation solution growth technique at ambient temperature. The average dimensions of grown crystal were 0.7 × 0.3 × 0.2 cm3. The solubility of the compound was analyzed using methanol and acetone. Optical property of the compound was ascertained by UV-visible absorption spectral study. The sharp and well defined Bragg peaks observed in the powder X-ray diffraction pattern confirm its crystallinity. The different kinds of protons and carbons in the compound were confirmed by 1H and 13C NMR spectral analyses. The presence of various functional groups in the compound was assigned through polarized Raman spectral study. The mechanical property of the crystal was measured by Vicker's microhardness test and the compound was found to be soft material. The dielectric constant and dielectric loss of the crystal decrease with increase in frequency. The antibacterial and antifungal activities of the crystal were studied by disc diffusion method and found that the compound shows good inhibition efficiency against various bacteria and fungi species.

  3. Synthesis, crystal structure, crystal growth and physical properties of N,N-diethyl anilinium picrate

    Science.gov (United States)

    Subramaniyan @ Raja, R.; Anandha Babu, G.; Ramasamy, P.

    2011-11-01

    Crystalline substance of N,N-diethyl anilinium picrate (NNDEAP) has been synthesized and single crystals of NNDEAP were successfully grown for the first time by the slow evaporation solution growth technique at room temperature with dimensions 14×10×10 mm3. The formation of the new crystal has been confirmed by single crystal X-ray diffraction studies. The structural perfection of the grown crystal was analyzed by high resolution X-ray diffraction (HRXRD) measurements. The functional groups of NNDEAP have been identified by Fourier transform infrared spectral studies. Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) have also been carried out and the thermal behavior of NNDEAP has been studied. The UV-vis-NIR studies have been carried out to identify the optical transmittance and the cut off wavelength of NNDEAP is identified. The dielectric loss and the dielectric constant as a function of frequency and temperature were measured for the grown crystal and the nature of variation of dielectric constant εr and dielectric losses (tan δ) were studied. Vicker's hardness test has been carried out on NNDEAP to measure the load dependent hardness. The laser induced surface damage threshold for the grown crystal was measured using Nd:YAG laser.

  4. Synthesis, structure, thermal and NLO characterization of 4-hydroxy tetramethylpiperazinium picrate crystals

    Indian Academy of Sciences (India)

    T Dhanabal; G Amirthaganesan; M Dhandapani; Samar K Das

    2012-07-01

    Good quality single crystals of 4-hydroxy tetramethylpiperazinium picrate (TMPP) were grown by slow evaporation solution growth method at room temperature. The average dimensions of the grown crystals were 0.6 × 0.2 × 0.2 cm3. The solubility of the compound was estimated using methanol and acetone. The elemental analysis confirms the formation of the compound in the stoichiometric proportion. The UV-visible transmittance study indicates that the crystal possesses minimum transmittance at 370 nm and no absorption at 470-900 nm. The Bragg peaks obtained in the powder X-ray diffraction pattern confirm its crystallinity. The thermal behaviour of the crystal was investigated using thermogravimetric (TG) and differential thermal analysis (DTA) techniques. The structure of the compound was determined by using single crystal X-ray diffraction method. The compound was found to be crystallize in the monoclinic space group P2(1)/c (a = 6.9513(8)Å, b = 11.8016(14)Å, c = 22.018(2)Å, = 90.00°, = 92.575(2)°, = 90.00°). The thermal anomalies observed in the differential scanning calorimetry (DSC) heating and cooling cycles indicate the occurrence of first order phase transition. Fourier transform infrared (FTIR) and polarized Raman spectral analyses were used to confirm the presence of various functional groups in the compound. The nonlinear optical property (NLO) of the crystal was analysed by Kurtz-Perry powder technique and found that the compound has SHG efficiency 1.5 times greater that of potassium dihydrogen phosphate (KDP).

  5. Molecular Design of Crown Ethers.22.Synthesis of Benzocrown Ether Derivatives and Their Solvent Extraction with Univalent/Bivalent Metal Picrates

    Institute of Scientific and Technical Information of China (English)

    YANG,Ying-Wei(杨英威); LI,Chun-Ju(李春举); ZHANG,Heng-Yi(张衡益); LIU,Yu(刘育)

    2004-01-01

    Three novel benzocrown ether derivatives have been synthesized and their cation binding behavior with uniand bi-valent metal ions was evaluated by the solvent extraction of aqueous metal picrates. The obtained results indicate that the size-fit of crown ether and metal cation, and electron effect of the side arm attached to benzocrown ethers affect their cation binding ability and selectivity.

  6. Synthesis, structural and spectral characterization of a novel NLO crystal N,N‧-diphenylguanidinium picrate: diacetone solvate

    Science.gov (United States)

    Shanmugavadivu, T.; Dhandapani, M.; Naveen, S.; Lokanath, N. K.

    2017-09-01

    An organic NLO active material N,N‧-diphenylguanidinium picrate: diacetone solvate (C13H14N3+. C6H2N3O7-. 2C3H6O) (DPGPD) was synthesized and single crystals were grown by slow evaporation-solution growth technique at room temperature. DPGPD crystallizes in monoclinic crystal system with noncentrosymmetric space group, Cc confirmed by single crystal X-ray diffraction analysis. The presence of various functional groups was identified from FT-IR spectral analysis and the proton transfer during the formation of compound was confirmed by NMR spectroscopic techniques. The thermal stability was investigated by TG/DTA analyses. Optical transmittance was measured by UV-Vis-NIR spectroscopy and band gap energy was calculated. Photoluminescence spectrum was used to explore its applicability towards laser diodes. Dielectric property of the material was ascertained at different temperatures and it is found that the grown crystal has higher dielectric constant in low frequencies. Photoconductivity study revealed that DPGPD exhibits positive photoconductivity. SHG property was found to be 0.6 times higher than that of KDP.

  7. Studies on growth and characterization of a novel nonlinear optical and ferroelectric material - N,N-dimethylurea picrate single crystal

    Science.gov (United States)

    Shanthi, A.; Krishnan, C.; Selvarajan, P.

    2014-05-01

    A novel organic nonlinear optical (NLO) material viz. N,N-dimethylurea picrate (NNDMP) was grown by the slow evaporation technique using N,N-dimethyl formamide as a solvent. The solubility of the grown sample has been estimated for various temperatures. The XRD study reveals that the grown crystal crystallizes in the monoclinic crystal system and the corresponding lattice parameters were determined. The relative second harmonic generation (SHG) efficiency of the NNDMP was found to be 1.045 times that of KDP by Kurtz-Perry powder technique. FTIR and FT-Raman spectral analyses explain the various functional groups present in the sample. The optical spectral analysis of the grown crystal has been performed by UV-vis-NIR spectroscopy and the band gap energy was found out. The thermogravimetric analysis and differential thermal analysis (TG/DTA) reveal that the NNDMP crystal is stable at up to 172 °C. A prominent first-order ferroelectric to paraelectric phase transition at 323 K has been observed and activation energy was determined for the AC conduction process in the sample.

  8. Investigations on critical parameters, growth, structural and spectral studies of beta-alaninium picrate (BAP) single crystals

    Science.gov (United States)

    Shanthi, D.; Selvarajan, P.; Perumal, S.

    2014-12-01

    Beta-alaninium picrate (BAP) salt has been synthesized and the solubility of the synthesized sample in double distilled water was determined at different temperatures. Solution stability was studied by observing the metastable zone width by employing the polythermal method. Induction period values for different supersaturation ratios at room temperature were determined based on the isothermal method. The nucleation parameters such as critical radius, critical free energy change, interfacial tension, and nucleation rate have been estimated for BAP salt on the basis of the classical nucleation theory. The lattice parameters of the grown BAP crystal were determined using the x-ray diffraction (XRD) technique. The reflection planes of the sample were confirmed by the powder XRD study and diffraction peaks were indexed. Fourier transform infrared spectroscopy and Fourier transform-Raman studies were used to confirm the presence of various functional groups in the BAP crystal. The nonlinear optical property of the grown crystal was studied using the Kurtz-Perry powder technique. UV-visible spectral studies were carried out to understand optical transparency and the type of band gap of the grown BAP crystal.

  9. Fabrication of optical element from unidirectional grown imidazole-imidazolium picrate monohydrate (IIP) organic crystals for nonlinear optical applications

    Science.gov (United States)

    Vivek, P.; Murugakoothan, P.

    2014-12-01

    Nonlinear optical bulk single crystal of Imidazole-imidazolium picrate monohydrate (IIP) has been grown by Sankaranarayanan-Ramasamy (SR) method using acetonitrile as solvent. First time we report the bulk growth of IIP crystal by SR method. The transparent IIP single crystal of maximum diameter 21 mm and length 46 mm was obtained by employing SR method. The grown crystal was subjected to high resolution X-ray diffraction, UV-vis-NIR transmittance, refractive index, hardness, dielectric and laser damage threshold studies. The crystalline perfection of the grown crystal was analyzed using HRXRD. Cut off wavelength and optical transmission window of the crystal was assessed by UV-vis-NIR and the refractive index of the crystal was found. The mechanical property of the crystal was estimated by Vicker's hardness test. The dielectric property of the crystal was measured as a function of frequency. The laser damage threshold value was determined. The particle size dependent second harmonic generation efficiency for IIP was evaluated with standard reference material potassium dihydrogen phosphate (KDP) by Kurtz-Perry powder method using Nd:YAG laser, which established the existence of phase matching. The second harmonic generation (SHG) of IIP crystal was investigated by the SHG Maker fringes technique. The mechanism of growth is revealed by carrying out chemical etching using acetonitrile as etchant.

  10. Synthesis, Crystal Growth and Characterization of bis Dl-Valine Picrate Single Crystal for Second-Order Nonlinear Optical Applications

    Science.gov (United States)

    Silambarasan, A.; Krishna Kumar, M.; Sudhahar, S.; Thirunavukkarasu, A.; Mohan Kumar, R.; Umarani, P. R.

    2013-08-01

    An organic compound Bis DL-Valine picrate (BDLVP) was synthesized successfully and single crystal was grown by slow evaporation solution growth method. The presence of functional groups in the compound was identified by FTIR spectral analysis. Single crystal X-ray diffraction study revealed that the grown crystal belongs to P21/n space group of monoclinic crystal system. Powder X-ray diffraction pattern was recorded to know the crystalline perfection of the grown crystal. The reaction mechanism, thermal decomposition stages and thermal stability of the grown crystal were studied by using TG/DTA analysis. From the UV-visible spectral study, the electronic band gap energy (Eg) of the grown crystal was found to be 2.43 eV. The second harmonic generation (SHG) efficiency of grown crystal was found to be 1.3 times higher than KDP crystal by using Kurtz powder SHG technique. The microhardness property of the grown crystal was examined by Vicker's microhardness test.

  11. Extraction equilibria of various metal picrates with 19-crown-6 between benzene and water. Effect of the extra methylene group on extraction ability and selectivity.

    Science.gov (United States)

    Katsuta, S; Kanazawa, M; Takeda, Y; Ouchi, M

    1999-07-12

    The overall extraction equilibrium constants (K(ex)) of picrates of Li(+), Na(+), K(+), Rb(+), Cs(+), Ag(+), Tl(+), and Sr(2+)with 19-crown-6 (19C6) were determined between benzene and water at 25 degrees C. The K(ex) values were analyzed into the constituent equilibrium constants, i.e. the extraction constant of picric acid, the distribution constant of the crown ether, the formation constant of the metal ion-crown ether complex in water, and the ion-pair extraction constant of the complex cation with the picrate anion. The effects of an extra methylene group of 19C6 on the extraction ability and selectivity are discussed in detail by comparing the constituent equilibrium constants of 19C6 with those of 18-crown-6 (18C6). The K(ex) value of 19C6 for each metal ion is lower than that of 18C6, which is mostly attributed to the higher lipophilicity of 19C6. The extraction ability of 19C6 for the univalent metal ions decreases in the order Tl(+)>K(+)>Rb(+)>Ag(+)>Cs(+)>Na(+)Li(+), which is the same as that observed for 18C6. The difference in logK(ex) between the univalent metals is generally smaller for 19C6 than for 18C6. The extraction selectivity of 19C6 is governed by the selectivity in the ion-pair extraction, whereas that of 18C6 depends on both the selectivities in the ion-pair extraction and in the complexation in water.

  12. Crystal growth, perfection, linear and nonlinear optical, photoconductivity, dielectric, thermal and laser damage threshold properties of 4-methylimidazolium picrate: an interesting organic crystal for photonic and optoelectronic devices

    Science.gov (United States)

    Rajesh, K.; Arun, A.; Mani, A.; Praveen Kumar, P.

    2016-10-01

    The 4-methylimidazolium picrate has been synthesized and characterized successfully. Single and powder x-ray diffraction studies were conducted which confirmed the crystal structure, and the value of the strain was calculated. The crystal perfection was determined by a HRXR diffractometer. The transmission spectrum exhibited a better transmittance of the crystal in the entire visible region with a lower cut-off wavelength of 209 nm. The linear absorption value was calculated by the optical limiting method. A birefringence study was also carried out. Second and third order nonlinear optical properties of the crystal were found by second harmonic generation and the z-scan technique. The crystals were also characterized by dielectric measurement and a photoconductivity analyzer to determine the dielectric property and the optical conductivity of the crystal. The laser damage threshold activity of the grown crystal was studied by a Q-switched Nd:YAG laser beam. Thermal studies established that the compound did not undergo a phase transition and was stable up to 240 °C.

  13. Synthesis and Structure of a Ternary Copper(II) Complex with Mixed Ligands of Diethylenetriamine and Picrate: DNA/Protein-Binding Property and In Vitro Anticancer Activity Studies.

    Science.gov (United States)

    Shi, Ya-Ning; Zheng, Kang; Zhu, Ling; Li, Yan-Tuan; Wu, Zhi-Yong; Yan, Cui-Wei

    2015-05-01

    Based on the importance of the design and synthesis of transition metal complexes with noncovalent DNA/protein-binding abilities in the field of metallo pharmaceuticals, a new mononuclear ternary copper(II) complex with mixed ligands of diethylenetriamine (dien) and picrate anion (pic), identified as [Cu(dien)(pic)](pic), was synthesized and characterized by elemental analysis, molar conductivity measurement, infrared spectrum, electronic spectral studies, and single-crystal X-ray diffractometry. The structure analysis reveals that the copper(II) complex crystallizes in the monoclinic space group P21 /c, and the copper(II) ion has a distorted square pyramidal coordination geometry. A two-dimensional supramolecular structure is formed through hydrogen bonds. The DNA/bovine serum albumin (BSA)-binding properties of the complex are explored, indicating that the complex can interact with herring sperm DNA via intercalation mode and bind to BSA responsible for quenching of tryptophan fluorescence by static quenching mechanism. The in vitro anticancer activity shows that the copper(II) complex is active against the selected tumor cell lines.

  14. Synthesis, spectroscopic (UV-Vis, FT-IR and NMR), single crystal XRD of 3,5-diethyl -2,6-di(thiophen-2-yl)piperidin-4-on-1-ium picrate: A comprehensive experimental and computational study

    Science.gov (United States)

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

    2017-01-01

    A piperidin-4-one containing picrate 3,5-diethyl -2,6-di(thiophen-2-yl)piperidin-4-on-1-ium picrate [3,5-DPPP] was synthesized. The molecular structure of 3,5-DPPP was confirmed by FT-IR, NMR, Uv-Vis, single crystal XRD analysis and DFT and HF methods with 6-31G(d,p) basis set. The XRD data confirm the transfer of protons from picric acid (O2) to piperidin-4-one ring (N1). The 3,5-DPPP compound is stabilized by the presence of intermolecular and intramolecular hydrogen bonds (N-H⋯O, C-H⋯S and C-H⋯O). Density functional theory and HF calculations have been used widely for calculating a wide variety of molecular properties such as optimized structure, FT-IR and Uv-Vis spectra, and provided reliable results which are in agreement with experimental data. The charge density data have been used to understand the properties of molecular systems. Furthermore, several quantum chemical insights have been obtained in the form of the total and partial density of states, the HOMO-LUMO energy gap and electrostatic potential map etc. In addition, the polarizability and first hyperpolarizability were calculated to show the potential applications of 3,5-DPPP in nonlinear optics.

  15. Extraction of Sodium Picrate by 3m-Crown-m Ethers and Their Monobenzo Derivatives (m = 5, 6 into Benzene: Estimation of Their Equilibrium-Potential Differences at the Less-Polar Diluent/Water Interface by an Extraction Method

    Directory of Open Access Journals (Sweden)

    Yoshihiro Kudo

    2016-01-01

    Full Text Available Individual distribution constants (KD,A of picrate ion (Pic− and extraction constants (Kex± of NaPic by some crown ethers (L into benzene (Bz at 25°C were calculated from data reported previously. These constants were defined as KD,Pic=Pic-o/[Pic-] and Kex±=NaL+oPic-o/(Na+Lo[Pic-], respectively. Here, the subscript “o” denotes an organic (o phase and practically o = Bz. 15-Crown-5 ether (15C5, 18-crown-6 one (18C6, and their monobenzo (B derivatives (B15C5 and B18C6 were selected as L. Interfacial equilibrium-potential differences (Δϕeq at extraction were estimated at 298 K. A plot of log⁡Kex± versus -Δϕeq for the four L extraction systems gave a straight line with slope = 84 V−1. This slope was compared with those, reported before, of the dichloromethane (DCM, 1,2-dichloroethane (DCE, and nitrobenzene (NB extraction systems. The slopes of the regression lines were in the order NB < DCM ≤ DCE < Bz. Also, the individual distribution constants of the complex ion NaL+ and an ion-pair complex (NaL+Pic- into Bz phase were calculated from the above extraction data. At least, a comparison between these values suggests that Bz molecules mainly interact with NaL+ moiety of NaL+Pic-.

  16. Crystal structures of 2-amino-4,4,7,7-tetramethyl-4,5,6,7-tetrahydro-1,3-benzothiazol-3-ium benzoate and 2-amino-4,4,7,7-tetramethyl-4,5,6,7-tetrahydro-1,3-benzothiazol-3-ium picrate

    Directory of Open Access Journals (Sweden)

    Belakavadi K. Sagar

    2017-09-01

    Full Text Available In both 2-amino-4,4,7,7-tetramethyl-4,5,6,7-tetrahydro-1,3- benzothiazol-3-ium benzoate, C11H19N2S+·C7H5O2−, (I, and 2-amino-4,4,7,7-tetramethyl-4,5,6,7-tetrahydro-1,3-benzothiazol-3-ium picrate (2,4,6-trinitrophenolate, C11H19N2S+·C6H2N3O7−, (II, the cations are conformationally chiral as the six-membered rings adopt half-chair conformations, which are disordered over two sets of atomic sites giving approximately enantiomeric disorder. For both cations, the bond lengths indicate delocalization of the positive charge comparable to that in an amidinium cation. The bond lengths in the picrate anion in (II are consistent with extensive delocalization of the negative charge into the ring and onto the nitro groups, in two of which the O atoms are disordered over two sets of sites. In (I, the ionic components are linked by N—H...O hydrogen bonds to form a chain of rings, and in (II, the N—H...O hydrogen bonds link the components into centrosymmetric four-ion aggregates containing seven hydrogen bonded rings of four different types.

  17. 1-Methyl-3-(2-oxo-2H-chromen-3-yl-1H-imidazol-3-ium picrate

    Directory of Open Access Journals (Sweden)

    Nguyen Van Tuyen

    2013-06-01

    Full Text Available The title salt, C13H11N2O2+·C6H2N3O7−, is the unexpected product of a domino reaction of 3-cyanomethyl-1-methylimidazolium chloride with salicylic aldehyde in the presence of picric acid. In the cation, the 1H-imidazole ring is twisted by 63.2 (1° from the 2H-chromen plane. In the crystal, cations and anions are alternately stacked along the a axis through π–π stacking interactions between the almost parallel aromatic rings [centroid–centroid distances = 3.458 (2 and 3.678 (2 Å]. The stacks are further linked by C—H...O hydrogen bonds into a two-tier layer parallel to (001.

  18. Qualitative Assessment of the Ignition of Highly Flammable Fuels by Primary Explosives,

    Science.gov (United States)

    1983-06-01

    primary explosives used in the investigation are listed below:- basic lead azide lead azide lead styphnate barium styphnate potassium picrate lead...in Bakelite Tubes Basic Lead Azide w Lead Styphnate LDNR Barium Styphnate I Flash Composition Potassium Picrate I TABLE 3 IGNITION OF HEXANE SOAKED...Flammability Nichrome Bridgewire in Aluminium Tube Potassium Picrate X LDVR X Barium Styphnate X Tetracene X 200 mq Lead Styphnate X 400 mq Lead

  19. Synthesis and Structure Identification of Related Substance D Picrate of Dextromethorphan Hydrobromide%氢溴酸右美沙芬有关物质D苦味酸盐的合成及结构确证

    Institute of Scientific and Technical Information of China (English)

    王宏博; 郭卫锋; 周后元

    2016-01-01

    为了控制氢溴酸右美沙芬质量,合成分离了欧洲药典7.4版收载的有关物质D:3-甲氧基-17-甲基-(9α,13α,14β)-吗啡喃;为便于质控称量和贮藏,制备了有关物质D的苦味酸盐,其结构经MS、1H NMR、13C NMR和X-射线单晶衍射确证.

  20. Synthesis and Properties of 4-Amino-1,2,4-triazole Picrate%4-氨基-1,2,4-三唑苦味酸盐的合成与性能

    Institute of Scientific and Technical Information of China (English)

    夏云霞; 王平; 孙杰; 董海山

    2008-01-01

    以4-氨基-1,2,4-三唑和苦味酸为原料合成了含能化合物4-氨基-1,2,4-三唑苦味酸盐(4-ATPA),其结构经元素分析、FTIR、MS和1HNMR表征.在甲醇和乙醇溶液中获得了两种不同显微形貌的4-ATPA晶体,SEM分析表明,它们分别为长柱形和椭球形,XRD及DSC分析表明它们的晶型相同.X射线单晶衍射计算得到晶体密度为1.720 g/cm3.经测定,4-ATPA的部分热性能及机械感度为:熔点195.26 ℃,400 ℃下不分解,真空安定性实验(VST)0.16 mL·g-1(120 ℃,48 h),失重(TG)0.14%(120 ℃,48 h);撞击感度为4%、摩擦感度为0%(90°)、特性落高H50=87.4 cm(5 kg落锤),均优于TNT,静电火花感度V50=3.909 kV,E50=0.233 J,与环三亚甲基三硝胺(RDX)相当,5 s爆发点360 ℃,1 000 s临界温度251 ℃.结果表明:4-ATPA有良好的综合热稳定性和较低的机械感度,是一种综合性能优良的炸药.

  1. Crystal Structure of Energetic Compound 4-Amino-1,2,4-triazolium Picrate%含能化合物4-氨基-1,2,4-三唑苦味酸盐的晶体结构

    Institute of Scientific and Technical Information of China (English)

    夏云霞; 王平; 孙杰; 毛志华

    2010-01-01

    在甲醇溶液中培养了化合物4-氨基-1,2,4-三唑苦味酸盐的单晶.该化合物属于正交晶系,Pcnb空间群,晶体学参数如下: a=9.177(4),b=13.279(6),c=19.855(6) (A),V=2419.5(16)(A)~3,Dc=1.720 g·cm~(-3),Z=8,μ(MoKα)=0.152 mm~(-1) ,F(000)=1280.在2580 个点中有2194 个独立衍射点(R_(int)=0.0048),R=0.0588,wR=0.1370,I>2σ(I).通过X射线单晶衍射得到该化合物结构中包含一个4-氨基-1,2,4-三唑阳离子和一个苦味酸阴离子.

  2. Streptomycin interference in Jaffe reaction - Possible false positive creatinine estimation in excessive dose exposure

    DEFF Research Database (Denmark)

    Syal, Kirtimaan; Srinivasan, Anand; Banerjee, Dibyajyoti

    2013-01-01

    Objectives: To study the potential of commonly used aminoglycoside antibiotics to form non-creatinine chromogen with alkaline picrate reagent. Design and methods: We studied the non-creatinine chromogen formation of various concentrations of streptomycin, amikacin, kanamycin, netilmicin, gentamicin...

  3. CMP(O) tripodands: synthesis, potentiometric studies and extractions

    NARCIS (Netherlands)

    Reinoso-Garcia, Marta M.; Janczewski, Dominik; Reinhoudt, David N.; Verboom, Willem; Malinowska, Elzbieta; Pietrzak, Mariusz; Hill, Clement; Baca, Jiri; Gruner, Bohumir; Selucky, Pavel; Gruttner, Cordula

    2006-01-01

    Ligand systems containing three carbamoylmethylphosphonate (CMP) or -phosphine oxide (CMPO) moieties attached to a tripodal platform have been synthesized for metal complexation and subsequent extraction from HNO3 solutions. The incorporation into ion selective electrodes (ISE) and picrate extractio

  4. THz+X Seedling Report

    Science.gov (United States)

    2005-11-23

    Tri Nitro Napthalene Lead Styphnate Tetryl - 5 - Ammonium Picrate Nitroxylene DDNP Nitrocellulose Gun Cotton (Nitrocellulose) Haleite...Nitrogranidine DEGN EDDN BTN PETN Ammonuim Perchlorate Potassium Nitrate Sodium Nitrate Barium Nitrate Strontium Nitrate Silver Nitrate Lead

  5. On the Failure of Correlating Partitioned Electrostatic Surface Potentials Using Bader’s Atoms-in-Molecules Theory to Impact Sensitivities

    Science.gov (United States)

    2013-04-01

    thus allowing researchers to efficiently and safely screen candidate materials and focus synthesis efforts on the most promising compounds. While...Methyl picrate 192 (37) 3-nitro-1,2,4- triazole -5-one NTO 291 (37) 3 3. Results and Discussion Inspired by the work of Murray et al. (12) and Rice...functional theory Methyl picrate 2-methoxy-1,3,5-trinitrobenzene NQ nitroguanidine NTO 3-nitro-1,2,4- triazole -5-one PBE Perdew, Burke, and Ernzerhof

  6. Synthesis, characterization and antibacterial activity of new complexes of some lanthanide ions with 15-crown-5 and 18-crown-6

    Directory of Open Access Journals (Sweden)

    Hussein Al-Amery

    2016-05-01

    Full Text Available Complexes of some lanthanide picrates (Ln3+ = Pr3+, Nd3+ and Dy3+ with 15-crown-5 and 18-crown-6 were synthesized and characterized by elemental analysis, ICP-AES, FTIR, 1H-NMR, 13C-NMR and UV-Visible spectrophotometric methods, thermal analysis (TGA & DTG, magnetic susceptibility , molar conductance and melting points. Also an in-vitro study on pathogenic gram positive (Staphylococcus aureus and pathogenic gram negative bacteria (Escherichia coli, Salmonella and pseudomonas aeruginosa was performed and the results were compared to those of a broad spectrum antibiotic (Chloramphinicol. The complexes of 15-crown-5 have the general formula [Ln(15C52(Pic]Pic2.nH2O where (Ln3+ = Nd3+ and Dy3+, (Pic = Picrate anion and (n = 2 or 4 except for Pr3+ complex which has the formula [Pr(15C5]Pic3.H2O , the 18-crown-6 complexes have the general formula [Ln(18C6]Pic3 where (Ln3+ = Pr3+ and Nd3+ except for Dy3+ complex which has the formula [Dy(18C6(Pic]Pic2.3H2O. In 15-crown-5 complexes both Nd3+ and Dy3+ were coordinated with two 15-crown-5 ligands and one picrate anion through its phenolic oxygen and the oxygen of it’s ortho nitro group, except for Pr3+ which was coordinated with only one 15-crown-5 ligand leaving three picrate anions as counter ions. In 18-crown-6 complexes both Pr3+ and Nd3+ were coordinated with one 18-crown-6 ligand leaving all the three picrate anions as counter ions outside the coordination sphere, except for the Dy3+ complex which was coordinated with one 18-crown-6 ligand and one picrate anion.

  7. Individual extraction constants of some univalent anions in the two-phase water-phenyltrifluoromethyl sulfone system.

    Science.gov (United States)

    Makrlík, Emanuel; Selucký, Pavel; Vaňura, Petr

    2011-12-01

    From extraction experiments and g-activity measurements, the extraction constants corresponding to the general equilibrium Cs+(aq) + A- (aq) Cs+(org) + A- (org) taking place in the two-phase water-phenyltrifluoromethyl sulfone (FS 13) system (A-= I-, ClO4-, MnO4-, Br-3, I-3, picrate, tetraphenylborate (BPh-4); aq = aqueous phase, org = FS 13 phase) were evaluated. Furthermore, the individual extraction constants of these 7 anions in the mentioned two-phase system were calculated; they were found to increase in the series of I-< ClO4- < Br-3 < MnO4-, picrate < I-3 < BPh-4.

  8. A new bile acid-derived lariat-ether: Design, synthesis and cation binding properties

    Indian Academy of Sciences (India)

    P Babu; Uday Maitra

    2003-10-01

    A new chola lariat ether (1, a 21-crown-6) was constructed from readily available precursors. The association constant of compound 1 with alkali metal picrates was measured using Cram’s extraction protocol. Evidence is presented for the involvement of the 3-methoxy group for the complexation. Energy minimised structures show that the A-ring gets slightly distorted upon metal ion binding.

  9. Installation Restoration General Environmental Technology Development. Task 3. Guidelines for In-Place Closure of Dry Lagoons. Volume 2. Evaluation of In-Place Closure Technologies.

    Science.gov (United States)

    1984-01-01

    Nitroqlycerine Tr itonal Ammonia picrate PETN U DMH Am Ito I An ilin e Nitt ouenzene barium nitrate Lead azide Lead styphnate Acid s Ammronium nitrate Lead * Zinc...temperature for RDX, 1MX, lead styphnate , and lead azilde thermal decomposition 305 65 Time versus temperature for NG, NC, NQ, and NH 4NO 3 thermal

  10. Structural Feature and Molecular Interaction of Basic Amino Acid-Picric Acid Complexes by X-Ray Crystal Analyses

    National Research Council Canada - National Science Library

    長田, 裕臣; 尹, 康子; 友尾, 幸司; 土井, 光暢; 石田, 寿昌; 若原, 章男

    1995-01-01

    As a part of elucidating the structural features of a host molecule necessary for the recognition of basic amino acids, the crystal structures of the picrates of DL-arginine (1), L-arginine (2), L-lysine (3), and L-ornitine (4...

  11. Charge density analysis of two proton transfer complexes: Understanding hydrogen bonding and determination of in-crystal dipole moments

    Indian Academy of Sciences (India)

    Reji Thomas; Shrinwantu Pal; Ayan Datta; Mariusz K Marchewka; Henryk Ratajczak; Swapan K Pati; G U Kulkarni

    2008-11-01

    An experimental charge density study has been carried out on proton-transfer complexes exhibiting nonlinear optical (NLO) properties-melaminium tartrate monohydrate and L-asparaginium picrate employing high-resolution X-ray diffraction at 100 K. Both the complexes crystallize in non-centric space group P21 and the structures exhibit interesting patterns of N-H…O and O-H…O hydrogen bonding. Experimental determination of the dipole moment () for the asymmetric unit reveals that for both the crystals, there is a large cooperative enhancement in the crystalline arising essentially due to hydrogen bond mediated charge transfer between the melaminium ion and the L-tartrate in one case, between the Lasparaginium ion and the picrate in the other complex. We have additionally performed theoretical calculations at the density functional theory (DFT) level to understand the origin of enhancement of the dipole moments in the two systems.

  12. Synthesis, structure and spectroscopic properties of rare earth complexes with a new aryl amide 2,2'-bipydine derivative

    Science.gov (United States)

    Song, Xue-Qin; Zheng, Jiang-Rong; Liu, Wei-Sheng; Ju, Zheng-Hua

    2008-01-01

    Solid complexes of rare earth nitrates and picrates with a new aryl amide ligand 3.3'-bis(benzylamido)-2,2'-bipyridine ( L) were synthesized and characterized by elemental analysis, IR and molar conductivity measurements. The molecular structures of the complex [TbL 2(NO 3) 3H 2O]·2H 2O have been determined by single-crystal X-ray diffraction. The fluorescent properties of the Eu(III) and Tb(III) nitrates and picrates complexes in solid state were also investigated in detail. Under the excitation, these complexes exhibited characteristic emissions of europium and terbium ions. It is worth noting that the nature of the anion has a great effect upon the composition of the complexes as well as emission properties of them.

  13. A Versatile Synthesis of 1,3,5-Triamino-2,4,6-Trinitrobenzene (TATB)

    Energy Technology Data Exchange (ETDEWEB)

    Mitchell, A R; Pagoria, P F; Schmidt, R D; Coburn, M D; Lee, G S; Hsu, P C

    2006-04-06

    A safe and versatile synthesis of high-purity 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) based on vicarious nucleophilic substitution (VNS) chemistry has now been achieved. The starting material can be selected from a variety of inexpensive nitroarenes obtained from commercial suppliers (4-nitroaniline, picric acid) or U.S. stockpiles (ammonium picrate, TNT). The use of picric acid and ammonium picrate (Explosive D) is preferred as both compounds are directly converted to picramide in the presence of ammonium salts (diammonium hydrogen phosphate, ammonium carbamate) in sulfolane at elevated temperature. The picramide resulting from this process is directly converted to TATB using an optimized VNS reaction employing inexpensive hydroxylamine as the nucleophilic aminating reagent. A crucial element in our synthesis is a novel and efficient purification of TATB.

  14. Kinetics of Model Reactions for Interfacial Polymerization

    Directory of Open Access Journals (Sweden)

    Henry Hall

    2012-02-01

    Full Text Available To model the rates of interfacial polycondensations, the rates of reaction of benzoyl chloride and methyl chloroformate with various aliphatic monoamines in acetonitrile were determined at 25 °C. Buffering with picric acid slowed these extremely fast reactions so the rate constants could be determined from the rate of disappearance of picrate ion. The rates of the amine reactions correlated linearly with their Swain-Scott nucleophilicities.

  15. Investigations of Novel Energetic Materials to Stabilize Rocket Motors

    Science.gov (United States)

    2002-04-30

    and various additives were developed in the second half of the 20th Century. The earliest such propellants were asphalt -based developed at GALCIT with...Decomposition of Energetic Materials 74. Volatile Metal Isocyanates from Flash Pyrolysis of Metal-NTO and Metal-Picrate Salts and an Application Hypothesis...B. Brill, T. L. Zhang and B. C. Tappan, Thermal Decomposition of Energetic Materials 74. Volatile Metal Isocyanates from Flash Pyrolysis of Metal-NTO

  16. Evaluation of Diazatetraoxa Cryptand as Extractant for Transition Metals and Pb2+

    Directory of Open Access Journals (Sweden)

    Gülsev Dilber

    2014-12-01

    Full Text Available The extractability of metal cations such as Mn2+, Co2+, Cu2+, Zn2+ and Pb2+ from aqueous phase to organic phase with 19-nitro-6,7,15,16,23,24-hexahydro-13H,26H-14,25-propanotribenzo-[b,I,o][1,4,11,14,7,18]-tetraoxadiazacycloikocine was investigated by means of UV-vis spectrophotometer. The aqueous phase and the organic phase contained metal picrate and the ligands, respectively. Chloroform and dichloromethane were the organic solvents. The effect of pH on the percent extraction was evaluated between 2.0 and 5.5 for both organic solvents. The range at which high percent extraction of the ligand was obtained was between pH 5.0 to 5.5 for both solvents. The most effective transport was observed for Mn2+ with 84.69 % picrate among the tested metal picrates with dichloromethane at pH 5.5. The extraction constant values (log Kex were determined for extracted metal complexes at the most effective extraction pH.

  17. Synthesis, characterization and luminescence properties of rare earth complexes with a new biphenylamide

    Energy Technology Data Exchange (ETDEWEB)

    Guo, Yan-Ling, E-mail: guoyl2004@163.com [School of Nuclear Science and Technology, Lanzhou University, Lanzhou 730000 (China); Dou, Wei; Wang, Yu-Jiao; Zhou, Xiao-Yan; Liu, Wei-Sheng [College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou 730000 (China)

    2013-03-15

    A new amide-based ligand derived from biphenyl, N,N-dibenzyl-2-{l_brace}2 Prime -[(dibenzylcarbamoyl)-methoxy]-biphenyl-2-yloxy{r_brace} -acetamide (L), and its complexes of rare earth picrates were synthesized. The complexes were characterized by elemental analysis, IR, {sup 1}H NMR, UV-Vis spectra and conductivity measurements. Under the excitation, the europium(III) complex exhibited characteristic emissions of europium. The luminescence properties of the europium(III) complex in solid state and in CHCl{sub 3}, acetone, acetonitrile and DMF were investigated. The lifetime of the {sup 5}D{sub 0} level of the Eu{sup 3+} ion in the complex is 0.68 ms. The quantum yield {Phi} of the europium picrate complex was found to be 2.54 Multiplication-Sign 10{sup -3} with quinine sulfate as reference. The lowest triplet state energy level of the ligand indicates that the triplet state energy level of the ligand matches better to the resonance level of Eu(III) than Tb(III) ion. - Highlights: Black-Right-Pointing-Pointer Synthesis of a new amide type podand and its lanthanide picrate complexes. Black-Right-Pointing-Pointer Characterization was done by elemental analysis, conductivity, IR, {sup 1}H NMR and UV-Vis. Black-Right-Pointing-Pointer Luminescence properties of Eu{sup 3+} complex were analyzed. Black-Right-Pointing-Pointer Triplet state energy level of ligand matches better to the resonance level of Eu{sup 3+} than Tb{sup 3+} ion.

  18. Multiheteromacrocycles that Complex Metal Ions. Second Progress Report, 1 May 1975 -- 30 April 1976

    Science.gov (United States)

    Cram, D. J.

    1976-01-15

    Objective is to develop cyclic and polycyclic host organic compounds to complex and lipophilize metal ions. Macrorings were synthesized: (OCH{sub 2} CH{sub 2} O CH{sub 2}COCH{sub 2} COCH{sub 2}){sub 2} and (OCH{sub 2} CH{sub 2} O CH{sub 2} COCH{sub 2} COCH{sub 2}){sub 3}. The smaller ring complexes divalent metals 10{sup 1+9} times better than the open-chain model CH{sub 3} O CH{sub 2} CO CH{sub 2} COCH{sub 2} O CH{sub 3}, and the order in which metal ions are complexed is Cu{sup 2+}, UO{sub 2}{sup 2+} greater than Ni{sup 2+} greater than Fe{sup 2+}, Co{sup 2+}, Zn{sup 2+}, Cd{sup 2+} greater than Mn{sup 2+}. The UO{sub 2}{sup 2+} and Cu{sup 2+} complexes were isolated and characterized. The larger ring complexes trivalent metals 10{sup 0.9-1.7} times better than the open- chain model compound, and the order is La{sup 3+}, Ce{sup 3+} greater than Cr{sup 3+}. Five other macrocycles were also synthesized, and their binding constants with Na, K, NH{sub 4}, and Cs picrates were measured. Six compounds containing one macroring and two inward-pointing ArOH or ArOCH{sub 3} groups were also prepared and tested for binding of Li, Na, K, Rb, and NH{sub 4} picrates. Racemic compounds containing two binaphthyls and its sulfur analog were prepared. Cage-shaped multiheteromacrocycles containing ten O ligand sites or four S and six O ligand sites were prepared and the binding capability of the first compound for picrates studied. Two ring systems with phosphonate ester groups were also prepared. (DLC)

  19. Mechanisms and rules of anion partition into ionic liquids: phenolate ions in ionic liquid/water biphasic systems.

    Science.gov (United States)

    Katsuta, Shoichi; Nakamura, Ko-ichi; Kudo, Yoshihiro; Takeda, Yasuyuki

    2012-01-19

    It is important to understand the mechanisms and general rules of ion partitioning in hydrophobic ionic liquid (IL)/water biphasic systems in order to predict the extractability of an ionic species with various ILs. In this study, we have investigated the partition of picrate ion (target anion, T(-)) from aqueous sodium picrate solutions into several ILs and the accompanying changes in aqueous concentrations of the IL component cation (C(+)) and anion (A(-)) at 298.2 K. The main ILs examined are 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)amide, 1-butyl-3-methylimidazolium hexafluorophosphate, and 1-methyl-3-octylimidazolium bis(trifluoromethanesulfonyl)amide. The aqueous concentrations of C(+) and A(-) decreased and increased, respectively, with the extraction of T(-) into the IL phase. From the standpoint of equilibrium, the partition behavior of T(-) can be explained both by the anion exchange with A(-) in the IL phase and by the ion pair extraction with C(+) in the aqueous phase. The aqueous concentrations of C(+) and A(-) are governed by the solubility product of the IL (K(sp)). The distribution ratio of T(-) is expressed as a function of Δ[T(-)](W), namely, the difference between the initial and equilibrium concentrations of T(-) in the aqueous phase; the distribution ratio of T(-) is nearly constant when Δ[T(-)](W) < K(sp)(1/2), but decreases with increasing Δ[T(-)](W) in the larger Δ[T(-)](W) region. The equilibrium constants of the ion pair extraction and the ion exchange extraction have been determined for picrate and other phenolate ions whose partition data were previously reported. The dependences of the extraction constants and extractability on the kinds of IL component ions can be quantitatively explained on the basis of the variations of K(sp).

  20. The synthesis of (N 2O 2S 2)-Schiff base ligands and investigation of their ion extraction capability from aqueous media

    Science.gov (United States)

    Zoubi, Wail A. L.; Kandil, Farouk; Chebani, Mohamad Khaled

    2011-09-01

    Two new Schiff bases (I) and (II) containing nitrogen-sulfur-oxygen donor atoms were designed and synthesized in a multi-step reaction sequence. The Schiff base (I) was used in solvent extraction of metal chlorides such as Cu 2+ and Cr 3+ as well as metal picrates such as Hg 2+ and UO 22+ from aqueous phase to the organic phase. The influences of the parameter functions, such as pH, solvent, ionic strength of aqueous phase, aqueous to organic phase and concentration of the extractant were investigated to shed light on their chemical extracting properties upon the extractability of metal ions. The effect of chloroform, dichloromethane and nitrobenzene as organic solvents over the metal chlorides extraction was investigated at 25 ± 0.1 °C by using flame atomic absorption and the result is that the ability of extraction in solvents as follows: C 6H 5NO 2 > CHCl 3 > CH 2Cl 2 and the compositions of the extracted species have been determined. The metal picrate extraction was investigated at 25 ± 0.1 °C by using UV-visible spectrometry. As well that the extraction of picrates metal such as UO 22+ and Hg 2+ with Schiff base(I) in absence and presence of 2-(2-aminoethyl) pyridine was investigated in chloroform. The extraction results revealed the presence of neutral donors 2-(2-aminoethyl) pyridine shifts the extraction percentage curves towards higher pH region, indicating a synergistic effect of this donors on extraction of UO 22+ and Hg 2+ by the studied Schiff base (I).

  1. Synthesis and cationic selectivity studies of novel calix[4]arene derivatives containing heteroatom at the lower rim

    Institute of Scientific and Technical Information of China (English)

    WANG; Hao; LI; Zhe; LIU; Yu

    2007-01-01

    A series of calixarene derivatives 2-5 containing heteroatom at the lower rim have been synthesized. 1H NMR studies and crystallographic structures demonstrated that the calix[4]arene derivatives adopted cone conformations. Their cationic binding abilities and selectivities towards heavy and transition metal ions have been evaluated by solvent extraction of aqueous metal picrates. The obtained results indicated that the introduction of nitrogen, sulfur, and/or phosphor atoms to the calix[4]arene framework could effectively enhance their binding ability and selectivity for heavy and transition metal ions, such as Pb2+ or Ag+.

  2. Physicochemical parameters of crystallization of dunite from the Guli ultrabasic massif (Maimecha Kotui province)

    Science.gov (United States)

    Simonov, V. A.; Vasiliev, Yu. R.; Stupakov, S. I.; Kotlyarov, A. V.; Karmanov, N. S.

    2015-09-01

    On the basis of analysis of molten inclusions in chrome-spinelide, physicochemical parameters of dunite crystallization were defined. Experimental, analytical studies directly indicate that dunite was formed from high-temperature melts close in petrochemical composition and high-temperature characteristics to meimechite magmas. Successive evolution of magmatic systems compositions in a course of intra-chamber crystallization of dunite was established: from picriteâ "meimechite (with olivine formation at 1590-1415°C and chrome-spinelide crystallization at 1405-1365°C) to picrate-basalt and basalt.

  3. Indirect photometric detection of boron cluster anions electrophoretically separated in methanol.

    Science.gov (United States)

    Vítová, Lada; Fojt, Lukáš; Vespalec, Radim

    2014-04-18

    3,5-Dinitrobenzoate and picrate are light absorbing anions pertinent to indirect photometric detection of boron cluster anions in buffered methanolic background electrolytes (BGEs). Tris(hydroxymethyl)aminomethane and morpholine have been used as buffering bases, which eliminated baseline steps, and minimized the baseline noise. In methanolic BGEs, mobilities of boron cluster anions depend on both ionic constituents of the BGE buffer. This dependence can be explained by ion pair interaction of detected anions with BGE cations, which are not bonded into ion pairs with the BGE anions. The former ion pair interaction decreases sensitivity of the indirect photometric detection.

  4. Molecular Design of Calixarene 5. Syntheses and Cation Selectivities of Novel Schiff' s Base p-tert-Butylcalix[4]arenes

    Institute of Scientific and Technical Information of China (English)

    刘育; 赵邦屯; 王浩; 陈企发; 张衡益

    2001-01-01

    Five novel Schiff's bases p-tert-butylcalix[4]arenes have ben synthesized in high yields by the reaction of 1,3-distally disubstituted p-tert-butyicalix[4]arene amine(1) with the corresponding aromatic aldehydes,and their cation binding abilities and selectivities with alkali and heavy metal ions have been evaluated by solvent extraction of aqueous metal picrates to show the highet Ag+ extractability for Schiff' s base p-tertbutylcalix[4]arene (6) and the best Na+/Li+ and Ag+/Tl+selectivities for Schiff's base p-tert-butylcalix[4]arene (4 and 2) over any other caltx[4]arene derivatives, respectively.

  5. Hexaaquamanganese(II dipicrate dihydrate

    Directory of Open Access Journals (Sweden)

    Mingjie Zhang

    2008-02-01

    Full Text Available In the title compound, [Mn(H2O6](C6H2N3O72·2H2O, the manganese cation, on an inversion centre, is coordinated by six water molecules, but the picrate anion has no coordinative interaction with the manganese cation. The anions in the stack are linked via short intermolecular O...C (3.013 and 2.973 Å and C...C (3.089 and 3.065 Å contacts and hydrogen bonds.

  6. {μ-trans-N,N′-Bis[2-(2-hydroxyethylaminoethyl]oxamidato(2−}bis[picratonickel(II

    Directory of Open Access Journals (Sweden)

    Chunliang Tian

    2010-01-01

    Full Text Available The title complex, [Ni2(C6H2N3O72(C10H20N4O4], contains a centrosymmetric binuclear unit in which the oxamide ligand (located on a centre of symmetry acts in a bis-tetradentate fashion and the picrate anion binds to nickel(II in a bidentate mode. The NiII atom displays a distorted octahedral coordination with axial elongation. The binuclear molecules are linked by intermolecular N—H...O, O—H...O and C—H...O hydrogen bonds into a two-dimensonal supramolecular network extending parallel to (100.

  7. High-speed ion-pair partition chromatography in pharmaceutical analysis.

    Science.gov (United States)

    Santi, W; Huen, J M; Frei, R W

    1975-12-24

    Ion-pair chromatography offers attractive possibilities in pharmaceutical analysis. The specificity of the separation systems can be varied over a wide range by appropriate selection of the stationary phase. The choice of a suitable counter-ion can also drastically improve the detection limit, permitting the determination of drug substances in low dosage and possibly of by-products or breakdown products. Ion-pair chromatography of tropane and ergot alkaloids has been investigated using picrate as counter-ion. Alumina, Kieselguhr and various grades of silica gel have been tested as supports. Partition properties studied in a batch procedure have been compared with the actual chromatographic conditions. Columns (10 cm) filled with silical gel (particle size, 5 mum; pore size, 1000 A) show the best performance in the separation of hyoscyamine, scopolamine and ergotamine as picrate ion-pairs. Close control of pH and temperature is essential for reproducible separations. Improvements in detection limits between 100 and 300 times have been observed with these systems. Ion-pair extractions of these alkaloids from dosage forms can be used for sample preparation prior to injection on the the column. This provides an added degree of selectivity and sensitivity.

  8. Determinação potenciométrica em fluxo de cloreto de cetilpiridinio em desinfectantes bucais Potentiometric determination of cetylpyridinium chloride in oral desinfectants by flow injection analysis

    Directory of Open Access Journals (Sweden)

    Paula C. S. Baptista

    2003-08-01

    Full Text Available The work describes a new procedure for cetylpyridinium chloride determination in oral disinfectants, based on a flow-injection system with potentiometric detection. The determination was based on the measurement of picrate concentration decrease as result of ion-pair reaction with the analyte present in the injected sample. In the optimised set-up the sample injection volume was kept at 400 µL and merged downstream with the reagent solution containing 1,0 x10-5 mol/L of picrate adjusted to pH 5.0 with citrate/citric acid buffer. The flow rate was fixed at 8 mL/min and the reactor length at 40 cm. The proposed procedure enables the determination of cetylpyridinium in the analytical range of 5,0x10-6 - 7,5x10-5 mol/L at a sampling rate of 60/h. The results for real samples had a precision better than 3% and were comparable to the labelled values.

  9. Thermal stability of the anionic sigma complexes of 2,4,6-trinitroanisole with the methylates of the alkaline-earth metals

    Energy Technology Data Exchange (ETDEWEB)

    Glaz, A.I.; Soldatova, T.A.; Golopolosova, T.V.; Gitis, S.S.

    1987-09-10

    The study of the stability of the 1,1-dimethoxy-2,4,6-trinitrocyclohexadienates of the alkali metals when they are heated in air showed that their temperature of decomposition and the heat effect of the process are dependent on the nature of the cation. Our study centered on the thermal decomposition of the products resulting from the addition of the methylates of calcium, strontium, and barium to 2,4,6-trinitroanisole. For a quantitative assessment of the process we used the combined methods of differential-thermal analysis and differential thermogravimetry. The anionic sigma-complexes of 2,4,6-trinitroanisole with the methylates of the alkaline-earth metals decompose on heating into the corresponding picrates; at the same time, when one passes from the calcium slat to the strontium and barium salts the decomposition temperature and the heat effect of the process show a drop which is linked to the structure both of the complexes and of the picrates forming therefrom.

  10. 1-Methylpiperazine-1,4-diium dipicrate

    Directory of Open Access Journals (Sweden)

    Grzegorz Dutkiewicz

    2011-02-01

    Full Text Available In the crystal structure of the title compound [systematic name: 1-methylpiperazine-1,4-diium bis(2,4,6-trinitrophenolate], C5H14N22+·2C6H2N3O7−, the ionic components are connected by relatively strong N—H...O hydrogen bonds into centrosymmetric six-membered conglomerates, which comprise two dications and four anions. Besides Coulombic interactions, only weak C—H...O interactions and some stacking between picrates (separation between the planes of ca. 3.4 Å but only a small overlapping can be identified between these `building blocks' of the crystal structure. The piperazine ring adopts a chair conformation with the methyl substituent in the equatorial position. In the picrate anions, the twist angles of the nitro groups depend on their positions relative to the phenolate O atom: it is much smaller for the NO2 groups para to the C—O− group [15.23 (9and 3.92 (14°] than for the groups in the ortho positions [28.76 (13–39.84 (11°].

  11. A seven-coordinated manganese(II) complex with V-shaped ligand bis(N-benzylbenzimidazol-2-ylmethyl)benzylamine: synthesis, structure, DNA-binding properties and antioxidant activities.

    Science.gov (United States)

    Wu, Huilu; Yuan, Jingkun; Bai, Ying; Wang, Hua; Pan, Guolong; Kong, Jin

    2012-11-05

    A manganese(II) complex of the type, [MnL(pic)(2)]·H(2)O, was obtained by the reaction of the V-shaped ligand bis(N-benzylbenzimidazol-2-ylmethyl)benzylamine (L) with Mn(pic)(2) (pic=picrate). The ligand L and Mn(II) complex were confirmed on the basis of elemental analysis, molarconductivities, (1)H NMR, IR, UV-vis spectra and X-ray crystallography. Single-crystal X-ray revealed that central Mn(II) atom is seven-coordinate with a MnN(3)O(4) environment, in which ligand L acts as a tridentate N-donor. The remaining coordination sites were occupied by four O atoms afforded by two picrate anion. Interaction of the free ligand L and Mn(II) complex with DNA were investigated by spectrophotometric methods and viscosity measurements. The results suggested that both ligand L and Mn(II) complex bind to DNA in an intercalative binding mode, and DNA-binding affinity of the Mn(II) complex is stronger than that of ligand L. Moreover, antioxidant assay in vitro shows the Mn(II) complex possesses significant antioxidant activities.

  12. Cyclic peptides-assisted trans- port of metal ions across liquid-organic membrane

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    The formation of alkali and alkaline-earth metal picrate complexes with cyclo(Pro-Gly)n ionophores (1, n = 3; 2, n = 4) can facilitate the migration of metal ions across a bulk liquid CH2Cl2 membrane. The migration behavior was studied by measuring the solution absorption at 356 nm, using a UV/Vis spectrophotometer, and the rates can be determined by comparing the initial absorption of donor solutions with the absorption of the corresponding receiver solutions as the function of time. It was found that cyclic peptide 1 shows higher transport activity for the studied alkali and alkaline-earth metal ions than compound 2, which is related to the backbone flexibility of the cyclic peptides. The findings in this work suggest that the rate of ionophore-facilitated ion transport depends not only on the ability of complex forma-tion in aqueous phase, but also on the ability of complex dissociation in organic phase.

  13. Hydrogen peroxide as a new defensive compound in "benzoyl cyanide" producing polydesmid millipedes

    Science.gov (United States)

    Kuwahara, Yasumasa; Yamaguchi, Takuya; Ichiki, Yayoi; Tanabe, Tsutomu; Asano, Yasuhisa

    2017-04-01

    Hydrogen peroxide was newly and simultaneously demonstrated with well-known hydrogen cyanide as a component of defensive secretions of "benzoyl cyanide" producing polydesmid millipedes. Presence of hydrogen peroxide was successively evidenced by Trinder reagent's spray with colorless as well as oily smears of defensive secretions containing benzoyl cyanide and hydrogen cyanide by alkaline picrate paper treatment. Linear correlation was demonstrated between quantities of hydrogen peroxide and benzoyl cyanide. By qualitative assay, seven benzoyl cyanide containing polydesmidans (six species of adults and one species of a nymph at stadium I) tested positive to Trinder reagent, indicative of the presence of hydrogen peroxide (together with hydrogen cyanide), while two cyanogenic species without benzoyl cyanide exhibited negative responses to the reagent. Two types of millipedes were elucidated as species of cyanogenic Polydesmida.

  14. Extraction and Binding Efficiency of Calix[8]arene Derivative Toward Selected Transition Metals

    Directory of Open Access Journals (Sweden)

    Imdadullah Qureshi

    2008-12-01

    Full Text Available In this article we have explored the extraction efficiency as well as binding ability of calix[8]arene derivative (3 for selected transition metal ions (Co2+, Cd2+, Ni2+, Pb2+ and Cu2+. Picrate salt solutions of these metals were used in the liquid-liquid extraction experiments. It is apparent from the results that ligand 3 shows appreciable high extraction of transition metal cations, with the relative order Pb2+>Cu2+>Ni2+>Co2+>Cd2+ being observed. Highest extraction efficiency has been observed for Pb2+ and Cu2+ i.e. 95 and 91% respectively. The significant extraction and complexation ability for these metal ions may be attributed to the nature, size, structure and geometry of both ligand and metal ions.

  15. Conversion of Surplus Picric Acid/Explosive D to Higher Value Products

    Energy Technology Data Exchange (ETDEWEB)

    Mitchell, A R; Hsu, P C; Coburn, M D; Schmidt, R D; Pagoria, P F; Lee, G S; Kwak, S S W

    2003-02-28

    The global demilitarization of nuclear and conventional munitions is producing millions of pounds of surplus energetic materials. Historically, energetic materials (high explosives, propellants, and pyrotechnics) have been disposed of by open burning/open detonation (OB/OD). The use of OB/OD is becoming unacceptable due to public concerns and increasingly stringent environmental regulations. Clearly, there is a great need to develop environmentally sound and cost-effective alternatives to OB/OD. The conversion of surplus picric acid and/or ammonium picrate (Explosive D) to 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) has been subject of extensive process development studies at Lawrence Livermore National Laboratory (LLNL). LLNL, under the direction and sponsorship of the U.S. Army Defense Ammunition Center (DAC), is developing a process for the conversion of picric acid to TATB on a pilot scale.

  16. High Infestation by Dawestrema cycloancistrioides in Arapaima gigas Cultured in the Amazon Region, Peru

    Directory of Open Access Journals (Sweden)

    Patrick D. Mathews

    2014-01-01

    Full Text Available The aim of this study was to evaluate the presence of Dawestrema cycloancistrioides in semi-intensive fish farming of fingerlings of Arapaima gigas. Between September and November 2013, 60 individuals of A. gigas born in captivity, were collected in three concrete ponds, from a semi-intensive fish farm in the Peruvian Amazon. For the study of sclerotized structures, parasites were fixed in a solution of ammonium picrate glycerine and mounted in Canada balsam. To visualize internal structures, parasites were fixed in hot formaldehyde solution (4% for staining with Gomori’s trichrome. The parasitic indexes calculated were prevalence, mean intensity, and mean abundance. This study identified a high infestation of a monogenean D. cycloancistrioides in gills of A. gigas. The prevalence was 100%. The mean intensity and mean abundance of the parasite were 144.9 of parasites per individual. This study confirms the necessity of constant monitoring of fish in order to reduce fish mortality.

  17. trans-Bis(dimethyl sulfoxide-κObis(thiosemicarbazide-κ2N1,Scadmium dipicrate dihydrate

    Directory of Open Access Journals (Sweden)

    Helen Stoeckli-Evans

    2011-01-01

    Full Text Available In the cation of the title compound, [Cd(CH5N3S2(C2H6OS2](C6H2N3O72·2H2O, the CdII atom is located on an inversion center. It is hexacoordinated in an octahedral fashion by two thiosemicarbazide molecules, which coordinate in a bidentate manner via the S and N atoms, and to the O atom of two dimethyl sufoxide (DMSO molecules. The charges are equilibrated by two picrate anions and the complex crystallizes as a dihydrate. In the crystal, these units are linked by a number of O—H...O and N—H...S hydrogen bonds and weak C—H...O interactions, forming a three-dimensional network.

  18. Elevated creatinine after ingestion of model aviation fuel: interference with the Jaffe reaction by nitromethane.

    Science.gov (United States)

    Booth, C; Naidoo, D; Rosenberg, A; Kainer, G

    1999-10-01

    A 2 years 9 month-old-boy who ingested model aviation fuel was found to have an elevated serum creatinine concentration of 0.53 mmol/L (normal range 0.02-0.05 mmol/L) by the Jaffe (alkaline picrate) reaction. However, when the creatinine concentration was measured using a specific enzymatic assay, it was within the normal range. It was shown that nitromethane, a constituent of aviation fuel, interferes with the Jaffe reaction, leading to a falsely elevated creatinine reading. This phenomenon has been reported only once previously and, despite its potential clinical importance, nitromethane does not appear in published lists of substances that interfere with the Jaffe reaction.

  19. Synthesis, characterization, fluorescence and DNA-binding studies of europium(Ⅲ) pirates complexes with amide-based 2,3-dihydroxynaphthalene derivatives

    Institute of Scientific and Technical Information of China (English)

    LI Hanyu; YANG Tianlin; DING Ling; WANG Wenhua

    2012-01-01

    Two ligands 2,2'-[2,3-naphthylenebis(oxy)]-bis(N-benzyl(acetamide)(L1) and 22'-[23-naphthylenebis (oxy)]-bis(N,N-diphenyl (acetamide)(L2) and their europium(Ⅲ) picrate complexes were synthesized.The complexes were characterized by elemental analysis,infrared (IR),thermogravimetry and differential thermal analysis (TG-DTA) and molar conductivity.Fluorescent experiments showed that the resonance level of the Eu(Ⅲ) matched better to the triplet state energy level of the ligand L2 than that of the ligand L1 and the fluorescence intensifies of the complexes were reduced with the raising coordination ability of solvent.In addition,the interactions between the complexes and DNA were studied by means of spectrometry and cyclic voltammetry.The results suggested that the complexes could bind to DNA through intercalation and the complex 1 binded to DNA more strongly than the complex 2.

  20. Energetic materials destruction using molten salt

    Energy Technology Data Exchange (ETDEWEB)

    Upadhye, R.S.; Watkins, B.E.; Pruneda, C.O.; Brummond, W.A.

    1994-04-29

    The Lawrence Livermore National Laboratory in conjunction with the Energetic Materials Center is developing methods for the safe and environmentally sound destruction of explosives and propellants as a part of the Laboratory`s ancillary demilitarization mission. LLNL has built a small-scale unit to test the destruction of HE using the Molten Salt Destruction (MSD) Process. In addition to the high explosive HMX, destruction has been carried out on RDX, PETN, ammonium picrate, TNT, nitroguanadine, and TATB. Also destroyed was a liquid gun propellant comprising hydroxyammonium nitrate, triethanolammonium nitrate and water. In addition to these pure components, destruction has been carried out on a number of commonly used formulations, such as LX-10, LX-16, LX-17, and PBX-9404.

  1. An Efficient Ag+ Ionophore Based on Thiacalix[4]arene

    Institute of Scientific and Technical Information of China (English)

    LI Xiong; GONG Shu-Ling; YANG Wei-Ping; CHEN Yuan-Yin

    2008-01-01

    A novel Ag+ ionophore, p-tert-butyi-tetrakis(hydrazinocarbonylmethoxy)thiacalix[4]arene in 1,3-alternate conformation (thiacalix[4]arene tetrahydrazide, 1) was synthesized. Its binding properties towards alkali and transition metal cations were studied by noncompetitive liquid-liquid extraction of alkali metal (Li+, Na+, K+ and Cs+)and transition metal (Co2+, Ni2+, Cu2+, Zn2+, Ag+) picrates. It was found that the thiacalix[4]arene tetrahydrazide exhibited high extractability towards Ag+, lower percent extraction towards Cu2+, and little or no extraction ability towards the others. The selectivity towards Ag+ was further evaluated by competitive Ag+ extraction experiments in the mixture of the above-mentioned nine cations, the concentration of which was monitored with ICP-OES. 1HNMR titration experiments and ESI-MS proved the stoichiometry of 1 to Ag+ was 1 : 1, and the 'N-Ag+' interaction with the assistance of thiacalixarene skeleton was primarily involved in the complexation.

  2. Surveys on Gyrodactylus parasites onwild Atlantic salmon in Denmark

    DEFF Research Database (Denmark)

    Jørgensen, Louise von Gersdorff; Heinecke, Rasmus Demuth; Buchmann, Kurt

    Gyrodactylus salaris is a monogenean ectoparasite parasitizing salmonids in freshwater. This parasite is highly pathogenic to both Norwegian and Scottish salmon and has decimated the salmon populations in 45 Norwegian rivers after anthropogenic transfer from Sweden. G. salaris has also been found...... on several occasions in Danish rainbow trout farms but has never been recorded as a pathogenic parasite on Danish wild salmon. In the present study the occurrence of G. salaris and other Gyrodactylus parasites on wild Danish salmon fry and parr were monitored. Electrofishing was conducted in three river...... were examined for Gyrodactylus parasites under a dissection microscope. The location of each parasite was registered and each parasite was isolated for later morphological and genetic typing. The opisthaptor was separated from the body, fixed and mounted using Malmbergs fixative (ammonium picrate...

  3. A dynamic model of the marriage market-part 1: matching algorithm based on age preference and availability.

    Science.gov (United States)

    Matthews, A P; Garenne, M L

    2013-09-01

    The matching algorithm in a dynamic marriage market model is described in this first of two companion papers. Iterative Proportional Fitting is used to find a marriage function (an age distribution of new marriages for both sexes), in a stable reference population, that is consistent with the one-sex age distributions of new marriages, and includes age preference. The one-sex age distributions (which are the marginals of the two-sex distribution) are based on the Picrate model, and age preference on a normal distribution, both of which may be adjusted by choice of parameter values. For a population that is perturbed from the reference state, the total number of new marriages is found as the harmonic mean of target totals for men and women obtained by applying reference population marriage rates to the perturbed population. The marriage function uses the age preference function, assumed to be the same for the reference and the perturbed populations, to distribute the total number of new marriages. The marriage function also has an availability factor that varies as the population changes with time, where availability depends on the supply of unmarried men and women. To simplify exposition, only first marriage is treated, and the algorithm is illustrated by application to Zambia. In the second paper, remarriage and dissolution are included.

  4. Recent Progress on the Conversion of Surplus Picric Acid/Explosive D to Higher Value Products

    Energy Technology Data Exchange (ETDEWEB)

    R.Mitchell, A; Hsu, P C; Coburn, M D; Schmidt, R D; Pagoria, P F; Lee, G S; Kwak, S W

    2004-07-06

    The global demilitarization of nuclear and conventional munitions is producing millions of pounds of surplus energetic materials. Historically, energetic materials (high explosives, propellants, and pyrotechnics) have been disposed of by open burning/open detonation (OB/OD). The use of OB/OD is becoming unacceptable due to public concerns and increasingly stringent environmental regulations. Clearly, there is a great need to develop environmentally sound and cost-effective alternatives to OB/OD. The conversion of surplus picric acid and/or ammonium picrate (Explosive D) to1,3,5-triamino-2,4,6- trinitrobenzene (TATB) has been subject of extensive process development studies at Lawrence Livermore National Laboratory (LLNL). LLNL, under the direction and sponsorship of the U.S. Army Defense Ammunition Center (DAC), is developing a process for the conversion of picric acid to TATB on a larger scale. In FY 03, a 10 g per batch process was developed with good results. Development for a one pound per batch system is required as part of overall scale up process for producing TATB from the surplus feedstocks.

  5. [Method selected for the determination of creatinine in plasma or serum. Choice of optimal conditions of measurement].

    Science.gov (United States)

    Labbé, D; Vassault, A; Cherruau, B; Baltassat, P; Bonète, R; Carroger, G; Costantini, A; Guérin, S; Houot, O; Lacour, B; Nicolas, A; Thioulouse, E; Trépo, D

    1996-01-01

    The method selected by the SFBC (Société française de biologie clinique) is derived from the colorimetric reaction of creatinine with alkaline picrate, measured kinetically, without any pretreatment step. The key parameters of the reaction determining the quality of the results are studied, with special regard to samples including known interferents. The aims of the study were to gain an optimal analytical sensitivity and to reduce main interferences (acetoacetate, bilirubine, glucose, protein) which plague the Jaffé reaction, through a comprehensive study of the reagents, of their concentrations and of the analytical procedures. The selected concentrations (in the test) are: 150 mmol/L sodium hydroxide, 10 mmol/L picric acid and 2 g/L sodium dodecyl sulfate. Ten millilitres of a BRIJ solution (30% volvol) are added to the reagent. The operating procedures are as follow: sample ratio 0.07 to 0.08; wavelength 505 to 510 nm; temperature 37 degrees C; incubation of the specimen with the alkaline reagent 5 mn (at least), before starting the reaction with picric acid. A seric calibrator is recommended. The first measurement is taken 20 to 40 s after starting the reaction. Total measurement time is 120 to 150 seconds.

  6. A novel liquid chromatography-mass spectrometric method for the simultaneous determination of trimethylamine, dimethylamine and methylamine in fishery products.

    Science.gov (United States)

    Baliño-Zuazo, Lander; Barranco, Alejandro

    2016-04-01

    A novel multianalyte method has been developed to determine the concentration of trimethylamine (TMA), dimethylamine (DMA) and methylamine (MA) in fish. The optimal points of the key parameters (pH 8, 60 °C and 60 min of reaction time) were determined for the reaction with tert-butyl bromoacetate. An HILIC column was used to elute all the compounds in only 12 min and selective quantitation of the compounds was achieved. The methodology was validated in trout, hake and Atlantic horse mackerel and was used to study the shelf life of fish under refrigeration. A good correlation with the picrate method was obtained and the proposed methodology has been proved to be robust, specific and sensible with a limit of detection of 0.08 mg N-TMA kg(-1) in freshwater fish and 1 mg N-TMA kg(-1) in marine fish. In addition, TMA has been proved to be a good spoilage indicator also in freshwater fish. Copyright © 2015 Elsevier Ltd. All rights reserved.

  7. V-shaped ligand 1,3-bis(1-ethylbenzimidazol-2-yl)-2-thiapropane and manganese(II), cobalt(II) and copper(II) complexes: Synthesis, crystal structure, DNA-binding properties and antioxidant activities.

    Science.gov (United States)

    Wu, Huilu; Yang, Zaihui; Wang, Fei; Peng, Hongping; Zhang, Han; Wang, Cuiping; Wang, Kaitong

    2015-07-01

    A V-shaped ligand 1,3-bis(1-ethylbenzimidazol-2-yl)-2-thiapropane (bebt) and its transition metal complexes, [Mn(bebt)(pic)2]·CH3OH (pic=picrate) 1, [Co(bebt)2](pic)22 and [Cu(bebt)2](pic)2·2DMF 3, have been synthesized and characterized. The coordinate forms of complexes 1 and 2 are basically alike, which can be described as six-coordinated distorted octahedron. The geometric structure around Cu(II) atom can be described as distorted tetrahedral in complex 3. The DNA-binding properties of the ligand bebt and complexes have been investigated by electronic absorption, fluorescence, and viscosity measurements. The results suggest that bebt and complexes bind to DNA via an intercalative binding mode and the order of the binding affinity is 1<2<3

  8. Preparation,Crystal Structure and Thermal Analyses of a Nitrogen-rich Coordination Compound [Co(DAT)6](PA)2·4H2O

    Institute of Scientific and Technical Information of China (English)

    CUI Yan; ZHANG Jian-Guo; ZHANG Tong-Lai; YANG Li; ZANG Yan; SHU Yuan-Jie

    2008-01-01

    A new coordination compound [Co(DAT)6](PA)2·4H2O has been prepared by using 1,5-diaminotetrazole(DAT)as ligands and picrate(PA)as acidic anions,and structurally characterized by X-ray single crystal diffraction,ele-mental analysis and FT-IR spectroscopy.The cobalt(Ⅱ)cation coordinates with six N atoms from six bulky DAT molecules to form a six-coordinated and slightly distorted octahedral configuration.The coordination cation is situ-ated between two PA anions whose benzene-ring planes are parallel to each other.The coordination cation and the lecular units are linked together by the intermolecular hydrogen bonds to form the crystal structure,in the formation investigated by using DSC,TG-DTG and FT-IR analyses.The kinetic parameters of the first exothermic process of the title compound were studied by applying the Kissinger's and Ozawa-Doyle's methods.

  9. Transition metal cations extraction by ester and ketone derivatives of chromogenic azocalix[4]arenes.

    Science.gov (United States)

    Ak, Metin; Taban, Deniz; Deligöz, Hasalettin

    2008-06-15

    The molecule of azocalix[n]arene is a macrocyclic used effectively in the complexation of the heavy metal pollutants (like silver and mercury). In this work, our main aim is to prepare new chromogenic azocalix[n]arene molecules to elaborate an extractant with high extractant selectivity for metal ions able to detect this type of pollutant. The solvent extraction properties of four acetyls, four methyl ketones and four benzoyls derivatives from azocalix[4]arenes which were prepared by linking 4-ethyl, 4-n-butyl, 4-acetamid anilin and 2-aminothiazol to calix[4]arene through a diazo-coupling reaction, the alkaline earth (Sr2+) and the transition (Ag+, Hg2+, Co2+, Ni2+, Cu2+, Zn2+, Cd2+, Cr3+) metal cations have been determined by extraction studies with metal picrates. Both ketones are better extractants than esters, and show a strong preference for Ag+, while Cu2+ and Cr3+ are the most extracted cation with the esters. Both acetyl and benzoyl esters are good carriers for Ag+ and Hg2+.

  10. Synthesis, Crystal Structure, Thermal Decomposition and Sensitive Properties of a New Complex [Cu(IMI)4](PA)2

    Institute of Scientific and Technical Information of China (English)

    WANG Shi-wei; WU Bi-dong; YANG Li; ZHANG Tong-lai; ZHOU Zun-ning; ZHANG Jian-guo

    2012-01-01

    A new coordination complex [Cu(IMI)4](PA)2 had been synthesized with imidazole(IMI) as ligands and picrate(PA ) groups as outer anions,and characterized by Fourier transform infrared(FTIR) spectrum and elemental analysis.Its crystal structure was determined by single crystal X-ray diffraction(XRD) analysis.The crystallographic data show that the crystal belongs to monoclinic,C2/c space group,a=2.542(5) nm,b=0.91773(18) nm,c=1.3778(3)nm,β=107.854(3)° and Z=4.Furthermore,the central copper(Ⅱ) ion is coordinated by four N atoms from four imidazole ligands.All the molecular units are linked into a zigzag pattern along a-axis by the hydrogen bonds,and extended to the distance regularly.Thermal decomposition mechanisms were determined based on differential scanning calorimetry(DSC) and thermogravimetry-diff.erential thermogravimetry(TG-DTG) analysis,and kinetic parameters of the first exothermic process were studied using Kissinger's and Ozawa-Doyle's method,respectively.Sensitivity tests show that the title complex has low sensitivity to external stimulus,but it has a higher energy of combustion of 14.2kJ/g due to which it may be used as the additives of energetic materials to improve the explosive performance.

  11. Transport properties and electroanalytical response characteristics of drotaverine ion-selective sensors.

    Science.gov (United States)

    Kharitonov, Sergey V

    2005-08-01

    The construction and electroanalytical response characteristics of poly(vinyl chloride) matrix ion-selective sensors (ISSs) for drotaverine hydrochloride are described. The membranes incorporate ion-association complexes of drotaverine with tetraphenylborate, picrate, tetraiodomercurate, tetraiodobismuthate, Reinecke salt, and heteropolycompounds of Keggin structure-molybdophosphoric acid, tungstophosphoric acid, molybdosiliconic acid and tungstosiliconic acid as electroactive materials for ionometric sensor controls. These ISSs have a linear response to drotaverine hydrochloride over the range 8 x 10(-6) to 5 x 10(-2) mol L(-1) with cationic slopes from 51 to 58 mV per concentration decade. These ISSs have a fast response time (up to 1 min), a low determination limit (down to 4.3 x 10(-6) mol L(-1)), good stability (3-5 weeks), and reasonable selectivity. Permeabilities and ion fluxes through a membrane were calculated for major and interfering ions. Dependences of the transport properties of the membranes on the concentrations of the ion exchanger and near-membrane solution and their electrochemical characteristics are presented. The ISSs were used for direct potentiometry and potentiometric titration (sodium tetraphenylborate) of drotaverine hydrochloride. Results with mean accuracy of 99.1+/-1.0% of nominal were obtained which corresponded well to data obtained by use of high-performance liquid chromatography.

  12. Structure and spectral properties of L-histidinium dipicrate dihydrate.

    Science.gov (United States)

    Sethuram, M; Dhandapani, M; Sethu Raman, M; Amirthaganesan, G; Senthilkumar, K

    2014-01-24

    Non-linear optical active L-histidinium dipicrate dihydrate (LHDD) single crystals were grown by slow evaporation method. The Fourier transform FT-IR, FT-Raman, (1)H and (13)C NMR spectra of the crystal have been recorded and analysed. The spectral analyses confirm the formation of the compound and the stoichiometry. The geometry and spectral characteristics were examined using the density functional theory (DFT) method, B3LYP with 6-31G(d,p) basis set. The first-order hyperpolarisability, energies of frontier molecular orbitals and the Mulliken population analysis were also calculated. The HOMO-LUMO energy gap value 2.73 eV indicates the charge transfer from picrate to histidinium through the hydrogen bond. The second-order NLO properties of the molecule are studied by Kurtz-Perry powder technique. SHG efficiency of the compound is nearly 2.5 times greater than KDP. Theoretical calculations indicate hyperpolarisability of LHDD is 39 times greater than urea. The results show that the title molecule can be used for opto-electronic applications. Copyright © 2013 Elsevier B.V. All rights reserved.

  13. Alternative method for measurement of albumin/creatinine ratio using spectrophotometric sequential injection analysis.

    Science.gov (United States)

    Siangproh, Weena; Teshima, Norio; Sakai, Tadao; Katoh, Shuji; Chailapakul, Orawon

    2009-09-15

    A simple, automatic and practical system for successive determination of albumin and creatinine has been developed by combining sequential injection analysis (SIA) and highly sensitive dye-binding assays. Albumin detection was based on the increase in the absorbance due to complex formation between albumin and eosin Y in acidic media. The absorbance of the complex was monitored at 547 nm. For the creatinine assay, the concentration of creatinine was measured by reaction with alkaline picrate to form a colored product which absorbs at 500 nm. The influences of experimental variables such as effects of pH, reagent concentration, standard/sample volume and interferences were investigated. Under optimal conditions, the automated method showed linearity up to 20 mg L(-1) for albumin and 100 mg L(-1) for creatinine. The 3 sigma detection limits were 0.6 and 3.5 mg L(-1) for albumin and creatinine, respectively, and the relative standard deviations (n=10) were 2.49% for 20 mg L(-1) albumin, and 3.14% for 20 mg L(-1) creatinine. Application of the proposed method to the direct analysis of urinary samples yielded results which agreed with those obtained from the Bradford protein assay and a creatinine enzymatic assay according to a paired t-test. The results obtained should be a step towards developing a fully automated and reliable analytical system for clinical research, which requires direct determination of albumin and creatinine and/or its ratios.

  14. Experimental and DFT study on complexation of the strontium cation with cyclosporin A

    Science.gov (United States)

    Makrlík, Emanuel; Böhm, Stanislav; Vaňura, Petr

    2015-11-01

    By using extraction experiments and γ-activity measurements, the extraction constant corresponding to the equilibrium Sr2+(aq) + 2A-(aq) + 1(nb) ⇄ 1·Sr2+(nb) + 2A-(nb) occurring in the two-phase water-nitrobenzene system (A- = picrate, 1 = cyclosporin A; aq = aqueous phase, nb = nitrobenzene phase) was evaluated as log Kex (1·Sr2+,2A-) = 0.1 ± 0.1. Further, the stability constant of the 1·Sr2+ complex in nitrobenzene saturated with water was calculated for a temperature of 25 °C: log βnb (1·Sr2+) = 9.2 ± 0.1. Finally, applying quantum mechanical DFT calculations, the most probable structure of the proven 1·Sr2+ cationic complex was derived. In the resulting complex, the "central" cation Sr2+ is bound by five bonds to the corresponding five oxygen atoms of the parent cyclosporin A ligand. The interaction energy, E(int), of the investigated 1·Sr2+ complex, involving the 7-point correction for the basis set superposition error, was calculated as -894.5 kJ/mol.

  15. Distribution and Adsorption of Ionic Species into a Liposome Membrane and Their Dependence upon the Species and Concentration of a Coexisting Counterion.

    Science.gov (United States)

    Murakami, Koji; Hori, Kisho; Maeda, Kohji; Fukuyama, Mao; Yoshida, Yumi

    2016-10-10

    The distribution of ions into a bilayer lipid membrane (BLM) and their adsorption on the BLM are investigated by extracting a hydrophobic cation, rhodamine 6G (R6G(+)), into a liposome through the dialysis membrane method. R6G(+) distribution mainly depends upon the concentration of the coexisting anion and its species (Cl(-), Br(-), BF4(-), ClO4(-), and picrate). On the other hand, R6G(+) adsorption on the BLM surface follows the Langmuir adsorption model and is independent of the coexisting anion in the aqueous phase. We propose an extraction model of ionic species into the BLM, to explain the dependence of extraction of ionic species upon the coexisting anion. In this model, an ion is distributed with a coexisting counterion into the BLM and then forms an ion pair in the BLM. Here, the ion adsorption equilibrium on the BLM surface is independent of the species and concentration of the coexisting counterion under the same ionic strength. On the basis of this model, we estimate the distribution constant of R6G(+) and anion (KD), the ion-pair formation constant in the BLM (Kip), and the R6G(+) adsorption constant on the BLM surface (Kad). Even for an ultrathin membrane system, such as a BLM, R6G(+) is distributed with a coexisting counterion and the distribution equilibrium of the ionic species at the water-BLM interface is analyzable similar to that at the water-organic solvent interface.

  16. Junction properties and conduction mechanism of new terbium complexeswith triethylene glycol ligand for potential application in organic electronic device

    Institute of Scientific and Technical Information of China (English)

    N.K.Za’aba1; M.A. Mohd Sarjidan; W.H.Abd. Majid; Eny Kusrini; Muhammad I.Saleh

    2014-01-01

    Terbium-picrate triethylene glycol (EO3-Tb-Pic) complex was prepared in thin film and single layer device structure of ITO/EO3-Tb-Pic/Al, using spin coating technique. The UV-Vis absorption spectroscopy analysis was performed to evaluate the elec-tronic molecular transition of the complex. The optical band gap, Eg estimated from the Tauc model revealed that EO3-Tb-Pic thin film exhibited a direct transition with Eg of 2.70 eV. The electronic parameters of the ITO/EO3-Tb-Pic/Al device such as the ideality factor n, barrier heightΦb, saturation current Io, and series resistance Rs, were extracted from the conventional lnI-V, Cheung’s func-tions and Norde’s method. It was found that the evaluated parameters calculated from Norde’s and Cheung’s methods were consistent with those calculated from the conventional I-V method. In the double logarithmic I-V plot, three distinct regions based on the slope were identified, and the conduction mechanisms were discussed and explained. The mobility,μvalue was estimated from SCLC re-gion as 2.58×10-7 cm2/(V·s). This newly obtained lanthanide complex may be potentially utilized in electronic devices.

  17. Glass distilling collector applied for HCN recovery from submerged culture broth and fruiting body of Pleurotus eryngii for identification and quantification.

    Science.gov (United States)

    Chou, Pei-Yu; Hong, Chian-Huei; Chen, Wenlung; Li, Yu-Jang; Chen, Yen-Shang; Chiou, Robin Y-Y

    2006-03-08

    Detection and surveillance of food commodities containing cyanide is a crucial issue of food safety. In this study, five strains of Pleurotus eryngii (P. eryngii) were grown in submerged culture of yeast malt broth (YMB) with the suspected production of HCN. A safety-warranted U-bent glass distilling collector with three enlarged bulbs on each arm was designed to recover the broth vapor. When AgNO(3) solution was used as an absorbent to interact with the vapor, a white precipitate was formed. The precipitate was isolated and identified as AgCN by FT-Raman spectroscopic analysis. When the absorbent was substituted by KOH, after evaporation to dryness, dissolved in D(2)O, and followed by (13)C-NMR analysis, a KCN spectrum was achieved. Formation of AgCN and KCN confirmed HCN production in the broth by P. eryngii. When a sodium picrate solution (1.4%) was used as an absorbent and various authentic KCN solutions were applied for distillation and followed by absorbance determination at 510 nm, a linear dose-dependent relationship was obtained and the procedure was applied for HCN quantification of the marketed P. eryngii mushrooms (fruiting body). As estimated, 67.3% of the products contained HCN less than 1.0 mg/kg, 17.3% between 1.0 and 2.0 mg/kg, and 15.4% higher than 2.0 mg/kg. When the mushrooms were sliced and cooked in water at 95 degrees C for 6 min, 89.1% of the original HCN was lost. When the P. eryngii strains were respectively grown by submerged cultivation in YMB or YMB supplemented with 2.5% glycine for 16 days, HCN content was slightly higher in the latter than in the former for each strain.

  18. Synthesis and structure elucidation of new μ-oxamido-bridged dicopper(II) complex with in vitro anticancer activity: A combined study from experiment verification and docking calculation on DNA/protein-binding property.

    Science.gov (United States)

    Zhu, Ling; Zheng, Kang; Li, Yan-Tuan; Wu, Zhi-Yong; Yan, Cui-Wei

    2016-02-01

    A new oxamido-bridged dicopper(II) complex with formula of [Cu2(deap)(pic)2], where H2deap and pic represent N,N'-bis[3-(diethylamino)propyl]oxamide and picrate, respectively, was synthesized and characterized by elemental analyses, molar conductance measurements, IR and electronic spectral study, and single-crystal X-ray diffraction. The crystal structure analyses revealed that the two copper(II) atoms in the dicopper(II) complex are bridged by the trans-deap(2-) ligand with the distances of 5.2116(17)Å, and the coordination environment around the copper(II) atoms can be described as a square-planar geometry. Hydrogen bonding and π-π stacking interactions link the dicopper(II) complex into a three-dimensional infinite network. The DNA/protein-binding properties of the complex are investigated by molecular docking and experimental assays. The results indicate that the dicopper(II) complex can interact with HS-DNA in the mode of intercalation and effectively quench the intrinsic fluorescence of protein BSA by 1:1 binding with the most possible binding site in the proximity of Trp134. The in vitro anticancer activities suggest that the complex is active against the selected tumor cell lines, and IC50 values for SMMC-7721 and HepG2 are lower than cisplatin. The effects of the electron density distribution of the terminal ligand and the chelate ring arrangement around copper(II) ions bridged by symmetric N,N'-bis(substituted)oxamides on DNA/BSA-binding ability and in vitro anticancer activity are preliminarily discussed.

  19. A genome scan for quantitative trait loci affecting cyanogenic potential of cassava root in an outbred population

    Directory of Open Access Journals (Sweden)

    Boonseng Opas

    2011-05-01

    Full Text Available Abstract Background Cassava (Manihot esculenta Crantz can produce cyanide, a toxic compound, without self-injury. That ability was called the cyanogenic potential (CN. This project aimed to identify quantitative trait loci (QTL associated with the CN in an outbred population derived from 'Hanatee' × 'Huay Bong 60', two contrasting cultivars. CN was evaluated in 2008 and in 2009 at Rayong province, and in 2009 at Lop Buri province, Thailand. CN was measured using a picrate paper kit. QTL analysis affecting CN was performed with 303 SSR markers. Results The phenotypic values showed continuous variation with transgressive segregation events with more (115 ppm and less CN (15 ppm than either parent ('Hanatee' had 33 ppm and 'Huay Bong 60' had 95 ppm. The linkage map consisted of 303 SSR markers, on 27 linkage groups with a map that encompassed 1,328 cM. The average marker interval was 5.8 cM. Five QTL underlying CN were detected. CN08R1from 2008 at Rayong, CN09R1and CN09R2 from 2009 at Rayong, and CN09L1 and CN09L2 from 2009 at Lop Buri were mapped on linkage group 2, 5, 10 and 11, respectively. Among all the identified QTL, CN09R1 was the most significantly associated with the CN trait with LOD score 5.75 and explained the greatest percentage of phenotypic variation (%Expl. of 26%. Conclusions Five new QTL affecting CN were successfully identified from 4 linkage groups. Discovery of these QTL can provide useful markers to assist in cassava breeding and studying genes affecting the trait.

  20. Synthesis, characterization, and energetic properties of salts of the 1-cyanomethyl-1,1-dimethylhydrazinium cation.

    Science.gov (United States)

    Miró Sabaté, Carles; Delalu, Henri; Jeanneau, Erwann

    2012-05-01

    1,1-Dimethylhydrazine can be readily alkylated with bromoacetonitrile to form 1-cyanomethyl-1,1-dimethylhydrazinium bromide ([(CH(3))(2)N(CH(2)CN)NH(2)]Br, 1). The metathesis reaction of compound 1 led to the formation of a new family of energetic salts based on the [(CH(3))(2)N(CH(2)CN)NH(2)](+) cation and nitrate (2), perchlorate (3), azide (4), 5-aminotetrazolate ([H(2)N-CN(4)](-), 5), 5,5'-azobistetrazolate ([N(4)C-N=N-CN(4)](2-), 7), and picrate (8) anions. The new materials were characterized by elemental analysis, mass spectrometry, and (multinuclear) NMR and vibrational (infrared and Raman) spectroscopies. Additionally, the molecular structure of the [(CH(3))(2)N(CH(2)CN)NH(2)](+) cation in compounds 1, 3, and 8 and that of sodium 5,5'-azobistetrazolate octahydrate (NaZT·8H(2)O) were solved by X-ray diffraction techniques. The hydrogen-bonding networks found in the structure of salts 1, 3, 8, and NaZT·8H(2)O are described using graph-set analysis. The melting and decomposition points of the new compounds were determined by differential scanning calorimetry, and insight into their sensitivity towards impact, friction, and electrostatics was gained by submitting the materials to standard tests. Furthermore, we estimated some performance parameters of interest and predicted the decomposition gases formed upon decomposition of salts 2-8 and of mixtures with an oxidizer. The interesting thermal, sensitivity, and performance properties of some of the compounds described in this work make them attractive towards a prospective energetic application.

  1. A genome scan for quantitative trait loci affecting cyanogenic potential of cassava root in an outbred population

    Science.gov (United States)

    2011-01-01

    Background Cassava (Manihot esculenta Crantz) can produce cyanide, a toxic compound, without self-injury. That ability was called the cyanogenic potential (CN). This project aimed to identify quantitative trait loci (QTL) associated with the CN in an outbred population derived from 'Hanatee' × 'Huay Bong 60', two contrasting cultivars. CN was evaluated in 2008 and in 2009 at Rayong province, and in 2009 at Lop Buri province, Thailand. CN was measured using a picrate paper kit. QTL analysis affecting CN was performed with 303 SSR markers. Results The phenotypic values showed continuous variation with transgressive segregation events with more (115 ppm) and less CN (15 ppm) than either parent ('Hanatee' had 33 ppm and 'Huay Bong 60' had 95 ppm). The linkage map consisted of 303 SSR markers, on 27 linkage groups with a map that encompassed 1,328 cM. The average marker interval was 5.8 cM. Five QTL underlying CN were detected. CN08R1from 2008 at Rayong, CN09R1and CN09R2 from 2009 at Rayong, and CN09L1 and CN09L2 from 2009 at Lop Buri were mapped on linkage group 2, 5, 10 and 11, respectively. Among all the identified QTL, CN09R1 was the most significantly associated with the CN trait with LOD score 5.75 and explained the greatest percentage of phenotypic variation (%Expl.) of 26%. Conclusions Five new QTL affecting CN were successfully identified from 4 linkage groups. Discovery of these QTL can provide useful markers to assist in cassava breeding and studying genes affecting the trait. PMID:21609492

  2. Characterization of GABA/sub A/ receptor-mediated /sup 36/chloride uptake in rat brain synaptoneurosomes

    Energy Technology Data Exchange (ETDEWEB)

    Luu, M.D.; Morrow, A.L.; Paul, S.M.; Schwartz, R.D.

    1987-09-07

    ..gamma..-Aminobutyric acid (GABA) receptor-mediated /sup 36/chloride (/sup 36/Cl/sup -/) uptake was measured in synaptoneurosomes from rat brain. GABA and GABA agonists stimulated /sup 36/Cl/sup -/ uptake in a concentration-dependent manner with the following order of potency: Muscimol>GABA>piperidine-4-sulfonic acid (P4S)>4,5,6,7-tetrahydroisoxazolo-(5,4-c)pyridin-3-ol (THIP)=3-aminopropanesulfonic acid (3APS)>>taurine. Both P4S and 3APS behaved as partial agonists, while the GABA/sub B/ agonist, baclofen, was ineffective. The response to muscimol was inhibited by bicuculline and picrotoxin in a mixed competitive/non-competitive manner. Other inhibitors of GABA receptor-opened channels or non-neuronal anion channels such as penicillin, picrate, furosemide and disulfonic acid stilbenes also inhibited the response to muscimol. A regional variation in muscimol-stimulated /sup 36/Cl/sup -/ uptake was observed; the largest responses were observed in the cerebral cortex, cerebellum and hippocampus, moderate responses were obtained in the striatum and hypothalamus and the smallest response was observed in the pons-medulla. GABA receptor-mediated /sup 36/Cl/sup -/ uptake was also dependent on the anion present in the media. The muscinol response varied in media containing the following anions: Br/sup -/>Cl/sup -/greater than or equal toNO/sub 3//sup -/>I/sup -/greater than or equal toSCN/sup -/>>C/sub 3/H/sub 5/OO/sup -/greater than or equal toClO/sub 4//sup -/>F/sup -/, consistent with the relative anion permeability through GABA receptor-gated anion channels and the enhancement of convulsant binding to the GABA receptor-gated Cl/sup -/ channel. 43 references, 4 figures, 3 tables.

  3. Estimation of Critical Temperature of Thermal Explosion for Nitrosubstituted Azetidines Using Non-isothermal DSC

    Institute of Scientific and Technical Information of China (English)

    HU, Rongzu; ZHAO, Fengqi; GAO, Hongxu; ZHANG, Jiaoqiang; ZHANG, Hai; MA, Haixia

    2009-01-01

    Based on reasonable hypothesis, two general expressions and their six derived formulae for estimating the critical temperature (T_b) of thermal explosion for energetic materials (EM) were derived from the Semenov's thermal explosion theory and eight non-isothermal kinetic equations. We can easily obtain the values of the initial temperature (T_(0i)) at which DSC curve deviates from the baseline of the non-isothermal DSC curve of EM, the onset temperature (T_(ei)), the exothermic decomposition reaction kinetic parameters and the values of T_(00) and T_(e0) from the equation T_(0i or ei)=T_(00 or e0)+α_1β_i+α_2β_i~2+…+α_(L-2)β_i~(L-2), i=1,2,…,L and then calculate the values of T_b by the six derived formulae. The T_b values for seven nitrosubstituted azetidines, 3,3-dinitroazetidinium nitrate (1), 3,3-dinitroazetidinium picrate (2), 3,3-dinitroazetidinium-3-nitro-1,2,4-triazol-5-onate (3), 1,3-bis(3',3'-dinitro-azetidine group)-2,2-dinitropropane (4), 1-(2',2',2'-trinitroethyi)-3,3-dinitroazetidine (5), 3,3-dinitroazetidinium perchiorate (6) and 1-(3',Y-dinitroazetidineyl)-2,2-dinitropropane (7), obtained with the six derived formulae are agreeable to each other, whose differences are within 1.5%. The results indicate that the heat-resistance stability of the seven nitrosubstituted azetidines decreases in the order 6>7>5>4>3>2>1.

  4. Binding properties of oxacalix[4]arenes derivatives toward metal cations; Interactions entre cations metalliques et derives des oxacalix[4]arenes

    Energy Technology Data Exchange (ETDEWEB)

    Mellah, B

    2006-11-15

    The objective of this work was to establish the binding properties of oxacalix[4]arene derivatives with different numbers of the oxa bridges, functional groups (ketones, pyridine, ester, amide and methoxy) and conformations. Their interactions with alkali and alkaline-earth, heavy and transition metal cations have been evaluated according to different approaches: (i) extraction of corresponding picrates from an aqueous phase into dichloromethane; (ii) determination of the thermodynamic parameters of complexation in methanol and/or acetonitrile by UV-spectrophotometry and micro-calorimetry; (iii) determination of the stoichiometry of the complexes by ESI-MS; (iv) {sup 1}H-NMR titrations allowing to localize the metal ions in the ligand cavity. In a first part dealing on homo-oxacalix[4]arenes, selectivities for Na{sup +}, K{sup +}, Ca{sup 2+}, Pb{sup 2+} and Mn{sup 2+} of ketones derivatives was shown. The presence of oxa bridge in these derivatives increases their efficiency while decreasing their selectivity with respect to related calixarenes. The pyridine derivative prefers transition and heavy metal cations, in agreement with the presence of the soft nitrogen atoms. In the second part, di-oxacalix[4]arene ester and secondary amide derivatives were shown to be less effective than tertiary amide counterparts but to present high selectivities for Li{sup +}, Ba{sup 2+}, Zn{sup 2+} and Hg{sup 2+}. A third part devoted to the octa-homo-tetra-oxacalix[4]arene tetra-methoxy shows that the 1:1 metal complexes formed are generally more stable than those of calixarenes, suggesting the participation of the oxygen atoms of the bridge in the complexation. Selectivity for Cs{sup +}, Ba{sup 2+}, Cu{sup 2+} and Hg{sup 2+} were noted. (author)

  5. Synthesis, characterization and extraction studies of N,N"-bis[1-biphenyl-2-hydroxyimino-2-(4-acetylanilino)-1-ethylidene]-diamines and their homo-and heteronuclear copper(II) complexes

    Indian Academy of Sciences (India)

    Bülent Dede; Fatma Kari̇pci̇n; Mustafa Cengi̇z

    2009-03-01

    A new series of homo- and heteropolynuclear copper(II) complexes of N,N"-bis[1-biphenyl-2-hydroxyimino-2-(4-acetylanilino)-1-ethylidene]-diamines have been prepared and characterized by different physical techniques. The starting point of the research was the reaction of chloroacetyl chloride with biphenyl in the presence of aluminum chloride. 4-Biphenylhydroximoyl chloride was obtained by reacting synthesized 4-(chloroacetyl)biphenyl with alkyl nitrite. Substituted 4-(alkylaminoisonitrosoacetyl) biphenyl (ketooxime) was prepared by reacting 4-biphenylhydroximoyl chloride with 4-aminoacetophenone in EtOH. Homodi-, homotrinuclear and heterodinuclear copper(II) perchlorate complexes of tetradentate Schiff bases which possess N4 donor sets derived from the condensation of 4-(arylaminoisonitrosoacetyl)biphenyl and diamine derivatives were synthesized and characterized. Elemental analysis, FT-IR, ESR, molar conductivity, magnetic moment measurements and thermal analyses studies were utilized for the investigation of the complexes. The free ligands were also characterized by 1H- and 13C-NMR spectra. Elemental analyses, stoichiometric and spectroscopic data of the metal complexes indicated that the metal:ligand ratio of dinuclear copper(II) complexes were found to be 2 : 1 while this ratio was 3 : 2 in trinuclear copper(II) complexes and the metal complexes indicated that the metal ions are coordinated to the oxime and imine nitrogen atoms. The extraction abilities of the novel ligands were also evaluated in chloroform by using several transition metal picrates such as Mn2+, Co2+, Ni2+, Cu2+, Zn2+, Pb2+, Cd2+, Hg2+. It has been observed that both ligands show a high affinity to Cu2+ ions.

  6. A facile low-cost enzymatic paper-based assay for the determination of urine creatinine.

    Science.gov (United States)

    Talalak, Kwanrutai; Noiphung, Julaluk; Songjaroen, Temsiri; Chailapakul, Orawon; Laiwattanapaisal, Wanida

    2015-11-01

    Creatinine is one of many markers used to investigate kidney function. This paper describes a low-cost enzymatic paper-based analytical device (enz-PAD) for determining urine creatinine. The disposable dead volumes of creatinine enzyme reagents from an automatic analyser cassette were utilised. Whatman No. 3 paper was cut into long rectangular shapes (4×40 mm(2)) on which the enzyme reagents, R1 and R2, were adsorbed in two consecutive regions. The assay was performed by immersing test strips into urine samples contained in microwells to allow creatinine in the sample to react with immobilised active ingredients and, then, traverse via capillary action to the detection area where chromogen products accumulated. The method is based on hydrogen peroxide (H2O2) formation via creatinine conversion using creatininase, creatinase, and sarcosine oxidase. The liberated H2O2 reacts with 4-aminophenazone and 2,4,6-triiodo-3-hydroxybenzoic acid to form quinoneimine with a pink-red colour at the detection zone. The linear range of the creatinine assay was 2.5-25 mg dL(-1) (r(2)=0.983), and the detection limit was 2.0 mg dL(-1). The colorimetric enz-PAD for the creatinine assay was highly correlated with a conventional alkaline picrate method when real urine samples were evaluated (r(2)=0.977; n=40). This simple and nearly zero-cost paper-based device provides a novel alternative method for screening urinary creatinine and will be highly beneficial for developing countries.

  7. Recent advances in the molten salt technology for the destruction of energetic materials

    Energy Technology Data Exchange (ETDEWEB)

    Upadhye, R.S.; Watkins, B.E.; Pruneda, C.O.

    1995-11-01

    The DOE has thousands of pounds of energetic materials which result from dismantlement operations at the Pantex Plant. The authors have demonstrated the Molten Salt Destruction (MSD) Process for the treatment of explosives and explosive-containing wastes on a 1.5 kilogram of explosive per hour scale and are currently building a 5 kilogram per hour unit. MSD converts the organic constituents of the waste into non-hazardous substances such as carbon dioxide, nitrogen and water. Any inorganic constituents of the waste, such as binders and metallic particles, are retained in the molten salt. The destruction of energetic material waste is accomplished by introducing it, together with air, into a crucible containing a molten salt, in this case a eutectic mixture of Na, K, and Li carbonates. The following pure component DOE and DoD explosives have been destroyed in LLNL`s experimental unit at their High Explosives Applications Facility (HEAF): ammonium picrate, HMX, K-6, NQ, NTO, PETN, RDX, TATB, and TNT. In addition, the following formulations were also destroyed: Comp B, LX-10, LX-16, LX-17, PBX-9404, and XM46, a US Army liquid gun propellant. In this 1.5 kg/hr unit, the fractions of carbon converted to CO and of chemically bound nitrogen converted to NOx were found to be well below 1T. In addition to destroying explosive powders and molding powders the authors have also destroyed materials that are typical of real world wastes. These include shavings from machined pressed parts of plastic bonded explosives and sump waste containing both explosives and non-explosive debris. Based on the information obtained on the smaller unit, the authors have constructed a 5 kg/hr MSD unit, incorporating LLNL`s advanced chimney design. This unit is currently under shakedown tests and evaluation.

  8. Identification of improvised explosives residues using physical-chemical analytical methods under real conditions after an explosion

    Science.gov (United States)

    Kotrlý, Marek; Mareš, Bohumil; Turková, Ivana; Beroun, Ivo

    2016-05-01

    Within the analysis of cases relating to the use of explosives for crimes, we have experienced a shift from using industrial explosives towards substances made in amateur and illegal way. Availability of industrial explosives is increasingly limited to a narrow sphere of subjects with a relevant permission. Thus, on the part of perpetrators, terrorists, ever greater attention is paid to illegal production of explosives that are easily made from readily available raw materials. Another alarming fact is the availability of information found on the internet. Procedures of preparation are often very simple and do not require even a deeper professional knowledge. Explosive characteristics are not actually accessible for many of these substances (detonation velocity, sensitivity, working capacity, brisance, physical and chemical stability, etc.). Therefore, a project is being implemented, which on grounds of assessment of individual information available in literature and on the internet, aiming at choosing individual areas of potentially abusable substances (e.g. mixtures of nitric acid (98%) with organic substances, mixtures nitromethane and tetranitromethane with organic substances, mixtures of chlorates and perchlorates of alkali metals with organic substances, chemically individual compounds of organic base type of perchloric acid, azides, fulminates, acetylides, picrates, styphnates of heavy metals, etc.). It is directed towards preparation of these explosives also in non-stoichiometric mixtures, conducting test explosives, determination of explosive characteristics (if they are unknown) and analysis of both primary phases and post-blast residues through available analytical techniques, such as gas and liquid chromatography with mass detection, FTIR, micro-Raman spectrometry, electron microscopy with microanalysis and Raman microspectrometry directly in SEM chamber for analysis at the level of individual microparticles. The received characteristics will be used to

  9. Co-existence of Distinct Supramolecular Assemblies in Solution and in the Solid State.

    Science.gov (United States)

    Reddy, G N Manjunatha; Huqi, Aida; Iuga, Dinu; Sakurai, Satoshi; Marsh, Andrew; Davis, Jeffery T; Masiero, Stefano; Brown, Steven P

    2017-02-16

    The formation of distinct supramolecular assemblies, including a metastable species, is revealed for a lipophilic guanosine (G) derivative in solution and in the solid state. Structurally different G-quartet-based assemblies are formed in chloroform depending on the nature of the cation, anion and the salt concentration, as characterized by circular dichroism and time course diffusion-ordered NMR spectroscopy data. Intriguingly, even the presence of potassium ions that stabilize G-quartets in chloroform was insufficient to exclusively retain such assemblies in the solid state, leading to the formation of mixed quartet and ribbon-like assemblies as revealed by fast magic-angle spinning (MAS) NMR spectroscopy. Distinct N-H⋅⋅⋅N and N-H⋅⋅⋅O intermolecular hydrogen bonding interactions drive quartet and ribbon-like self-assembly resulting in markedly different 2D (1) H solid-state NMR spectra, thus facilitating a direct identification of mixed assemblies. A dissolution NMR experiment confirmed that the quartet and ribbon interconversion is reversible-further demonstrating the changes that occur in the self-assembly process of a lipophilic nucleoside upon a solid-state to solution-state transition and vice versa. A systematic study for complexation with different cations (K(+) , Sr(2+) ) and anions (picrate, ethanoate and iodide) emphasizes that the existence of a stable solution or solid-state structure may not reflect the stability of the same supramolecular entity in another phase. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. 急慢性肾衰的指甲肌酐测定与尿视黄醇结合蛋白检测的比较%THE VALUE OF COMPARING MENSTRUATING NAIL CREATININE AND URINE RETINOL-BINDING PROTEIN IN CHRONIC RENAL FAILURE AND ACUTE RENAL FAILURE.

    Institute of Scientific and Technical Information of China (English)

    符克英; 钟路; 占锋

    2001-01-01

    目的:探讨指甲肌酐在鉴别急慢性肾衰的临床意义。方法 指甲肌酐(NCr)应用碱性苦味酸法,尿视黄醇结合蛋白(RBP)应用ELISA法及其与尿肌酐比值。结果 慢性肾衰组(NCr)及健康对照组(NCr)及急性肾衰组(NCr)比较有显著差异(P<0.01)健康对照组(NCr)及急性肾衰组(NCr)比较无显著差异(P>0.05),慢性肾衰组(RBP,RBP/Cr)及急性肾衰组(RBP,RBP/Cr)与健康对照组(RBP,RBP/Cr)比较有显著差异(P<0.01),慢性肾衰组(RBP,RBP/Cr)与急性肾衰组(RBP,RBP/Cr)比较无显著差异(P>0.05)。结论 指甲肌酐含量的测定在鉴别急慢性肾衰中有着重要的临床价值。%Objective:To discuss the clinic significance about nailcreatinine in pa tients of acute renal failure and chronic renal failure.Methods: To use the alkal escent picrate methodology menstruates the nail creatinine(NCr),and to use the E LISA methodology menstruates the retinol-binding protein(RBP),and to use routine methodology menstruates the proportionality between RBP and urine creatinine(RB P/Ucr).Results:In creatinine(NCr),there is a remarkable signific ance between chr onic renal failure group and normal control group ,acute renal failure group(P< 0.01),there is no significance between normal control group and acute renal fail ure(P>0.05),but in RBP,RBP/Ucr,there is a remarkable significance between signi ficance,acute renal failure group and normal control group(P<0.01),there is no significance between in chronic renal failure group and acute renal failure grou p.Conclusions:There is significant value for differentiating chronic renal failure and acute renal failure.

  11. Energetic hydrazine-based salts with nitrogen-rich and oxidizing anions.

    Science.gov (United States)

    Sabaté, Carles Miró; Delalu, Henri; Jeanneau, Erwann

    2012-09-01

    1,1,1-Trimethylhydrazinium iodide ([(CH(3))(3)N-NH(2)]I, 1) was reacted with a silver salt to form the corresponding nitrate ([(CH(3))(3)N-NH(2)][NO(3)], 2), perchlorate ([(CH(3))(3)N-NH(2)][ClO(4)], 3), azide ([(CH(3))(3)N-NH(2)][N(3)], 4), 5-amino-1H-tetrazolate ([(CH(3))(3)N-NH(2)][H(2)N-CN(4)], 5), and sulfate ([(CH(3))(3)N-NH(2)](2)[SO(4)]·2H(2)O, 6·2H(2)O) salts. The metathesis reaction of compound 6·2H(2)O with barium salts led to the formation of the corresponding picrate ([(CH(3))(3)N-NH(2)][(NO(2))(3)Ph-O], 7), dinitramide ([(CH(3))(3)N-NH(2)][N(NO(2))(2)], 8), 5-nitrotetrazolate ([(CH(3))(3)N-NH(2)][O(2)N-CN(4)], 9), and nitroformiate ([(CH(3))(3)N-NH(2)][C(NO(2))(3)], 10) salts. Compounds 1-10 were characterized by elemental analysis, mass spectrometry, infrared/Raman spectroscopy, and multinuclear NMR spectroscopy ((1)H, (13)C, and (15)N). Additionally, compounds 1, 6, and 7 were also characterized by low-temperature X-ray diffraction techniques (XRD). Ba(NH(4))(NT)(3) (NT=5-nitrotetrazole anion) was accidentally obtained during the synthesis of the 5-nitrotetrazole salt 9 and was also characterized by low-temperature XRD. Furthermore, the structure of the [(CH(3))(3)N-NH(2)](+) cation was optimized using the B3LYP method and used to calculate its vibrational frequencies, NBO charges, and electronic energy. Differential scanning calorimetry (DSC) was used to assess the thermal stabilities of salts 2-5 and 7-10, and the sensitivities of the materials towards classical stimuli were estimated by submitting the compounds to standard (BAM) tests. Lastly, we computed the performance parameters (detonation pressures/velocities and specific impulses) and the decomposition gases of compounds 2-5 and 7-10 and those of their oxygen-balanced mixtures with an oxidizer.

  12. Partial crystallization of picritic melt and its applications for the genesis of high-Ti and low-Ti basalts

    Science.gov (United States)

    Yang, J.; WANG, C.; Jin, Z.; Jin, S.; Yan, S.

    2015-12-01

    Geochemical and petrological studies have revealed the existence of high-Ti and low-Ti basalts in large igneous provinces (LIPs). However the originate of these high-Ti and low-Ti magmas are still under debate. Several different mechanisms have been proposed: (1) the high-Ti basalts are formed by the melting of mantle plume containing recycled oceanic crust (Spandler et al., 2008) while low-Ti basalts are formed by the melting of subcontinental lithospheric mantle (Xiao et al., 2004); (2) both high-Ti and low-Ti basalts are from mantle plume source, but the production of high-Ti basalts are associated with the thick lithosphere while the low-Ti basalts are controlled by the thin lithosphere (Arndt et al., 1993); (3) they are derived from the different degrees of melting, with high-Ti basalts representing low degree of partial melting of mantle plume (Xu et al., 2004). The low Mg# (below 0.7) of high-Ti and low-Ti basalts provides that they are far away from direct melting of mantle peridotite. In addition, seismic data indicate unusually high seismic velocities bodies beneath the LIPs which explained by the fractionated cumulates from picritic magmas (Farnetani et al., 1996). Therefore, we believed that the crystallization differentiation process might play a more significant role in the genesis of high-Ti and low-Ti basalts.In order to investigate the generation of high-Ti and low-Ti basalts, a series of high pressure and high temperature partial crystallization experiments were performed at pressures of 1.5, 3.0 and 5.0 GPa and a temperature range of 1200-1700℃. The starting material is picrate glass with relative high TiO2 (2.7 wt %), which is synthesized according to the chemical composition of primary magmas of Emeishan LIP (Xu et al., 2001). The experimental results show that: (1) At a given pressure, the TiO2 content is decreased with increasing melt fraction; (2) At a given melt fraction, the TiO2 content of melts is increased with increasing pressure. On

  13. Simulations of electrolytes at the liquid-liquid interface and of lanthanide cations complexes in gas phase; Simulations d'electrolytes a l'interface liquide/liquide et de complexes de cations lanthanides en phase gazeuse

    Energy Technology Data Exchange (ETDEWEB)

    Berny, F

    2000-07-01

    Two processes related to liquid/liquid extraction of ions by extractant molecules were studied: the ion approach at the interface and the ion complexation by ligands. In the first part, the behaviour of salts at the chloroform/water interface was simulated by molecular dynamics. The aim was to understand the way these salts ions approach the interface in order to be extracted. Some ions are repelled by the interface (K{sup +}, Cl{sup -}, UO{sub 2}{sup 2+}, Na{sup +}, NO{sub 3}{sup -}) whereas others adsorb (amphiphilic molecules and also ClO{sub 4}{sup -}, SCN{sup -}, guanidinium Gu{sup +} and picrate Pic{sup -}). The surface-active counter-ions make the ion approach at the interface easier. In a perfectly homogeneous mixture of the two solvents (water and chloroform) de-mixing, the ions seem to influence the phases separation rate. Nitric acid which is known to favour liquid/liquid extraction reveals strong adsorption at the interface in its neutral form and a smaller one in its ionic form (H{sub 3}O{sup +}/NO{sub 3}{sup -}). HNO{sub 3} and H{sub 3}O{sup +} display particular orientations at the interface: hydrogen atoms are pointing in the direction of the water slab. The nature of the organic phase can also influence the ion approach at the interface. For example, Gu{sup +} and Pic{sup -} adsorb much less at the supercritical CO{sub 2}/water interface than at the chloroform/water interface. In the second part, complexes of La{sup 3+}, Eu{sup 3+} and Yb{sup 3+} with ligands such as amide, urea, thio-amide, thiourea were studied by quantum mechanics. Our calculations show that cation-ligand interactions depend on the nature of substituents on ligands, on the presence of counter-ions or on the number of ligands in the complex. Sulfur compounds seem to less interact with cations than oxygen compounds. Ureas interact as much as amides and are potentially good ligands. (author)

  14. Recent advances in the molten salt destruction of energetic materials

    Energy Technology Data Exchange (ETDEWEB)

    Pruneda, C. O., LLNL

    1996-09-01

    We have demonstrated the use of the Molten Salt Destruction (MSD) Process for destroying explosives, liquid gun propellant, and explosives-contaminated materials on a 1.5 kg of explosive/hr bench- scale unit (1, 2, 3, 4, 5). In our recently constructed 5 kg/hr pilot- scale unit we have also demonstrated the destruction of a liquid gun propellant and simulated wastes containing HMX (octogen). MSD converts the organic constituents of the waste into non-hazardous substances such as carbon dioxide, nitrogen, and water. Any inorganic constituents of the waste, such as metallic particles, are retained in the molten salt. The destruction of energetic materials waste is accomplished by introducing it, together with air, into a vessel containing molten salt (a eutectic mixture of sodium, potassium, and lithium carbonates). The following pure explosives have been destroyed in our bench-scale experimental unit located at Lawrence Livermore National Laboratory`s (LLNL) High Explosives Applications Facility (HEAF): ammonium picrate, HMX, K- 6 (keto-RDX), NQ, NTO, PETN, RDX, TATB, and TNT. In addition, the following compositions were also destroyed: Comp B, LX- IO, LX- 1 6, LX- 17, PBX-9404, and XM46 (liquid gun propellant). In this 1.5 kg/hr bench-scale unit, the fractions of carbon converted to CO and of chemically bound nitrogen converted to NO{sub x} were found to be well below 1%. In addition to destroying explosive powders and compositions we have also destroyed materials that are typical of residues which result from explosives operations. These include shavings from machined pressed parts of plastic-bonded explosives and sump waste containing both explosives and non-explosive debris. Based on the process data obtained on the bench-scale unit we designed and constructed a next-generation 5 kg/hr pilot-scale unit, incorporating LLNL`s advanced chimney design. The pilot unit has completed process implementation operations and explosives safety reviews. To date, in this

  15. Estudos experimentais em coelhos com plantas cianogênicas Experiments in rabbits with cyanogenic plants

    Directory of Open Access Journals (Sweden)

    Marilene F. Brito

    2000-06-01

    well correlated with the picrate test for cyanide.