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Sample records for 1-furfuryl pyrrole characterization

  1. Characterization of poly pyrrole/montmorillonite electro polymerised onto Pt

    In this study films of polypyrrole/montmorillonite (PPy/MT) were electropolymerized on platinum in order to evaluate the performance of this technique in the preparation of nanocomposite materials and to determine the thermal properties and conductivity of the composites. The films were synthesized from a solution containing pyrrole, dodecylbenzene sulfonate, acid and two types of clays: montmorillonite-Na + (MT-Na) and montmorillonite-30B (MT-M). The characterization of the films we have used FT-IR, TEM, XRD, TGA, DSC and resistivity measurement by the four-point van der Pauw method. The study showed that the adopted method of exfoliation and the electropolymerization method used, allows obtaining nanocomposite materials. Analyses of FT-IR, TEM and XRD show that the clays are exfoliated in the polymer matrix. Thermal analysis of the films indicates that the addition of clay reflects an enhancement in the thermal properties of the matrix of PPy, but decreases the conductivity of the same. (author)

  2. Synthesis, Characterization and Biological Study of Novel Pyrrole Derivatives

    Rakesh R. Mishra

    2012-07-01

    Full Text Available A facile condensation of aromatic aldehydes with 2-(5-(phenoxymethyl-2-thioxo-1,3,4-oxadiazol-3(2H-ylaceto hydrazide (1 was give the corresponding N’-aryl-2-(5-(phenoxymethyl-2-thioxo-1,3,4-oxadiazol-3(2H-ylacetohydrazide (2a-e in good yield. Cyclo condensation of compounds (2a-e with maleic anhydride yields 2-aryl-5-oxo-1-(2-(5-(phenoxymethyl-2-thioxo-1,3,4-oxadiazol-3(2H-ylacetamido-2,5-dihydro-1H-pyrrole-3-carboxylic acid (3a-e. The structures of these compounds were established on the basis of analytical and spectral data. All the newly synthesized compounds were evaluated for their antibacterial and antifungal activities.

  3. Synthesis and Physical Characterization of Carbon Nano tubes Coated by Conducting Poly pyrrole

    This study describes the preparation of poly pyrrole multi walled carbon nano tube (PPy/ MWNT) composites by in situ chemical oxidative polymerization. Various ratios of functionalized MWNTs are dispersed in the water, and PPy are then synthesized via in-situ chemical oxidative polymerization on the surface of the carbon nano tubes. The morphology of the resulting complex nano tubes (MWNT-PPY) was characterized by scanning electron microscopy (SEM). The conductivity of each composite showed a maximum in the temperature scale of 120- 160 degree Celsius and then decreased dramatically with the increase of temperature. (author)

  4. -pyrrole substituted porphyrin-pyrene dyads using vinylene spacer: Synthesis, characterization and photophysical properties

    P Silviya Reeta; Ravi Kumar Kanaparthi; L Giribabu

    2013-03-01

    We have designed and synthesized donor-acceptor conjugates having donor pyrene at the pyrrole- position of either free-base porphyrin or Zn(II) porphyrin using vinylene spacer. Both the dyads have been completely characterized by elemental analysis,MALDI-MS, UV-Vis., and fluorescence (steady state and timeresolved) spectroscopies as well as cyclic voltammetry. The absorption maxima of both dyads are red-shifted by 8-12 nm. The ground state properties showed that there exist minimum - interaction between the aromatic subunits of these D-A systems. Quenched emission was observed in both the dyads when excited at 290 nm. The quenched emission explained in terms of intramolecular excitation energy transfer competes with the photo-induced electron transfer reaction in these D-A system.

  5. Synthesis, characterization, molecular docking and biological studies of self assembled transition metal dithiocarbamates of substituted pyrrole-2-carboxaldehyde.

    Nami, Shahab A A; Ullah, Irfan; Alam, Mahboob; Lee, Dong-Ung; Sarikavakli, Nursabah

    2016-07-01

    A series of self assembled 3d transition metal dithiocarbamate, M(pdtc) [where M=Mn(II), Fe(II), Co(II), Ni(II) and Cu(II)] have been synthesized and spectroscopically characterized. The bidentate dithiocarbamate ligand Na2pdtc (Disodium-1,4-phenyldiaminobis (pyrrole-1-sulfino)dithioate) was prepared by insertion reaction of carbondisulfide with Schiff base, N,N'-bis-(1H-pyrrol-2-ylmethylene)-benzene-1,4-diamine (L1) in basic medium. The simple substitution reaction between the metal halide and Na2pdtc yielded the title complexes in moderate yields. However, the in situ procedure gives high yield with the formation of single product as evident by TLC. Elemental analysis, IR, (1)H and (13)C NMR spectra, UV-vis., magnetic susceptibility and conductance measurements were done to characterize the complexes, M(pdtc). All the evidences suggest that the complexes have tetrahedral geometry excepting Cu(II) which is found to be square planar. A symmetrical bidentate coordination of the dithiocarbamato moiety has been observed in all the complexes. The conductivity data show that the complexes are non-electrolyte in nature. The anti-oxidant activity of the ligand, Na2pdtc and its transition metal complexes, M(pdtc) have been carried out using DPPH and Cu(pdtc) was found to be most effective. The anti-microbial activity of the Na2pdtc and M(pdtc) complexes have been carried out and on this basis the molecular docking study of the most effective complex, Cu(pdtc) has also been reported. PMID:27197060

  6. Electrochemical synthesis of Poly[3, 4-Propylenedioxythiophene-co-N-Phenylsulfonyl Pyrrole]: Morphological, electrochemical and spectroscopic characterization

    2011-06-01

    Full Text Available Electroactive random copolymers of 3,4-Propylenedioxythiophene (ProDOT and N-Phenylsulfonyl Pyrrole (PSP were electrochemically synthesized on single carbon fiber microelectrode (SCFME by cyclic voltammetry (CV. Fourier Transform Infrared-Attenuated Total Reflectance (FTIR-ATR measurements indicate the inclusion of PSP into the copolymer structure. The influence of feed ratios on the copolymers was studied by CV and electrochemical impedance spectroscopy (EIS and equivalent circuit modelling (ECM. The morphologies and film thicknesses of copolymers were characterized by scanning electron microscopy (SEM and atomic force microscopy (AFM. The results have shown that the principal changes in morphology, conductivity, porous nature and thickness of Poly(ProDOT-co-PSP film depend on the concentration of PSP. The strong electron-withdrawing sulfonyl group substitution on PSP significantly inhibited electrochemical copolymerization. Semicircular characteristics at Nyquist plots reflected an increasing trend with the increase of PSP concentration in the feed at high frequency. The semicircular characteristic of the copolymer film is useful for the bioelectrochemical sensor applications.

  7. Characterization of poly pyrrole/montmorillonite electro polymerised onto Pt; Caracterizacao de filmes PPy/montmorilonita eletropolimerizados sobre Pt

    Castagno, K.R.L., E-mail: katiarlc@pelotas.ifsul.edu.b [Instituto Federal Sul-rio-grandense (IFSul), RS (Brazil). Dept. de Quimica; Azambuja, D.S.; Dalmoro, V.; Mauller, R.S. [Universidade Federal do Rio Grande do Sul (UFRGS), Pelotas, RS (Brazil). Inst. de Quimica

    2010-07-01

    In this study films of polypyrrole/montmorillonite (PPy/MT) were electropolymerized on platinum in order to evaluate the performance of this technique in the preparation of nanocomposite materials and to determine the thermal properties and conductivity of the composites. The films were synthesized from a solution containing pyrrole, dodecylbenzene sulfonate, acid and two types of clays: montmorillonite-Na + (MT-Na) and montmorillonite-30B (MT-M). The characterization of the films we have used FT-IR, TEM, XRD, TGA, DSC and resistivity measurement by the four-point van der Pauw method. The study showed that the adopted method of exfoliation and the electropolymerization method used, allows obtaining nanocomposite materials. Analyses of FT-IR, TEM and XRD show that the clays are exfoliated in the polymer matrix. Thermal analysis of the films indicates that the addition of clay reflects an enhancement in the thermal properties of the matrix of PPy, but decreases the conductivity of the same. (author)

  8. Synthesis, characterization and anticancer studies of new steroidal oxadiazole, pyrrole and pyrazole derivatives

    Shamsuzzaman

    2015-07-01

    Full Text Available In the present study steroidal derivatives, 3β-[5′-mercapto-1′,3′,4′-oxadiazole-2-yl]methoxy cholest-5-ene 2, 3β-[2′,5′-dimethylpyrrole-1-yl]aminocarbonylmethoxycholest-5-ene 3 and 3β-[3′,5′-dimethyl pyrazole-1-yl]carbonylmethoxycholest-5-ene 4 have been synthesized from cholest-5-en-3β-O-acetyl hydrazide 1 using CS2/KOH, acetonyl acetone and acetyl acetone, respectively as reagents and are characterized by IR, 1H NMR,13C NMR, MS and elemental analysis. Compounds 2–4 were also evaluated for anticancer activity against human leukemia cell line (HL-60 by MTT assay and compound 4 displayed the promising behavior by showing better anticancer activity.

  9. The Oxidation of Pyrrole.

    Howard, James K; Rihak, Kieran J; Bissember, Alex C; Smith, Jason A

    2016-01-01

    The dearomatization of heterocycles has been a powerful means for producing functional molecules in synthesis. In the case of pyrroles, reductive methods (such as the Birch reduction) have been most widely exploited, while oxidative methods are generally dismissed as too difficult or unpredictable to be useful. However, since the early twentieth century considerable research has been carried out on the controlled oxidation of pyrroles to give highly functionalized products, using a variety of oxidants. This review presents a summary of all work up until the present day in the area of pyrrole oxidation, looking at the use of peroxide, singlet oxygen, hypervalent iodine reagents, a range or organic and inorganic oxidants, and electrochemical approaches. It also offers some perspective on the potential future role of pyrrole oxidation in synthesis. PMID:26294175

  10. Flexible supercapacitor based on electrochemically synthesized pyrrole formyl pyrrole copolymer coated on carbon microfibers

    Gholami, Mehrdad; Moozarm Nia, Pooria; Narimani, Leila; Sokhakian, Mehran; Alias, Yatimah

    2016-08-01

    The main objective of this work is to prepare a flexible supercapacitor using electrochemically synthesized pyrrole formyl pyrrole copolymer P(Py-co-FPy) coated on the carbon microfibers. Due to difficulties of working with carbon microfibers, glassy carbon was used to find out optimized conditions by varying mole ratio of pyrrole and formyl pyrrole monomers on the capacitance value. The prepared electrodes were characterized using Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscope (FESEM), Brunauer-Emmett-Teller (BET) analysis, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Then the X-ray photoelectron spectroscopy (XPS) was used to characterize the optimized electrode. The specific capacitance is calculated using cyclic voltammetry, charge/discharge method, and impedance spectroscopy. The charge/discharge study reveals that the best specific capacitance is estimated to be 220.3 mF cm-2 for equal mole fraction of pyrrole and formyl pyrrole Py (0.1)-FP (0.1) at discharge current of 3 × 10-4 A. This optimized electrode keeps about 92% of its capacitance value in high current of discharging. The specific capacitances calculated by all the mentioned methods are in agreement with each other. Finally, the found optimized conditions were successfully applied to produce a flexible supercapacitor on the surface of carbon microfibers.

  11. Characterization of electro-conductive fabrics prepared by in situ chemical and electrochemical polymerization of pyrrole onto polyester fabric

    Highlights: • Surface resistivity of the fabrics decreased rapidly with an increase in add-on. • Add-on and resistivity were not correlated below a resistivity value of about 200 Ω. • Higher add-on but lower surface roughness resulted in lower surface resistivity. • The voltage–current and voltage–temperature behaviours were found to be non-linear. • Electro-conductive fabric exhibited 98% electromagnetic shielding efficiency. - Abstract: This paper reports a study on electro-conductive fabrics prepared by a combined in situ chemical and electrochemical polymerization of pyrrole. Specific observations are made to establish the roles of add-on and surface roughness on the surface resistivity of the electro-conductive fabrics. The performance characteristics of the fabrics are reported in terms of electrical conductivity, voltage–current and voltage–temperature characteristics and electromagnetic interference (EMI) shielding capability. The surface resistivity of the fabric was found to be as low as 11.79 Ω. The voltage–current profile of the fabric is observed to be non-ohmic as well as the voltage–temperature curve is found to be exponential. The EMI shielding efficiency of the fabric was found to be about 98%

  12. Characterization of electro-conductive fabrics prepared by in situ chemical and electrochemical polymerization of pyrrole onto polyester fabric

    Maiti, Syamal; Das, Dipayan; Sen, Kushal, E-mail: kushal@textile.iitd.ernet.in

    2014-09-15

    Highlights: • Surface resistivity of the fabrics decreased rapidly with an increase in add-on. • Add-on and resistivity were not correlated below a resistivity value of about 200 Ω. • Higher add-on but lower surface roughness resulted in lower surface resistivity. • The voltage–current and voltage–temperature behaviours were found to be non-linear. • Electro-conductive fabric exhibited 98% electromagnetic shielding efficiency. - Abstract: This paper reports a study on electro-conductive fabrics prepared by a combined in situ chemical and electrochemical polymerization of pyrrole. Specific observations are made to establish the roles of add-on and surface roughness on the surface resistivity of the electro-conductive fabrics. The performance characteristics of the fabrics are reported in terms of electrical conductivity, voltage–current and voltage–temperature characteristics and electromagnetic interference (EMI) shielding capability. The surface resistivity of the fabric was found to be as low as 11.79 Ω. The voltage–current profile of the fabric is observed to be non-ohmic as well as the voltage–temperature curve is found to be exponential. The EMI shielding efficiency of the fabric was found to be about 98%.

  13. Design, spectral characterization, DFT and biological studies of transition metal complexes of Schiff base derived from 2-aminobenzamide, pyrrole and furan aldehyde

    Tyagi, Prateek; Chandra, Sulekh; Saraswat, B. S.; Sharma, Deepansh

    2015-05-01

    A series of two biologically active Schiff base ligands L1, L2 have been synthesized in equimolar reaction of 2-aminobenzamide with pyrrol-2-carboxaldehyde and furan-2-carboxaldehyde. The synthesized Schiff bases were used for complexation with different metal ions like Co(II), Ni(II) and Cu(II) by using a molar ratio of ligand: metal as 2:1. The characterization of newly formed complexes was done by 1H NMR, UV-Vis, TGA, IR, mass spectrophotometry, EPR and molar conductivity studies. The thermal studies suggested that the complexes are more stable as compared to ligand. In DFT studies the geometries of Schiff bases and metal complexes were fully optimized with respect to the energy using the 6-31+g(d,p) basis set. On the basis of the spectral studies an octahedral geometry has been assigned for Co(II) and Ni(II) complexes and distorted octahedral geometry for Cu(II) complexes. All the synthesized compounds, were studied for their in vitro antimicrobial activities, against four bacterial strains and two fungal strains by using serial dilution method. The data also revealed that the metal complexes showed better activity than the ligands due to chelation/coordination.

  14. Synthesis and characterization of new electron-withdrawing moiety thieno[2,3-c]pyrrole-4,6-dione-based molecules for small molecule solar cells

    Fu, Lei; Pan, Hongbin; Larsen-Olsen, Thue Trofod;

    2013-01-01

    –π–donor–π–acceptor type end-capped with thieno[2,3-c]pyrrole-4,6-dione (TPD) units for small molecule solar cells have been prepared through coupling of dithienosilole and TPD units bridged with thienylene and bithienylene. They are soluble in common organic solvents and show an interesting absorption. These small...

  15. Synthesis, characterization and computational study on ethyl 4-(3-Furan-2yl-acryloyl)-3,5-dimethyl-1H-pyrrole-2-carboxylate

    Singh, R. N.; Rawat, Poonam; Sahu, Sangeeta

    2014-11-01

    As part of study on pyrrole derivatives, we have synthesized a pyrrole chalcone derivative: ethyl 4-(3-Furan-2yl-acryloyl)-3,5-dimethyl-1H-pyrrole-2-carboxylate (EFADPC) by aldol condensation of ethyl 3, 5-dimethyl-4-actyl-1H-pyrrole-2-carboxylate with furan-2-carbaldehyde in the presence of strong hydroxyl base as catalyst. The product EFADPC has been confirmed by spectroscopic (FT-IR, 1H NMR, and UV-visible) analyses. Quantum chemical calculation also provides good correlation with experimental data. The molecular electrostatic potential surface (MEP), natural bond orbital interactions (NBO), electronic descriptors, quantum theory of atoms' in molecules (QTAIM) and experimental FT-IR spectrum have been used to predict the sites and nature of interactions which indicate that the dimer formation with multiple interactions through Nsbnd H···O and Csbnd H···O. The vibrational analysis shows red shifts in νNsbnd H and νCdbnd O as result of dimer formation. The binding energy of dimer is calculated as 13.82, 15.24 kcal/mol using DFT, QTAIM analysis, respectively. The result of ellipticity confirms the existence of resonance assisted hydrogen bonds (RAHB) in dimer. The MEP and local reactivity descriptors analyses have been performed and the results indicate that carbonyl carbon and β-carbon of chalcone frame have been prone to nucleophilic attack and lead to large number of heterocyclic compounds such as oxirane, oxazoles, pyrazoles, pyridines, pyrimidines, and pyran.

  16. Preparation of ultrathin pyrrolic conductor films as backings of radioactive sources

    A procedure for electropolymerization of pyrrole has been set up in order to produce thin (> 15 μ g/cm2) homogeneous (thickness variation 2. The experimental equipment, reagent and procedure utilized is described as well as the characterization pyrrolic films produced

  17. Synthesis of new pyrrole-containing biomolecules as building blocks for functionalized polypyrroles in nanobiotechnology

    New pyrroles were synthesized wherein biomolecules such as α-amino acids, peptides or carbohydrates are attached to position 1 or 3 via suitable linkers. These conjugates were copolymerized with pyrrole by chemical polymerisation alone giving corresponding copolymers or in the presence of magnetic iron oxid nanoparticles resulting in functionalized core-shell-nanoparticles. Such products are interesting for biosensing, imaging or separation of biomaterials. They were characterized by several methods such as TEM, HRTEM, FTIR and measuring of magnetization.

  18. Study on the nature of interaction of pyrrole with various hydrides

    Graphical abstract: The equilibrium geometries of the pyrrole-HnX (X=F, O, N, Cl, S and P) complexes are shown in above figure. These geometries are classified as N-H...X type and H-π-type (also referred to in this paper as geometry types I and II, respectively). The N-H...X type geometry features a hydrogen bond formed between the hydrogen atom of pyrrole and X atom of HnX, and has C1 symmetry. The π-type geometry is characterized by an H-π bond formed between a hydrogen atom of HnX and the π-electron system of the aromatic ring, and has C1 symmetry. For the pyrrole-HF, H2O, NH3, H2S and -PH3 complexes have N-H...X type and π-type. For the pyrrole-HCl complexes have only H-π-type. Display Omitted Highlights: → We investigated the intermolecular interaction of pyrrole with the various hydrides. → There are N-H...X and H-π-type hydrogen-bonding complexes. → With the exception of pyrrole-H2O and pyrrole-NH3 complexes, all of the other pyrrole-HnX complexes favors π-type H-bonding. → The electrostatic and dispersion interactions dominate the H-π-type complexes. - Abstract: Equilibrium geometries, interaction energies, atomic charge, and charge transfer for the N-H...X and H-π-type hydrogen-bonding complexes between pyrrole and various hydrides HnX (X=F, O, N, Cl, S, and P) were studied at the MP2/aug-cc-pVDZ level. With the exception of pyrrole-H2O and pyrrole-NH3 complexes, all of the other pyrrole-HnX complexes favors π-type H-bonding. To further study the nature of the π-type H-bonding, an SAPT (the symmetry adapted perturbation theory) energy decomposition analysis was carried out and the results indicate that the electrostatic and dispersion interactions dominate the H-π-type complexes.

  19. Syntheses of Calix[4]Pyrroles by Amberlyst-15 Catalyzed Cyclocondensations of Pyrrole with Selected Ketones

    Tanuja Bisht

    2007-11-01

    Full Text Available A facile and efficient protocol is reported for the synthesis of calix[4]pyrrolesand N-confused calix[4]pyrroles in moderate to excellent yields by reaction of dialkyl orcycloalkyl ketones with pyrrole catalyzed by reusable AmberlystTM-15 under eco-friendlyconditions.

  20. Synthesis of hollow poly(aniline-co-pyrrole)-Fe3O4 composite nanospheres and their microwave absorption behavior

    Zhu, Yao-Feng; Zhang, Li; Natsuki, Toshiaki; Fu, Ya-Qin; Ni, Qing-Qing

    2012-01-01

    Hollow poly(aniline-co-pyrrole)-Fe3O4 (HPAP-Fe3O4) nanospheres with significant electromagnetic properties were successfully prepared via the oxidative polymerization of a mixture of aniline and pyrrole in the presence of a magnetic fluid, using a non-ionic surfactant as a template. The products were characterized by field emission scanning electron microscopy, transmission electron microscopy. Fourier transform infrared spectroscopy, X-ray powder diffraction, thermogravimetric analysis and X...

  1. Electrophilic surface sites as precondition for the chemisorption of pyrrole on GaAs(001) surfaces

    We report how the presence of electrophilic surface sites influences the adsorption mechanism of pyrrole on GaAs(001) surfaces. For this purpose, we have investigated the adsorption behavior of pyrrole on different GaAs(001) reconstructions with different stoichiometries and thus different surface chemistries. The interfaces were characterized by x-ray photoelectron spectroscopy, scanning tunneling microscopy, and by reflectance anisotropy spectroscopy in a spectral range between 1.5 and 5 eV. On the As-rich c(4 × 4) reconstruction that exhibits only nucleophilic surface sites, pyrrole was found to physisorb on the surface without any significant modification of the structural and electronic properties of the surface. On the Ga-rich GaAs(001)-(4 × 2)/(6 × 6) reconstructions which exhibit nucleophilic as well as electrophilic surface sites, pyrrole was found to form stable covalent bonds mainly to the electrophilic (charge deficient) Ga atoms of the surface. These results clearly demonstrate that the existence of electrophilic surface sites is a crucial precondition for the chemisorption of pyrrole on GaAs(001) surfaces

  2. Pyrrole-added Fe2O3 films by ultrasonic spray pyrolisis

    Carlos Torres Frausto; Alejandro Avila Garcia

    2009-01-01

    Fe2O3 thin films were grown by Ultrasonic Spray Pyrolisis from a 0.05 aqueous solution of FeCl3 added with a small amount of pyrrole monomer. Films at different substrate temperature and pyrrole content were grown. They were characterized by using x-ray diffraction (XRD), infrared spectroscopy (FTIR) and atomic force microscopy (AFM). Results indicated that at low substrate temperature (approximately 200ºC) the films mainly resemble the polypyrrole structure. At higher temperatures up to 400...

  3. Tris[2-(pyrrol-2-ylmethyleneaminoethyl]amine

    Hongbing Fu

    2008-03-01

    Full Text Available The title compound, C21H27N7, was synthesized by reaction of tris(2-aminoethylamine and pyrrole-2-carbaldehyde in ethanol at room temperature. The structure is stabilized by intra- and intermolecular C—H...N and N—H...N hydrogen-bonding interactions.

  4. Synthesis, autoxidation and photooxidation of hindered pyrrole derivatives. Hindered pyrrolic nitroxide radicals

    2,5-di-t-butyl and 2,3,5-tri-t-butyl pyrrole are prepared from pinacoline and their structure is confirmed by comparison with 2,5-di-t-butyl furan and thiophene (I.R., U.V. and N.M.R. 13C satellites observation giving J13C-H and JH3-H4). The sensitized photooxidation of these hindered pyrroles gives corresponding hydroperoxides which most likely structure is determined using physical and chemical methods. Oxidation of 2,5-di-t-butyl and 2,3,5-tri-t-butyl pyrrole by hydrogen peroxide in presence of inorganic per-acid of by p-nitro-perbenzoic acid does not give the pyrrolic nitroxides in contrast with secondary amines. Some N-hydroxypyrroles are then prepared from pinacoline and ethyl pivaloyl-acetate. Their oxidation by lead dioxide gives the corresponding pyrrolic nitroxides. 2,5-di-t-butyl 3,4-di-ethoxycarbonyl pyrryl 1-oxy is isolated and studied spectroscopically (visible and U.V., E.P.R.). In marked contrast with ordinary nitroxides it does not show solvent effect. It can be compared with 2,4-di-t-butyl cyclopentadienone, a carbon analog. For both, the long wave length transition does not show the usual n - π* behaviour; that is confirmed by E.P.R. Using Huckel method for pyrrolic nitroxide skeleton, it is possible to have a good interpretation of experimental data. (author)

  5. The electrochemical synthesis of poly(pyrrole-co-o-anisidine) on 3102 aluminum alloy and its corrosion protection properties

    Mert, B. Dogru, E-mail: bdogru@cu.edu.tr [Cukurova University, Science and Letters Faculty, Chemistry Department, 01330 Balcali, Adana (Turkey); Yazici, B. [Cukurova University, Science and Letters Faculty, Chemistry Department, 01330 Balcali, Adana (Turkey)

    2011-02-15

    Research highlights: {yields} The electrochemical synthesis of strongly adherent, uniform polypyrrole (PPy) and poly(pyrrole-co-o-anisidine) coatings were successfully achieved on 3102 aluminum alloy from 0.1 M monomer (pyrrole and pyrrole:o-anisidine, 8:2) containing oxalic acid by means of the cyclic voltammetry technique. {yields} The results were showed that the water permeation of copolymer coating is lower than PPy. {yields} This study was showed that copolymer is suitable coating for protection of 3102 Al alloy against corrosion. - Abstract: The electrochemical syntheses of polypyrrole (PPy) and poly(pyrrole-co-o-anisidine) were achieved on 3102 aluminum alloy (Al) from 0.1 M monomer (pyrrole:o-anisidine, 8:2) containing 0.4 M oxalic acid solution using the cyclic voltammetry technique. The synthesized films were characterized by FT-IR spectroscopy. The thermal stability of films was determined by thermogravimetric analysis (TGA) technique. Surface morphologies were characterized by scanning electron microscope (SEM) images. The potential of zero charge (pzc) of Al was determined using electrochemical impedance spectroscopy (EIS). The corrosion behavior of samples was investigated with open circuit potential (E{sub ocp})-time, EIS, and anodic polarization techniques. It was found that copolymer coated Al provides better barrier property against of corrosion in 3.5% NaCl solution.

  6. Preparation of conductive membranes using poly pyrrole

    Conductive membranes show many benefits including fouling reduction for feeds containing ionic species. These membranes may be prepared either by conductive polymers or coating of the surfaces of non-conductive membranes with conductive polymer. In this research, the commercial micro filtration GVHP membrane manufactured from PVDF was coated with poly pyrrole using two different techniques. The conductivity of the prepared membranes was measured. In this paper, effects of various factors including concentration of the solutions, oxidizing agents, time for leaving the support in the solutions, support type and temperature on membrane conductivity were investigated

  7. Revisiting the relaxation dynamics of isolated pyrrole

    Montero, Raúl; Ovejas, Virginia; Fernández-Fernández, Marta; Longarte, Asier, E-mail: asier.longarte@ehu.es [Departamento de Química Física, Universidad del País Vasco (UPV/EHU), Apart. 644, 48080 Bilbao (Spain); Peralta Conde, Álvaro [Centro de Láseres Pulsados (CLPU), Edificio M3, Parque Científico, 37185 Villamayor (Spain)

    2014-07-07

    Herein, the interpretation of the femtosecond-scale temporal evolution of the pyrrole ion signal, after excitation in the 267–217 nm interval, recently published by our group [R. Montero, A. Peralta Conde, V. Ovejas, M. Fernández-Fernández, F. Castaño, J. R. Vázquez de Aldana, and A. Longarte, J. Chem. Phys.137, 064317 (2012)] is re-visited. The observation of a shift in the pyrrole{sup +} transient respect to zero delay reference, initially attributed to ultrafast dynamics on the πσ{sup *} type state (3s a{sub 1} ← π 1a{sub 2}), is demonstrated to be caused by the existence of pump + probe populated states, along the ionization process. The influence of these resonances in pump-prone ionization experiments, when multi-photon probes are used, and the significance of a proper zero-time reference, is discussed. The possibility of preparing the πσ{sup *} state by direct excitation is investigated by collecting 1 + 1 photoelectron spectra, at excitation wavelengths ranging from 255 to 219 nm. No conclusive evidences of ionization through this state are found.

  8. Living on pyrrolic foundations - Advances in natural and artificial bioactive pyrrole derivatives.

    Domagala, Anna; Jarosz, Tomasz; Lapkowski, Mieczyslaw

    2015-07-15

    Pyrrole, a simple heterocyclic system, is an important building block for numerous biologically active compounds both natural and synthetic in origin, which boast an immense array of qualities, baleful and beneficial alike. The latter have given rise to a bountiful variety of pyrrole-based drugs, with many more being designed, developed and applied each year, as evidenced by the amount of entries in the Cambridge Structural Database skyrocketing from about six hundred in 2004 to more than a thousand over the course of the last decade. Particularly important in light of the ever-encroaching menace of drug-resistant bacteria, the vast progress in the field necessitates a sound organisational framework and summary - a task, to which we contribute this summary and checklist of the most recent developments, indicating the classes of compounds, which have attracted the most significant research attention. PMID:26087028

  9. Hydrolytic study of the copolymer Poly pyrrole/ Polyethyleneglycol and Poly pyrrole synthesized by plasma

    In this work the study about the hydrolytic compatibility of semiconductor polymers, copolymer Poly pyrrole/ Polyethyleneglycol (PPy/PEG) and Poly pyrrole (PPy) for their possible use as biomaterials. The polymers were synthesized by plasma between 10 and 100 W, with discharges of splendor RF to 13.5 MHz with resistive coupling. The hydrolytic affinity was evaluated calculating the contact angle with solutions of NaCl, NaCl-MgSO4 and Krebs-Ringer. The results show a hydrophilicity increment due to the increase of the surface ruggedness with the synthesis energy. On the contrary, the crystallinity diminishes when increasing the power in PPy and it stays approximately constant in PPy/PEG. The electric conductivity presents a growth from 2 to 4 magnitude orders in function of the water content in the polymers. (Author)

  10. Hydroquinone-pyrrole dyads with varied linkers.

    Huang, Hao; Karlsson, Christoffer; Strømme, Maria; Sjödin, Martin; Gogoll, Adolf

    2016-01-01

    A series of pyrroles functionalized in the 3-position with p-dimethoxybenzene via various linkers (CH2, CH2CH2, CH=CH, C≡C) has been synthesized. Their electronic properties have been deduced from (1)H NMR, (13)C NMR, and UV-vis spectra to detect possible interactions between the two aromatic subunits. The extent of conjugation between the subunits is largely controlled by the nature of the linker, with the largest conjugation found with the trans-ethene linker and the weakest with the aliphatic linkers. DFT calculations revealed substantial changes in the HOMO-LUMO gap that correlated with the extent of conjugation found experimentally. The results of this work are expected to open up for use of the investigated compounds as components of redox-active materials in sustainable, organic electrical energy storage devices. PMID:26877811

  11. Hydroquinone–pyrrole dyads with varied linkers

    Huang, Hao; Karlsson, Christoffer; Strømme, Maria; Sjödin, Martin

    2016-01-01

    Summary A series of pyrroles functionalized in the 3-position with p-dimethoxybenzene via various linkers (CH2, CH2CH2, CH=CH, C≡C) has been synthesized. Their electronic properties have been deduced from 1H NMR, 13C NMR, and UV–vis spectra to detect possible interactions between the two aromatic subunits. The extent of conjugation between the subunits is largely controlled by the nature of the linker, with the largest conjugation found with the trans-ethene linker and the weakest with the aliphatic linkers. DFT calculations revealed substantial changes in the HOMO–LUMO gap that correlated with the extent of conjugation found experimentally. The results of this work are expected to open up for use of the investigated compounds as components of redox-active materials in sustainable, organic electrical energy storage devices. PMID:26877811

  12. Electrochemical impedance of poly(9-tosyl-9H-carbazole-co-pyrrole) electrocoated carbon fiber

    Research highlights: → Impedance study of poly(9-tosyl-9H-carbazole-co-pyrrole) electrocoated carbon fiber. → Copolymer of 9-tosyl-9H-carbazole and pyrrole were electrocoated on carbon fiber. → Impedance spectroscopy and circuit models of poly(9-tosyl-9H-carbazole-co-pyrrole). - Abstract: In this paper, copolymer of 9-tosyl-9H-carbazole (TCz) and pyrrole (Py) comonomers were electrochemically deposited onto carbon fiber micro electrode (CFME) as an active electrode material. An electrochemical impedance study on the prepared electrodes is reported. Poly(TCz-co-Py)/CFME is characterized by cyclic voltammetry (CV), Fourier transform infrared reflectance-attenuated total reflection spectroscopy (FTIR-ATR), scanning electron microscopy-energy dispersive X-ray analysis (SEM-EDX), and electrochemical impedance spectroscopy (EIS). Capacitive behaviors of modified CFMEs were defined via Nyquist, Bode-magnitude and Bode-phase plots. An examination is made of which equivalent circuits of R(C(R(Q(RW)))) and R(C(R(Q(RW))))(CR) used for modeling the system. The effect of monomer ratio (mole fraction, XTCz = nTCz/nTCz + nPy) on the formation of copolymer is reported in 0.1 M sodium perchlorate (NaClO4)/acetonitrile (ACN) solution. The inclusion of TCz in the copolymer structure was also confirmed by FTIR-ATR, SEM, and CV measurements. The highest low frequency capacitance (CLF = 22.7 for R(C(R(Q(RW)))) and CLF = 22.6 mF cm-2 for R(C(R(Q(RW))))(CR)) were obtained for XTCz = 0.91.

  13. Polymerization of Pyrrole and Thiophene on Polyethylene Adipate Electrodes

    ERTURAN, Seyfettin; TORAMAN, Burcu YALVAÇ and Sena

    1998-01-01

    Polymerizations of pyrrole and thiophene on a platinum foil coated by polyethylene adipate (PEA) were carried out in acetonitrile by electrochemical methods. Different compositions of semi-conducting composite films of PEA/Polypyrrole(PPy), PEA/Polythiophene(PT) were prepared by the electrochemical polymerization of pyrrole and thiophene on PEA electrode. The polymerization was possible only for a certain thickness of the polyethylene adipate(PEA) on the platinum. Conductivities of PEA/PPy, P...

  14. Simple two-step synthesis of 2,4-disubstituted pyrroles and 3,5-disubstituted pyrrole-2-carbonitriles from enones

    Murat Kucukdisli

    2014-02-01

    Full Text Available The cyclocondensation of enones with aminoacetonitrile furnishes 3,4-dihydro-2H-pyrrole-2-carbonitriles which can be readily converted to 2,4-disubstituted pyrroles by microwave-induced dehydrocyanation. Alternatively, oxidation of the intermediates produces 3,5-disubstituted pyrrole-2-carbonitriles.

  15. Interaction of derived polymers from pyrrole with biocompatible solutions

    This work presents a study about the synthesis by plasma, the electric properties and superficial interaction of polymers derived from pyrrole doped with Iodine with potential use as bio material. Poly-pyrrole is a semiconductor and biocompatible polymer with potential application in the development of artificial muscles and implants where the electric interaction between cells and material is an important variable. The syntheses were made at 13.5 MHz in a glass tubular reactor of 1500 cm3 with electrodes of 6.5 cm diameter and stainless steel flanges. An electrode was connected to the RF terminal of the power supply that is combined with a matching coupling resistance. The monomer and dopant used in this work were pyrrole and Iodine respectively, in closed containers. They were vaporized and injected separately into the reactor at room temperature and 0.1 mbar. The vapors of the reagents mixed freely in the reactor. The synthesis time was 240 min at 40, 60, 80 and 100 W. The polymers were obtained as thin films adhered to the reactor walls. The films were washed and swollen with distilled water and removed from the reactor walls with a small spatula. The polymers were irradiated with gamma rays at 18 and 22 KGy. Due to the fact that the doses are cumulative, the final dose applied was 40 KGy. The polymers characterization was carried out by Fourier Transform Infrared Spectroscopy, thermogravimetric analysis (TGA), scanning electron microscopy, contact angle, electrical conductivity and X-ray diffraction. The analyses indicates that the polymers have very similar structure in almost the entire power range, showing C-O, C=C, C-H, O-H, N-H bonds with a predominantly amorphous structure. The TGA analyses showed that the material has 4 or 5 loses of material. The first one starts after that 115 C except for the material irradiated at 40 KGy, this one begins in 87 C, the second one is in the interval of 196 and 295 C, the third one between 311 and 500 C, and the last

  16. Reactions of a Ruthenium Complex with Substituted N-Propargyl Pyrroles.

    Chia, Pi-Yeh; Huang, Shou-Ling; Liu, Yi-Hong; Lin, Ying-Chih

    2016-04-01

    In an investigation into the chemical reactions of N-propargyl pyrroles 1 a-c, containing aldehyde, keto, and ester groups on the pyrrole ring, with [Ru]-Cl ([Ru]=Cp(PPh3 )2 Ru; Cp=C5 H5 ), an aldehyde group in the pyrrole ring is found to play a crucial role in stimulating the cyclization reaction. The reaction of 1 a, containing an aldehyde group, with [Ru]-Cl in the presence of NH4 PF6 yields the vinylidene complex 2 a, which further reacts with allyl amine to give the carbene complex 6 a with a pyrrolizine group. However, if 1 a is first reacted with allyl amine to yield the iminenyne 8 a, then the reaction of 8 a with [Ru]-Cl in the presence of NH4 PF6 yields the ruthenium complex 9 a, containing a cationic pyrrolopyrazinium group, which has been fully characterized by XRD analysis. These results can be adequately explained by coordination of the triple bond of the propargyl group to the ruthenium metal center first, followed by two processes, that is, formation of a vinylidene intermediate or direct nucleophilic attack. Additionally, the deprotonation of 2 a by R4 NOH yields the neutral acetylide complex 3 a. In the presence of NH4 PF6 , the attempted alkylation of 3 a resulted in the formation the Fischer-type amino-carbene complex 5 a as a result of the presence of NH3 , which served as a nucleophile. With KPF6 , the alkylation of 3 a with ethyl and benzyl bromoacetates afforded the disubstituted vinylidene complexes 10 a and 11 a, containing ester groups, which underwent deprotonation reactions to give the furyl complexes 12 a and 13 a, respectively. For 13 a, containing an O-benzyl group, subsequent 1,3-migration of the benzyl group was observed to yield product 14 a with a lactone unit. Similar reactivity was not observed for the corresponding N-propargyl pyrroles 1 b and 1 c, which contained keto and ester groups, respectively, on the pyrrole ring. PMID:26865008

  17. Electrogenerated poly(pyrrole-lactosyl) and poly(pyrrole-3'-sialyllactosyl) interfaces: towards the impedimetric detection of lectins

    Gondran, Chantal; Dubois, Marie-Pierre; Fort, Sebastien; Cosnier, Serge

    2013-07-01

    This paper reports on the impedimetric transduction of binding reaction between polymerized saccharides and target lectins. The controlled potential electro-oxidation of pyrrole-lactosyl and pyrrole-3’-sialyllactosyl at 0.95 V vs Ag/AgCl, provides thin and reproducible poly(pyrrole-saccharide) films. The affinity binding of two lectins: Arachis hypogaea, (PNA) and Maackia amurensis (MAA) onto poly(pyrrole-lactosyl) and poly(pyrrole-3’-sialyllactosyl) electrodes, was demonstrated by cyclic voltammetry in presence of ruthenium hexamine and hydroquinone. In addition, rotating disk experiments were carried out to determine the permeability of both polypyrrole films and its evolution after incubating with lectin target. Finally, the possibility of using the poly(pyrrole-lactosyl) or poly(pyrrole-3’-siallyllactosyl) films for the impedimetric transduction of the lectin binding reaction, was investigated with hydroquinone (2×10-3 mol L-1) as a redox probe in phosphate buffer. The resuting impedance spectra were interpreted and modeled as an equivalent circuit indicating that charge transfer resistance (Rct) and relaxation frequency (f°) parameters are sensitive to the lectin binding. Rct increases from 77 to 97 Ω cm2 for PNA binding and from 93 to 131 Ω cm2 for MAA binding. In parallel, f° decreases from 276 to 222 Hz for PNA binding and from 223 to 131 Hz for MAA binding. This evolution of both parameters reflects the steric hindrances generated by the immobilised lectins towards the permeation of the redox probe.

  18. Electrogenerated poly(pyrrole-lactosyl and poly(pyrrole-3’-sialyllactosyl interfaces: towards the impedimetric detection of lectins

    Chantal eGondran

    2013-07-01

    Full Text Available This paper reports on the impedimetric transduction of binding reaction between polymerized saccharides and target lectins. The controlled potential electro-oxidation of pyrrole-lactosyl and pyrrole-3’-sialyllactosyl at 0.95 V vs Ag/AgCl, provides thin and reproducible poly(pyrrole-saccharide films. The affinity binding of two lectins: Arachis hypogaea, (PNA and Maackia amurensis (MAA onto poly(pyrrole-lactosyl and poly(pyrrole-3’-sialyllactosyl electrodes, was demonstrated by cyclic voltammetry in presence of ruthenium hexamine and hydroquinone. In addition, rotating disk experiments were carried out to determine the permeability of both polypyrrole films and its evolution after incubating with lectin target. Finally, the possibility of using the poly(pyrrole-lactosyl or poly(pyrrole-3’-siallyllactosyl films for the impedimetric transduction of the lectin binding reaction, was investigated with hydroquinone (2×10-3 mol L-1 as a redox probe in phosphate buffer. The resuting impedance spectra were interpreted and modeled as an equivalent circuit indicating that charge transfer resistance (Rct and relaxation frequency (f° parameters are sensitive to the lectin binding. Rct increases from 77 to 97 Ω cm2 for PNA binding and from 93 to 131 Ω cm2 for MAA binding. In parallel, f° decreases from 276 to 222 Hz for PNA binding and from 223 to 131 Hz for MAA binding. This evolution of both parameters reflects the steric hindrances generated by the immobilised lectins towards the permeation of the redox probe.

  19. Synthesis and recognition properties of higher order tetrathiafulvalene (TTF) calix n pyrroles (n=4-6)

    Park, J. S.; Bejger, C.; Larsen, K. R.; Nielsen, K. A.; Jana, A.; Lynch, V. M.; Jeppesen, J. O.; Kim, D.; Sessler, J. L.

    2012-01-01

    proves most effective for the recognition of TNB and TNT. These findings are rationalized in terms of the number of electron rich TTF subunits and NH hydrogen bond donor groups within the series, as well as an ability to adopt conformations suitable for substrate recognition, and are supported by solid...... the condensation reaction, the expanded calix[n]pyrroles (n = 5 and 6) are characterized by a larger cavity size and a higher number of TTF units (albeit the same empirical formula). Analysis of the binding isotherms obtained from UV-Vis spectroscopic titrations carried out in CHCl3 in the presence of...

  20. Zinc hexacyanoferrate film as an effective protecting layer in two-step and one-step electropolymerization of pyrrole on zinc substrate

    The two-step and one-step electrosynthesis processes of polypyrrole (PPy) films on the zinc substrate are described. The two-step process includes (i) the zinc surface pretreatment with hexacyanoferrate ion in the aqueous medium in order to form a zinc hexacyanoferrate (ZnHCF) film non-blocking passive layer on the surface and with the view to prevent its reactivity and (ii) electropolymerization of pyrrole on the ZnHCF vertical bar Zn-modified electrode in aqueous pyrrole solution. In this context, both the non-electrolytic and electrolytic procedures were adapted, and the effect of some experimental conditions such as supporting electrolyte, pH and temperature of the solution at the zinc surface pretreatment step as well as pyrrole concentration and electrochemical techniques at the polymerization step was investigated. By optimizing the experimental conditions in both steps, we have obtained a homogeneous and strongly adherent PPy films on the zinc substrate. The one-step process is based on the use of an aqueous medium containing Fe(CN)64- and pyrrole. The ferrocyanide ion passivates the substrate by formation of ZnHCF film during the electropolymerization process of pyrrole and therefore makes it possible to obtain strongly adherent PPy films, with controlled thickness, either by cyclic voltammetry or by electrolysis at constant current or constant potential without any previously treatment of the zinc electrode surface. The polypyrrole films deposited on the zinc electrode were characterized by cyclic voltammetry and scanning electron microscopic (SEM) measurement

  1. Hydrazonoyl Chlorides as Precursors for Synthesis of Novel Bis-Pyrrole Derivatives

    Nabila Abdelshafy Kheder

    2016-01-01

    A convenient synthesis of some novel bis-pyrrole derivatives via hydrazonoyl halides is described. Antimicrobial evaluation of some selected examples of the synthesized products was carried out. The bis-pyrrole derivative having chloro substituents showed good activity against all of the used microbes. The molecular docking of the bis-pyrrole derivatives was performed by the Molecular Operating Environment (MOE) program.

  2. The first direct synthesis of β-unsubstituted meso-decamethylcalix[5]pyrrole

    Chacón-García, Luis; Chávez, Lizbeth; Cacho, Denisse R; Altamirano-Hernández, Josue

    2009-01-01

    The first direct synthesis of β-unsubstituted meso-decamethylcalix[5]pyrrole from pyrrole and acetone, with moderate yield, is described. The results showed that a bismuth salt was necessary to obtain calix[5]pyrrole, with the best results obtained using Bi(NO3)3.

  3. The first direct synthesis of β-unsubstituted meso-decamethylcalix[5]pyrrole

    Luis Chacón-García; Lizbeth Chávez; Cacho, Denisse R; Josue Altamirano-Hernández

    2009-01-01

    The first direct synthesis of β-unsubstituted meso-decamethylcalix[5]pyrrole from pyrrole and acetone, with moderate yield, is described. The results showed that a bismuth salt was necessary to obtain calix[5]pyrrole, with the best results obtained using Bi(NO3)3.

  4. Biofabrication Using Pyrrole Electropolymerization for the Immobilization of Glucose Oxidase and Lactate Oxidase on Implanted Microfabricated Biotransducers

    Christian N. Kotanen; Olukayode Karunwi; Anthony Guiseppi-Elie

    2014-01-01

    The dual responsive Electrochemical Cell-on-a-Chip Microdisc Electrode Array (ECC MDEA 5037) is a recently developed electrochemical transducer for use in a wireless, implantable biosensor system for the continuous measurement of interstitial glucose and lactate. Fabrication of the biorecognition membrane via pyrrole electropolymerization and both in vitro and in vivo characterization of the resulting biotransducer is described. The influence of EDC-NHS covalent conjugation of glucose oxidas...

  5. Versatile functionalization of nanoelectrodes by oligonucleotides via pyrrole electrochemistry.

    Descamps, Emeline; Nguyen, Khoa; Bouchain-Gautier, Christelle; Filoramo, Arianna; Goux-Capes, Laurence; Goffman, Marcello; Bourgoin, Jean-Philippe; Mailley, Pascal; Livache, Thierry

    2010-11-15

    Surface modification at the nanometer scale is a challenge for the future of molecular electronics. In particular, the precise anchoring and electrical addressing of biological scaffolds such as complex DNA nanonetworks is of importance for generating bio-directed assemblies of nano-objects for nanocircuit purposes. Herein, we consider the individual modification of nanoelectrodes with different oligonucleotide sequences by an electrochemically driven co-polymerization process of pyrrole and modified oligonucleotide sequences bearing pyrrole monomers. We demonstrate that this one-step technique presents the advantages of simplicity, localization of surface modification, mechanical, biological and chemical stability of the coatings, and high lateral resolution. PMID:20973021

  6. A colorimetric tetrathiafulvalene-calix 4 pyrrole anion sensor

    Nielsen, K. A.

    2012-01-01

    The interaction and colorimetric sensing properties of a tetrathiafulvalene substituted calix[4]pyrrole sensor with anions were investigated using H-1 NMR and absorption spectroscopic techniques. Visual color changes were observed upon addition of different anions (Cl-, Br-, CN-, and AcO-) to a s...

  7. Both visual and fluorescent sensors for Zn(2+) based on bis(pyrrol-2-yl-methyleneamine) platform.

    Wu, Wei-Na; Mao, Pan-Dong; Jia, Lei; Wang, Yuan; Xu, Zhou-Qing

    2016-09-01

    Two bis(pyrrol-2-yl-methyleneamine) chemo-sensors, 1, 3- and 1, 4-bis[3,4-dimethyl-5-ethyloxy -carbonyl-pyrrol-2-yl-methyleneamine]benzene (H2L(1) and H2L(2), respectively) have been synthesized and characterized, which exhibit high selectivity as off-on fluorescence sensors toward Zn(2+) in CH3CN/H2O (9:1, v/v) solution. The detection limits of both sensors are at the parts per million level. Moreover, the probes H2L(1) and H2L(2) could sense Zn(2+) by "naked eye" with a color change from colorless to yellow, and from yellow to dark yellow, respectively. To test the practical use of the probes, the determination of Zn(2+) in real water samples was also evaluated. PMID:27208758

  8. Both visual and fluorescent sensors for Zn2 + based on bis(pyrrol-2-yl-methyleneamine) platform

    Wu, Wei-Na; Mao, Pan-Dong; Jia, Lei; Wang, Yuan; Xu, Zhou-Qing

    2016-09-01

    Two bis(pyrrol-2-yl-methyleneamine) chemo-sensors, 1, 3- and 1, 4-bis[3,4-dimethyl-5-ethyloxy -carbonyl-pyrrol-2-yl-methyleneamine]benzene (H2L1 and H2L2, respectively) have been synthesized and characterized, which exhibit high selectivity as off-on fluorescence sensors toward Zn2 + in CH3CN/H2O (9:1, v/v) solution. The detection limits of both sensors are at the parts per million level. Moreover, the probes H2L1 and H2L2 could sense Zn2 + by "naked eye" with a color change from colorless to yellow, and from yellow to dark yellow, respectively. To test the practical use of the probes, the determination of Zn2 + in real water samples was also evaluated.

  9. Poly(1-(2-carboxyethyl)pyrrole)/polypyrrole composite nanowires for glucose biosensor

    A novel glucose biosensor based on poly(1-(2-carboxyethyl)pyrrole) (PPyCOOH)/polypyrrole (PPy) composite nanowires was developed by immobilizing glucose oxidase (GOD) on the nanowires via covalent linkages. The PPyCOOH/PPy composite nanowires were fabricated by a facile two-step electrochemical synthesis route. First, PPy nanowires were synthesized in phosphate buffer solution using organic sulfonic acid, p-toluenesulfonate acid, as soft-template. Then, PPyCOOH/PPy composite nanowires were obtained by polymerizing 1-(2-carboxyethyl)pyrrole onto PPy nanowires via electrochemical method. Scanning electron microscopic, FT-IR spectra, X-ray photoelectron spectroscopy and cyclic voltammograms were used to characterize the structural and electrical behaviors of the composite nanowires. The PPyCOOH/PPy composite nanowires exhibited uniform diameter, high reactive site (-COOH), large specific surface, excellent electroactivity and good adhesion to electrode. The glucose biosensor was constructed by covalently coupling GOD to the composite nanowires. The biosensor response was rapid (5 s), highly sensitive (33.6 μA mM−1 cm−2) with a wide linear range (up to 10.0 mM) and low detection limit (0.63 μM); it also exhibited high stability and specificity to glucose. The attractive electrochemical and structural properties of PPyCOOH/PPy composite nanowires suggested potential application for electrocatalysis and biosensor.

  10. Calix[4]pyrrole-based ion pair receptors.

    Kim, Sung Kuk; Sessler, Jonathan L

    2014-08-19

    Ion pair receptors, which are able to bind concurrently both a cation and an anion, often display higher selectivity and affinity for specific ion pairs than simple ion receptors capable of recognizing primarily either a cation or an anion. This enhancement in recognition function is attributable to direct or indirect cooperative interactions between cobound ions via electrostatic attractions between oppositely charged ions, as well as to positive allosteric effects. In addition, by virtue of binding the counterions of the targeted ion, ion pair receptors can minimize the solvation of the counterions, which can otherwise have a negative effect on the interactions between the receptors and the targeted ions. As a result of their more favorable interactions, ion pair receptors are attractive for use in applications, such as extraction and sensing, where control of the binding interactions is advantageous. In this Account, we illustrate this potential in the context of ion pair receptors based on the calix[4]pyrrole scaffold. Both simple ditopic ion pair receptors, containing sites for the recognition of a single anion and single cation, and so-called multitopic ion pair receptors will be discussed. The latter systems differ from conventional, so-called ditopic ion pair receptors in that they contain more than one binding site for a given targeted ion (e.g., a cation). This permits a level of selectivity and control over binding function not normally seen for simple ion or ion pair receptors containing one or two binding sites, respectively. Calix[4]pyrroles are macrocyclic compounds consisting of four pyrrole units linked via fully substituted sp(3) hybridized meso carbon atoms. They are effective receptors for Lewis basic anions (e.g., halides) in typical organic media and under certain conditions will recognize ion pairs containing charge diffuse cations, such as a small alkylammonium, imidazolium, or cesium cations. The calix[4]pyrrole framework is further

  11. Calix[4]pyrrole derivative: recognition of fluoride and mercury ions and extracting properties of the receptor-based new material.

    de Namor, Angela F Danil; Khalife, Rasha

    2008-12-11

    A calix[4]pyrrole derivative, namely, meso-tetramethyl tetrakis (4-phenoxy methyl ketone) calix[4]pyrrole, 1, was synthesized and structurally (1H NMR) and thermodynamically characterized. The complexing properties of this receptor with a wide variety of anions and cations in dipolar aprotic media (acetonitrile, propylene carbonate, and dimethyl sulfoxide) were investigated through 1H NMR and conductance studies. The former technique was used to assess whether or not complexation occurs and if so to identify the active sites of interaction of 1 with ions. The composition of the complexes was established by conductance measurements. It was found that in dipolar aprotic solvents, 1 interacts only with two polluting ions (fluoride and mercury). The complexation thermodynamics of 1 and these ions in these solvents is reported. The medium effect on the binding process involving the fluoride ion is discussed taking into account the solvation properties of reactants and the product. Complexes of moderate stability are found. Given that this is an important factor to consider for the recycling of the loaded material in extraction processes, 1 was treated with formaldehyde in basic medium leading to the production of a calix[4]pyrrole based material able to extract fluoride and mercury (II) ions from water. Thus the optimum conditions for the extraction of these ions from aqueous solutions were established. The material is easily recyclable using an organic acid. Final conclusions are given. PMID:19053691

  12. Synthetic, structural and biological studies of organosilicon(IV complexes of Schiff bases derived from pyrrole-2-carboxaldehyde

    KIRAN SING

    2010-07-01

    Full Text Available Selected new organosilicon(IV complexes having the general formula R2SiCl[L] and R2Si[L] 2 were synthesized by the reactions of Me2SiCl2 with Schiff bases (5-mercapto-4-[(1H-pyrrol-2ylmethyleneamino]-s-triazole, 5-mercapto-3-methyl-4-[(1H-pyrrol-2ylmethyleneamino]-s-triazole and 3-ethyl-5-mercapto-4-[(1H-pyrrol-2ylmethyleneamino]-s-triazole in 1:1 and 1:2 molar ratios. All of the compounds were characterized by elemental analysis, molar conductance, and IR, UV, 1H-, 13C- and 29Si-NMR spectral studies. All the spectral data suggest an involvement with an azomethine nitrogen in coordination to the central silicon atom. With the help of above-mentioned spectral studies, penta and hexacoordinated environments around the central silicon atoms in the 1:1 and 1:2 complexes, respectively, are proposed. Finally, the free ligands and their metal complexes were tested in vitro against some pathogenic bacteria and fungi to assess their antimicrobial properties.

  13. Sensing of antipyretic carboxylates by simple chromogenic calix[4]pyrroles.

    Nishiyabu, Ryuhei; Anzenbacher, Pavel

    2005-06-15

    We present a simple, two- or three-step method for the synthesis of chromogenic octamethylcalix[4]pyrrole-based (OMCP) sensors for anions. Electrophilic aromatic substitution allows for converting the pyrrole moieties of OMCP into a dye. The formation of a sensor-anion complex results in partial charge transfer and a dramatic change in color. The absorption (UV-vis) and NMR titration experiments show that the chromogenic OMCPs sense anions administered as aqueous solutions, even at high ionic strength ( approximately 0.1 M NaCl), while displaying selectivity for pyrophosphate and carboxylate anions. The experiments with polyurethane sensor films show a strong response for aqueous carboxylates, such as antipyretics naproxen approximately ibuprofen > salicylate, without being biased by bicarbonate or carboxy termini of blood plasma proteins. PMID:15941245

  14. Temperature dependence of dielectric properties of poly pyrrole composite films

    The composite polymer films of poly pyrrole-poly(vinyl alcohol)-iron chloride were prepared in the form of as-cast films. The dielectric properties of the samples were measured at the frequency range of 20 Hz to 1 MHz at different temperatures (300 K up to 353 K) by Inductance Capacitance Resistance (LCR) meter. The results show that the dielectric properties were strongly dependent on the variation of temperature applied. The composite polymer films exhibit the combination of intrinsic dielectric anisotropy, as a result of the competition of free charges, mainly between the polaron in poly pyrrole and the electronic polarisation that corresponded to PVA matrix. The main mechanism behind this finding can be explained by the dipole movement which highly activate at higher temperatures. In addition, high mobility of dipoles movement induced by thermal energy enables them to easily orient towards applied electric field. (author)

  15. Asymmetrically substituted calix[4]pyrrole with chiral substituents

    Štěpánek, P.; Šimák, Ondřej; Nováková, Z.; Wimmer, Zdeněk; Drašar, P.

    2011-01-01

    Roč. 9, č. 3 (2011), s. 682-683. ISSN 1477-0520 R&D Projects: GA MŠk 2B06024 Grant ostatní: NATO(XE) CBP.EAP.CLG.982972 Institutional research plan: CEZ:AV0Z40550506; CEZ:AV0Z50380511 Keywords : porphyrin derivatives * anion-binding * aggregation * pyrrole * ketones Subject RIV: CC - Organic Chemistry Impact factor: 3.696, year: 2011

  16. Numerical Analysis Of Hooke Jeeves-Runge Kutta To Determine Reaction Rate Equation In Pyrrole Polymerization

    The numerical analysis of Hooke Jeeves Methods combined with Runge Kutta Methods is used to determine the exact model of reaction rate equation of pyrrole polymerization. Chemical polymerization of pyrrole was conducted with FeCI3 / pyrrole solution at concentration ratio of 1.62 mole / mole and 2.18 mole / mole with varrying temperature of 28, 40, 50, and 60 oC. FeCl3 acts as an oxidation agent to form pyrrole cation that will polymerize. The numerical analysis was done to examine the exact model of reaction rate equation which is derived from reaction equation of initiation, propagation, and termination. From its numerical analysis, it is found that the pyrrole polymerization follows third order of pyrrole cation concentration

  17. Multiphoton ionization of pyrrole-water mixed clusters

    2001-01-01

    Multiphoton ionization of the hydrogen-bonded pyrrole-water clusters ( C4H5 N)n H2O)m is studied with a reflectron—time of flight mass spectrometer at 355 nm. With increasing partial concentration of pyrrole in a gas mixture source, a series of poly-pyrrole-water binary-mixed cluster ions can be observed, including unprotonated cluster ions [(C4H5N)x (H2O)y]* , protonated cluster ions [(C4H5N)x (H2O)yH]* and dehydrogenated cluster ions [ ( C4 H4 N) ( C4 H5 N) x ( H2O) y ] + . Ab initio calculations of their structures, bond strengths, charge distributions and re action energies are carried out. Stable structures of these clusters are obtained from the calculations. A probable forma tion mechanism of the cluster ions [(C4H5N)x(H2O)y] + , [(C4H5N)x (H2O)y]H+ and [(C4H4N) (C4H5N)x (H2O)y]-is supposed to be the ionization of clusters followed by dissociation.

  18. Hydrazonoyl Chlorides as Precursors for Synthesis of Novel Bis-Pyrrole Derivatives

    Nabila Abdelshafy Kheder

    2016-03-01

    Full Text Available A convenient synthesis of some novel bis-pyrrole derivatives via hydrazonoyl halides is described. Antimicrobial evaluation of some selected examples of the synthesized products was carried out. The bis-pyrrole derivative having chloro substituents showed good activity against all of the used microbes. The molecular docking of the bis-pyrrole derivatives was performed by the Molecular Operating Environment (MOE program.

  19. Poly(pyrrole-co-pyrrole propylic acid) film and its application in label-free surface plasmon resonance immunosensors.

    Hu, Weihua; Li, Chang Ming; Dong, Hua

    2008-12-01

    In this work, surface plasmon resonance (SPR) was used to study protein immobilization on poly(pyrrole-co-pyrrole propylic acid) (PPy/PPa) for immunosensing applications. SPR was employed to in situ monitor the electropolymerization process and to control thickness of the PPy/PPa copolymer film. Goat IgG as a model protein was covalently immobilized on the carboxyl-containing film through EDC/NHS as the coupling reagents. The effect of pyrrole propylic acid (Pa) proportion in the deposition solution on the protein immobilization capability was systemically investigated. The immobilization efficiency was demonstrated by a label-free SPR immunosensor. The heterogeneous kinetics of the immune reaction was discussed. This work could provide a facile method to immobilize proteins on an electrode surface by electropolymerized copolymer, and renders a universal approach to in situ study the protein immobilization process and sensing kinetics for scientific insights of the heteroimmunosensing scheme particularly in surface chemistry and molecular biology for further improvement of immunosensors. PMID:19068327

  20. A novel quinoxaline bearing electroactive monomer: Pyrrole as the donor moiety

    Taskin, Asli Tuba; Balan, Abidin; Epik, Bugra; Yildiz, Ersin [Middle East Technical University, Department of Chemistry, 06531, Ankara (Turkey); Udum, Yasemin Arslan [Gazi University, Institute of Science and Technology, Department of Advanced Technologies, 06570, Ankara (Turkey); Toppare, Levent [Middle East Technical University, Department of Chemistry, 06531, Ankara (Turkey)], E-mail: toppare@metu.edu.tr

    2009-09-30

    A novel electroactive monomer 5,8-di(1H-pyrrol-2-yl)-2,3-di(thiophen-2-yl)quinoxaline (PTQ) was successfully synthesized and its electrochromic properties were reported. Nuclear magnetic resonance ({sup 1}H NMR-{sup 13}C NMR) and mass spectroscopy were used to characterize the monomer. The monomer was electrochemically polymerized in the presence of tetrabutylammonium perchlorate (TBAP) as supporting electrolyte in dichloromethane. Monomer reveals relatively low oxidation potential at +0.70 V. Spectroelectrochemical behaviors and switching ability of homopolymer were investigated by UV-vis spectroscopy and cyclic voltammetry. Two {pi}-{pi}* transitions were observed at 400 and 815 nm with a low band gap, 1.0 eV. Polymer possesses 66% optical contrast in the Near IR region, which may be promising in NIR electrochromic device applications.

  1. A novel quinoxaline bearing electroactive monomer: Pyrrole as the donor moiety

    A novel electroactive monomer 5,8-di(1H-pyrrol-2-yl)-2,3-di(thiophen-2-yl)quinoxaline (PTQ) was successfully synthesized and its electrochromic properties were reported. Nuclear magnetic resonance (1H NMR-13C NMR) and mass spectroscopy were used to characterize the monomer. The monomer was electrochemically polymerized in the presence of tetrabutylammonium perchlorate (TBAP) as supporting electrolyte in dichloromethane. Monomer reveals relatively low oxidation potential at +0.70 V. Spectroelectrochemical behaviors and switching ability of homopolymer were investigated by UV-vis spectroscopy and cyclic voltammetry. Two π-π* transitions were observed at 400 and 815 nm with a low band gap, 1.0 eV. Polymer possesses 66% optical contrast in the Near IR region, which may be promising in NIR electrochromic device applications.

  2. One-pot Green Synthesis of Pyrrole Derivatives Catalyzed by Nano Sulfated Zirconia as a Solid Acid Catalyst%One-pot Green Synthesis of Pyrrole Derivatives Catalyzed by Nano Sulfated Zirconia as a Solid Acid Catalyst

    Teimouri, Abbas; Chermahini, Alireza Najafi

    2012-01-01

    A new and efficient method for the preparation of N-substituted pyrroles from one-pot Paal-Knorr condensation has been accomplished using nano-crystalline sulfated zirconia (SZ) as the catalyst in ethanol at moderate temperature. This new protocol has the advantages of easy availability, stability, reusability and eco-friendliness of the catalyst, high to excellent yields, simple experimental and work-up procedure. The synthesized compounds were confirmed through spectral characterization using IR, 1H NMR, 13C NMR and mass spectra.

  3. A Novel TetraTTF-calix[4]pyrrole Ouroborand for Explosive Detection

    Bähring, Steffen; Nielsen, Kent

    We have synthesized the first example of an asymmetric tetraTTF-calix[4]pyrrole. This system features Ouroborand qualities due to selfcomplexation with the pyridine substituent. This forces the usually highly flexible calix[4]pyrrole into a preorganized conformation with improved explosive...

  4. A Novel TetraTTF-calix[4]pyrrole Ouroborand for Explosive Detection

    Bähring, Steffen; Nielsen, Kent

    2010-01-01

    We have synthesized the first example of an asymmetric tetraTTF-calix[4]pyrrole. This system features Ouroborand qualities due to selfcomplexation with the pyridine substituent. This forces the usually highly flexible calix[4]pyrrole into a preorganized conformation with improved explosive...

  5. Novel and efficient supramolecular synthesis of pyrroles in the presence of β-cyclodextrin in water

    K. Ramesh; K. Karnakar; G. Satish; Y.V.D. Nageswar

    2012-01-01

    A simple and efficient synthesis of highly substituted pyrroles was achieved in water medium via multi-component strategy,using amine,DMAD/DEAD as well as phenacyl bromide catalyzed by β-CD.Utilizing this protocol various pyrrole derivatives were synthesized in good to excellent yields.

  6. Interesting reactivity of diketones with pyrrole under acidic condition

    Sanjeev Pran Mahanta; Pradeepta Kumar Panda

    2011-09-01

    The acid catalysed condensation of diketones with pyrrole did not result in the formation of expected divergent bisdipyrromethane always; instead the product depends on the chain length of the diketones, in particular the distance between the two carbonyl functional groups.When the two carbonyl groups are linked via one or two methylene groups, unusual ring annulation occurs resulting in the formation of various bridged bipyrroles. However, on further increase in the length of the spacer, between the two carbonyl groups, synthesis of the expected bisdipyrromethanes could be achieved.

  7. Pyrrolic Amide: A New Hydrogen Bond Building Block for Self-assembly

    YIN Zhen-Ming; LI Jian-Feng; HE Jia-Qi; ZHU Xiao-Qing; CHENG Jin-Pei

    2003-01-01

    @@ Molecular self-assembly has emerged as a powerful technology for the synthesis of nanostructured materials. In design of various molecular assemblies, hydrogen bonding is a preferably selected intra- or inter-molecular weak interaction in recent research by virtue of the directionality and specificity. The research for novel hydrogen bond building blocks that self-assembly into well defined structures is great important not only for gaining an understanding of the concepts of self-assembly but also for the design of new molecular materials. Pyrrolic amide moiety has one hydrogen bond acceptor (C =O) and two hydrogen bond donors (pyrrole NH and amide NH). By deliberately design, pyrrolic amide compounds would be new kinds hydrogen bond building blocks. So, pyrrolic amide compounds 1 ~ 6, which bear one, two or three pyrrolic amide moieties respectively, were designed and synthesized.

  8. Eco-friendly synthesis, spectral and computational study of pyrrole-2-carboxaldehyde salicylhydrazone (PCSH) for its application

    Rawat, Poonam; Singh, R. N.

    2015-11-01

    In this paper we present eco-friendly synthesis of Pyrrole-2-carboxaldehyde salicylhydrazone (PCSH) and its molecular structural elucidation, spectral analysis and reactivity evaluation. Pyrrole-2-carboxaldehyde and salicyl hydrazide in water undergo condensation reaction to produce PCSH in good yield (88%). All results of quantum chemical calculation corroborate well with the experimental findings. The PCSH has been characterized by elemental analysis, FT-IR, 1H NMR, UV-Visible, and ESI-Mass spectroscopy. Density functional theory (DFT) calculations have been carried out for PCSH by performing B3LYP functional using the standard basis set 6-31 + g (d, p), and additional basis sets 6D and 10F. Two most stable conformers for PCSH have been observed around the dihedral angle N1C5C6N7. The red shift observed in O-H stretching vibration in the FT-IR spectrum indicates the presence of intramolecular hydrogen bonding. The rotational barrier between syn-syn (closed) syn-syn (open) found to be 2966.9 kcal/mol. The presence of hydroxyl proton at 10.45 ppm downfield in experimental 1H NMR spectrum confirms the existence of intramolecular hydrogen bonding in PCSH. Further, topological parameters analysis at the bond critical points using 'Atoms in molecules' theory reveals intramolecular hydrogen bonding. The energy of homonuclear intramolecular hydrogen bond (O17-H28⋯O10) is calculated to be 14.03 kcal/mol. The ellipticity results confirm the resonance assisted nature of this intramolecular hydrogen bond. In addition to this work, the reactive sites in PCSH have been explored using DFT descriptors, predicting nucleophilic reactions at carbonyl carbon and electrophilic reactions are possible at pyrrolic NH, amidic NH and double bond Cdbnd N leading to several heterocyclic products and metal complexes.

  9. Transition metal doped poly(aniline-co-pyrrole)/multi-walled carbon nanotubes nanocomposite for high performance supercapacitor electrode materials

    Dhibar, Saptarshi; Bhattacharya, Pallab; Hatui, Goutam; Das, C.K., E-mail: chapal12@yahoo.co.in

    2015-03-15

    Highlights: • The CuCl{sub 2} doped copolymer (PANI and PPy)/MWCNTs nanocomposite was prepared. • The nanocomposite achieved highest specific capacitance of 383 F/g at a 0.5 A/g. • Nanocomposite exhibits better energy density as well as power density. • The nanocomposite also showed better electrical conductivity at room temperature. • The nanocomposite can be used as promising electrode materials for supercapacitor. - Abstract: In this present communication, copolymer of polyaniline (PANI) and polypyrrole (PPy) that is poly(aniline-co-pyrrole) [poly(An-co-Py)], copper chloride (CuCl{sub 2}) doped poly(aniline-co-pyrrole) [poly(An-co-Py) Cu], and CuCl{sub 2} doped poly(aniline-co-pyrrole)/multi walled carbon nanotubes (MWCNTs) [poly(An-co-Py) Cu CNT] nanocomposite have been prepared by a simple and inexpensive in-situ chemical oxidative polymerization method, using ammonium persulfate (APS) as oxidant and hydrochloric acid (HCl) as dopant and investigated as high performance supercapacitor electrode materials. The possible interaction between CuCl{sub 2} with copolymers and MWCNTs was investigated by Fourier transform infrared spectroscopy (FTIR) and UV–visible spectroscopy analysis. The morphological characteristic of all the electrode materials were analyzed by Field emission scanning electron microscopy (FESEM) and Transmission electron microscopy (TEM) study. The electrochemical characterizations of all the electrode materials were carried out by three electrode probe method where, standard calomel electrode and platinum were used as reference and counter electrodes, respectively. Among all the electrode materials, poly(An-co-Py) Cu CNT nanocomposite achieved highest specific capacitance value of 383 F/g at 0.5 A/g scan rate. The nanocomposite showed better electrical conductivity at room temperature and also attained nonlinear current–voltage characteristic. Based on the superior electrochemical as well as other properties the as prepared

  10. Ferrocene-Functionalized 4-(2,5-Di(thiophen-2-yl-1H-pyrrol-1-ylaniline: A Novel Design in Conducting Polymer-Based Electrochemical Biosensors

    Rukiye Ayranci

    2015-01-01

    Full Text Available Herein, we report a novel ferrocenyldithiophosphonate functional conducting polymer and its use as an immobilization matrix in amperometric biosensor applications. Initially, 4-(2,5-di(thiophen-2-yl-1H-pyrrol-1-ylamidoferrocenyldithiophosphonate was synthesized and copolymerized with 4-(2,5-di(thiophen-2-yl-1H-pyrrol-1-ylbenzenamine at graphite electrodes. The amino groups on the polymer were utilized for covalent attachment of the enzyme glucose oxidase. Besides, ferrocene on the backbone was used as a redox mediator during the electrochemical measurements. Prior to the analytical characterization, optimization studies were carried out. The changes in current signals at +0.45 V were proportional to glucose concentration from 0.5 to 5.0 mM. Finally, the resulting biosensor was applied for glucose analysis in real samples and the data were compared with the spectrophotometric Trinder method.

  11. Electrochromic properties of multicolored novel polymer synthesized via combination of benzotriazole and N-functionalized 2,5-di(2-thienyl)-1H-pyrrole units

    Synthesis of new conducting polymers is desired since their electrochemical and optical properties enable them to be used as active layers in many device applications. Benzotriazole and N-functionalized 2,5-di(2-thienyl)-1H-pyrrole (SNS Series) containing polymers showed very promising results as electrochromic materials. In order to observe the effect of the combination of these two units, three new monomers; 2-(6-(2,5-bis(5-methylthiophen-2-yl)-1H-pyrrol-1-yl)hexyl)-4,7-di (thiophen-2-yl)-2H benzo[d][1,2,3]triazole (M1), 2-(6-(2,5-di(thiophen-2-yl)-1H-pyrrol-1-yl)hexyl)-4,7-di(thiophen-2-yl) -2H-benzo[d][1,2,3]triazole (M2) and 2-(6-(2,5-di(thiophen-2-yl)-1H-pyrrol-1-yl)hexyl)-4,7-bis (5-methylthiophen-2-yl)-2H-benzo[d][1,2,3]triazole (M3) were synthesized. To better characterize the electronic and spectroscopic properties of the monomers, density functional theory (DFT) and its time-dependent generalization (TD-DFT) were used to calculate their vertical ionization potentials, vertical electron affinity and to simulate and interpret their infrared and UV-vis spectra. The monomers were electrochemically polymerized and the resultant polymers were characterized with cyclic voltammetry and UV-vis-NIR spectroscopy techniques. An electrochromic device was constructed with electrochemical polymer of M2. The device switched between red and blue colors and showed exceptional optical memory

  12. 2-Ethyl 4-methyl 5-ethyl-3-methyl-1H-pyrrole-2,4-dicarboxylate

    Gui-Fen Lu

    2012-02-01

    Full Text Available The title pyrrole derivative compound, C12H17NO4, was synthesized from methyl 3-oxopentanoate by a Knorr-type reaction and contains a pyrrole ring to which two diagonal alkoxycarbonyl groups and two diagonal alkyl substituents are attached. The methylcarbonyl and ethylcarbonyl substituents are approximately co-planar with the pyrrole ring, making dihedral angles of 5.64 (2 and 3.44 (1°, respectively. In the crystal, adjacent molecules are assembled by pairs of N—H...O hydrogen bonds into dimers in a head-to-head mode.

  13. Ru-catalyzed site-selective direct arylation polycondensation via ortho-metalation of pyrrole derivative

    A Ti-conjugated polymer consisting of pyrrole and fluorene units was synthesized via Ru-catalyzed direct arylation polycondensation. The introduction of a 2-pyrimidinyl substituent into the N -position of the pyrrole monomer as a directing group induced ortho-metalation, with effective site-selective polycondensation at the α-position of the pyrrole monomer, without the need for protection of the β-position. Subsequent removal of the 2-pyrimidinyl substituent led to the elongation of π-conjugation along the main chain of the polymer via elimination of the steric hindrance due to the bulky substituent

  14. (4-Butoxyphenyl(1H-pyrrol-2-ylmethanone

    Rajni Kant

    2012-05-01

    Full Text Available The asymmetric unit of the title compound, C15H17NO2, contains two independent molecules in which the dihedral angles between the pyrrole and benzene rings are 42.43 (9 and 45.70 (9°. In both molecules, the butoxy chains are disordered over two sets of sites, with occupancy ratios of 0.701 (7:0.299 (7 and 0.869 (4:0.131 (4. Each molecule forms a dimer with an inversion-related molecule, through a pair of N—H...O hydrogen bonds. Weak C—H...O interactions link these dimers in the crystal structure.

  15. Discovery of pyrrole-based hepatoselective ligands as potent inhibitors of HMG-CoA reductase.

    Bratton, Larry D; Auerbach, Bruce; Choi, Chulho; Dillon, Lisa; Hanselman, Jeffrey C; Larsen, Scott D; Lu, Gina; Olsen, Karl; Pfefferkorn, Jeffrey A; Robertson, Andrew; Sekerke, Catherine; Trivedi, Bharat K; Unangst, Paul C

    2007-08-15

    In an effort to identify hepatoselective inhibitors of HMG-CoA reductase, two series of pyrroles were synthesized and evaluated. Efforts were made to modify (3R,5R)-7-[3-(4-fluorophenyl)-1-isopropyl-4-phenyl-5-phenylcarbamoyl-1H-pyrrol-2-yl]-3,5-dihydroxy-heptanoic acid sodium salt 30 in order to reduce its lipophilicity and therefore increase hepatoselectivity. Two strategies that were explored were replacement of the lipophilic 3-phenyl substituent with either a polar function (pyridyl series) or with lower alkyl substituents (lower alkyl series) and attachment of additional polar moieties at the 2-position of the pyrrole ring. One compound was identified to be both highly hepatoselective and active in vivo. We report the discovery, synthesis, and optimization of substituted pyrrole-based hepatoselective ligands as potent inhibitors of HMG-CoA reductase for reducing low density lipoprotein cholesterol (LDL-c) in the treatment of hypercholesterolemia. PMID:17560788

  16. Five gene products are required for assembly of the central pyrrole moiety of coumermycin A1

    Novotná, J.; Gust, B.; Kulik, A.; Spížek, Jaroslav; Heide, L.

    2013-01-01

    Roč. 40, č. 8 (2013), s. 915-925. ISSN 1367-5435 Institutional support: RVO:61388971 Keywords : Streptomyces * Coumermycin * Pyrrole Subject RIV: EE - Microbiology, Virology Impact factor: 2.505, year: 2013

  17. Auto-oligomerization and hydration of pyrrole revealed by x-ray absorption spectroscopy

    Near edge x-ray absorption fine structure spectra have been measured at the carbon and nitrogen K-edges of the prototypical aromatic molecule, pyrrole, both in the gas phase and when solvated in water, and compared with spectra simulated using a combination of classical molecular dynamics and first principles density functional theory in the excited state core hole approximation. The excellent agreement enabled detailed assignments. Pyrrole is highly reactive, particularly in water, and reaction products formed by the auto-oligomerization of pyrrole are identified. The solvated spectra have been measured at two different temperatures, indicating that the final states remain largely unaffected by both hydration and temperature. This is somewhat unexpected, since the nitrogen in pyrrole can donate a hydrogen bond to water.

  18. Auto-oligomerization and hydration of pyrrole revealed by x-ray absorption spectroscopy

    Advanced Light Source; Schwartz, Craig P.; Uejio, Janel S.; Duffin, Andrew M.; England, Alice H.; Prendergast, David; Saykally, Richard J

    2009-05-29

    Near edge x-ray absorption fine structure (NEXAFS) spectra have been measured at the carbon and nitrogen K-edges of the prototypical aromatic molecule, pyrrole, both in the gas phase and when solvated in water, and compared with spectra simulated using a combination of classical molecular dynamics and first principles density functional theory in the excited state core hole approximation. The excellent agreement enabled detailed assignments. Pyrrole is highly reactive, particularly in water, and reaction products formed by the auto-oligomerization of pyrrole are identified. The solvated spectra have been measured at two different temperatures, indicating that the final states remain largely unaffected by both hydration and temperature. This is somewhat unexpected, since the nitrogen in pyrrole can donate a hydrogen bond to water.

  19. Synthesis of new 2,5-dimethyl pyrrole derivatives from acetonylacetone

    Xiao Ming Ji; Ye Lu; Ming Qin Zhao; Xiao Yun Zhang; Yun Liu; Le Liu

    2010-01-01

    Acetonylacetone 1 was treated with thiourea, aniline, glycine and glutamic acid to give pyrrole derivatives 2, 3, 5, and 9 by Paal-Knorr reaction, respectively. Then 3 was successfully transformed into the related pyrrole derivative 4 by Mannich reaction.Compounds 6, 7 and 8 were obtained by reacting 5 with phenethyl alcohol, phenylallylic alcohol and leaf alcohol by esterification reactions, respectively. The structures of all new products were elucidated by IR, NMR and HRMS spectra.

  20. Energetics of 1-(aminophenyl)pyrroles: A joint calorimetric and computational study

    Santos, Ana Filipa L.O.M. [Centro de Investigacao em Quimica, Department of Chemistry and Biochemistry, Faculty of Science, University of Porto, Rua do Campo Alegre, 687, P-4169-007 Porto (Portugal); Ribeiro da Silva, Manuel A.V., E-mail: risilva@fc.up.pt [Centro de Investigacao em Quimica, Department of Chemistry and Biochemistry, Faculty of Science, University of Porto, Rua do Campo Alegre, 687, P-4169-007 Porto (Portugal)

    2011-10-15

    Highlights: > Enthalpy of formation of crystalline 1-(2-aminophenyl)pyrrole was determined by combustion calorimetry. > Vapor pressures of 1-(aminophenyl)pyrrole were measured as function of temperature by the Knudsen effusion technique. > Enthalpies of formation of the three gaseous isomers of 1-(aminophenyl)pyrrole were obtained by G3(MP2)//B3LYP calculations. - Abstract: Static bomb calorimetry and the Knudsen effusion mass-loss technique were used to derive, respectively, the standard (p{sup o} = 0.1 MPa) molar enthalpy of formation, in the crystalline phase, {Delta}{sub f}H{sub m}{sup 0}(cr), and the standard molar enthalpy of sublimation, at T = 298.15 K, {Delta}{sub cr}{sup g}H{sub m}{sup 0}, of 1-(2-aminophenyl)pyrrole. These experiments allowed the determination of its standard (p{sup o} = 0.1 MPa) molar enthalpy of formation, in the gaseous phase, {Delta}{sub f}H{sub m}{sup 0}(g), at T = 298.15 K, as (224.1 {+-} 2.4) kJ . mol{sup -1}. The gas-phase enthalpy of formation of 1-(2-aminophenyl)pyrrole was also estimated by G3(MP2)//B3LYP calculations, which were further extended to the (aminophenyl)pyrroles that were not studied experimentally. Experimental and theoretical results are in very good agreement.

  1. Facile synthesis, structural elucidation and spectral analysis of pyrrole 4-imidazole derivatives

    Singh, R. N.; Rawat, Poonam; Baboo, Vikas

    2015-12-01

    In this work pyrrole 4-imidazole derivatives (3A-3D): benzimidazoles and pyrrole 4-imidazoline have been synthesized by condensation, cyclization and oxidation of ethyl 4-formyl-3,5-dimethyl-1H-pyrrole carboxylate and phenylene diamine derivatives/ethylene diamine. The structure of these biheterocyclic compounds have been derived by elemental and spectroscopic - IR, UV, MS, 1H and 13C NMR analysis as well as theoretical study. The static first hyperpolarizability, β0 values for pyrrole 4-imidazole derivatives, (3A-3D) have been calculated as 10.901 × 10-31, 19.607 × 10-31, 40.323 × 10-31, 5.686 × 10-31 esu, respectively. The gradual increase in β0 value of synthesized pyrrole-benzimidazole derivatives from 3A to 3C is due to addition of acceptors -Cl atom in 3B to -NO2 group in 3C on benzimidazole side. The experimental absorption spectra found to be in UV region and the high β0 values show that the synthesized pyrrole-imidazoles are suitable as non-linear optical (NLO) materials.

  2. Synthesis of π-conjugated systems bearing thiophene and pyrrole heterocycles through palladium-catalyzed decarboxylative cross-coupling reaction

    Castro, M. Cidália R.; Fonseca, A. Maurício C.; Raposo, M. Manuela M.

    2012-01-01

    Thiophene and pyrrole moieties play important roles in synthetic and medicinal chemistry, as they are present in a large number of natural products and biologically active compounds. For this reason, amongst all five-membered aromatic heterocycles, molecules containing the pyrrole nucleus have attracted the greatest attention of researchers and have been studied in most detail. Especially, 2-aryl- and 2-heteroaryl-substituted pyrroles are of great interest to the pharmaceutical industry, for ...

  3. Hydrogen transfer in excited pyrrole-ammonia clusters

    David, O.; Dedonder-Lardeux, C.; Jouvet, C.; Kang, H.; Martrenchard, S.; Ebata, T.; Sobolewski, A. L.

    2004-06-01

    The excited state hydrogen atom transfer reaction (ESHT) has been studied in pyrrole-ammonia clusters [PyH-(NH3)n+hν→Py•+•NH4(NH3)n-1]. The reaction is clearly evidenced through two-color R2P1 experiments using delayed ionization and presents a threshold around 235 nm (5.3 eV). The cluster dynamics has also been explored by picosecond time scale experiments. The clusters decay in the 10-30 ps range with lifetimes increasing with the cluster size. The appearance times for the reaction products are similar to the decay times of the parent clusters. Evaporation processes are also observed in competition with the reaction, and the cluster lifetime after evaporation is estimated to be around 10 ns. The kinetic energy of the reaction products is fairly large and the energy distribution seems quasi mono kinetic. These experimental results rule out the hypothesis that the reaction proceeds through a direct N-H bond rupture but rather imply the existence of a fairly long-lived intermediate state. Calculations performed at the CASSCF/CASMP2 level confirm the experimental observations, and provide some hints regarding the reaction mechanism.

  4. 2-(4-Chloro-N-{2-[(1H-pyrrol-2-ylcarbonyloxy]ethyl}anilinoethyl 1H-pyrrole-2-carboxylate

    Ying Yan

    2012-02-01

    Full Text Available In the title molecule, C20H20ClN3O4, both the pyrrole N—H groups adopt a syn conformation with respect to the carbonyl groups. In the crystal, intermolecular N—H...O hydrogen bonds link the molecules into layers parallel to (102.

  5. Highly Sensitive Bisphenol-A Electrochemical Aptasensor Based on Poly(Pyrrole-Nitrilotriacetic Acid)-Aptamer Film.

    Kazane, Imen; Gorgy, Karine; Gondran, Chantal; Spinelli, Nicolas; Zazoua, Ali; Defrancq, E; Cosnier, Serge

    2016-07-19

    An electrochemical highly sensitive aptasensor was developed based on electropolymerized poly(pyrrole-nitrilotriacetic) acid film and a new aptamer functionalized by a pentahistidine peptide for the quantification of bisphenol A. A surface coverage of antibisphenol A aptamer of 1.84 × 10(-10) mol cm(-2) was estimated from the electrochemical signal of the [Ru(III)(NH3)6](3+) complex bound by electrostatic interactions onto the aptamer-modified electrode. The binding of bisphenol A onto the polymer film was successfully characterized by electrochemical methods as square wave voltammetry and electrochemical impedance spectroscopy measurements. The designed label-free impedimetric aptasensor displayed a wide linear range from 10(-11) to 10(-6) mol L(-1) with a sensitivity of 372 Ω per unit of log of concentration and an excellent specificity toward interfering agents such as 4,4'-dihydroxybiphenyl and bisphenol P. PMID:27332710

  6. Novel Octahydropyrrolo[3,4-c]pyrroles Are Selective Orexin-2 Antagonists: SAR Leading to a Clinical Candidate.

    Letavic, Michael A; Bonaventure, Pascal; Carruthers, Nicholas I; Dugovic, Christine; Koudriakova, Tatiana; Lord, Brian; Lovenberg, Timothy W; Ly, Kiev S; Mani, Neelakandha S; Nepomuceno, Diane; Pippel, Daniel J; Rizzolio, Michele; Shelton, Jonathan E; Shah, Chandra R; Shireman, Brock T; Young, Lana K; Yun, Sujin

    2015-07-23

    The preclinical characterization of novel octahydropyrrolo[3,4-c]pyrroles that are potent and selective orexin-2 antagonists is described. Optimization of physicochemical and DMPK properties led to the discovery of compounds with tissue distribution and duration of action suitable for evaluation in the treatment of primary insomnia. These selective orexin-2 antagonists are proven to promote sleep in rats, and this work ultimately led to the identification of a compound that progressed into human clinical trials for the treatment of primary insomnia. The synthesis, SAR, and optimization of the pharmacokinetic properties of this series of compounds as well as the identification of the clinical candidate, JNJ-42847922 (34), are described herein. PMID:26087021

  7. Synthesis of 2,2'-Dipyrryl Ketones from Pyrrole-2-carboxylic Acids with Trifluoroacetic Anhydride

    Kim, Se Hee; Lim, Jin Woo; Yu, Jin; Kim, Jae Nyoung [Chonnam National Univ., Gwangju (Korea, Republic of)

    2013-09-15

    An efficient synthesis of 2,2'-dipyrryl ketones has been carried out from pyrrole-2-carboxylic acids using trifluoroacetic anhydride (TFAA). Simultaneous generation of both mixed anhydride and 2-unsubstituted pyrrole, via facile decarboxylation with in-situ generated TFA, made their cross reaction (intermolecular Friedel-Crafts acylation) possible and efficient.

  8. A novel and facile approach for synthesis of 5-amino-7-aryl-6-cyano-4-pyrano[3,2-]pyrroles

    Reza Sandaroos; Saman Damavandi

    2012-07-01

    An efficient and iron-catalysed synthesis of 4-pyrano[3,2-]pyrrole is reported. The reactions proceed through a one-pot, three component cyclocondensation of 3-hydroxypyrrole, malononitrile and various aldehydes to afford 4-pyrano[3,2-]pyrrole derivatives in moderate to good yield using ferric hydrogensulphate, Fe(HSO4)3, as the catalyst.

  9. A copper-catalyzed coupling reaction of vinyl halides and carbazates: application in the assembly of polysubstituted pyrroles.

    Zhou, Chengang; Ma, Dawei

    2014-03-21

    CuI-catalyzed coupling of vinyl halides with carbazates gives N-protected N-alkenylhydrazines, which are condensed with ketones under acidic conditions to give polysubstituted pyrroles. The pyrrole synthesis may go through a similar mechanism with Fischer indole synthesis, which involves a [3,3]-sigmatropic rearrangement and other reactions. PMID:24514455

  10. Isolation and identification of a pyrrolic glutathione conjugate metabolite of the pyrrolizidine alkaloid monocrotaline.

    Lamé, M W; Morin, D; Jones, A D; Segall, H J; Wilson, D W

    1990-05-01

    This report describes the isolation and identification of a monocrotaline-derived, glutathione-conjugated pyrrole obtained from the bile of male Sprague-Dawley rats. Bile obtained from rats given an intravenous bolus of 14C-monocrotaline was fractionated using a series of chromatographic separations. Initial purification with cholestyramine resin removed bile acid and pigment contaminants. Subsequent anion exchange and reversed-phase HPLC separations yielded several fractions that contained the 14C label and tested positive for pyrroles using Ehrlich's reagent. These fractions were analyzed using fast-atom-bombardment tandem mass spectrometry (FAB MS/MS). In addition to glutathione-conjugated dehydroretronecine, at least one other pyrrole present had similar ionic properties. The latter was not present in amounts sufficient for positive identification. PMID:2111054

  11. Acetylcholinesterase-Inhibiting Activity of Pyrrole Derivatives from a Novel Marine Gliding Bacterium, Rapidithrix thailandica

    Khanit Suwanborirux; Anuchit Plubrukarn; Kornkanok Ingkaninan; Akkharawit Kanjana-opas; Supreeya Yuenyongsawad; Oraphan Sakulkeo; Yutthapong Sangnoi

    2008-01-01

    Acetylcholinesterase-inhibiting activity of marinoquinoline A (1), a new pyrroloquinoline from a novel species of a marine gliding bacterium Rapidithrix thailandica, was assessed (IC50 4.9 mM). Two related pyrrole derivatives, 3-(2'-aminophenyl)-pyrrole (3) and 2,2-dimethyl-pyrrolo-1,2-dihydroquinoline (4), were also isolated from two other strains of R. thailandica. The isolation of 3 froma natural source is reported here for the first time. Compound 4 was proposed to be an isolation artifac...

  12. Acetylcholinesterase-Inhibiting Activity of Pyrrole Derivatives from a Novel Marine Gliding Bacterium, Rapidithrix thailandica

    Sangnoi, Yutthapong; Sakulkeo, Oraphan; Yuenyongsawad, Supreeya; Kanjana-opas, Akkharawit; Ingkaninan, Kornkanok; Plubrukarn, Anuchit; Suwanborirux, Khanit

    2008-01-01

    Acetylcholinesterase-inhibiting activity of marinoquinoline A (1), a new pyrroloquinoline from a novel species of a marine gliding bacterium Rapidithrix thailandica, was assessed (IC50 4.9 μM). Two related pyrrole derivatives, 3-(2′-aminophenyl)-pyrrole (3) and 2,2-dimethyl-pyrrolo-1,2-dihydroquinoline (4), were also isolated from two other strains of R. thailandica. The isolation of 3 from a natural source is reported here for the first time. Compound 4 was proposed to be an isolation artifa...

  13. 2-[(E-(1H-Pyrrol-2-ylmethylidenehydrazinyl]pyridine monohydrate

    James L. Wardell

    2009-12-01

    Full Text Available The title hydrate, C10H10N4·H2O, shows a small twist in the hydrozone derivative, the dihedral angle between the pyridine and pyrrole rings being 11.08 (12°. The pyridine and pyrrole N atoms lie to the same side of the molecule being sustained in place by hydrogen-bonding interactions with the water molecule. Further intermolecular O—H...N and N—H...O hydrogen bonding leads to the formation of supramolecular arrays in the ab plane.

  14. Hydrolytic study of the copolymer Poly pyrrole/ Polyethyleneglycol and Poly pyrrole synthesized by plasma; Estudio hidrolitico del copolimero polipirrol/polietilenglicol y polipirrol sintetizado por plasma

    Colin, E.; Enriquez, M.A.; Olayo, M.G.; Cruz, G.J.; Carapia, L.; Romero, M. [ININ, 52045 Ocoyoacac, Estado de Mexico (Mexico); Morales, J.; Olayo, R. [UAM-I, A.P. 55-534 Iztapalapa, Mexico D.F. (Mexico)

    2006-07-01

    In this work the study about the hydrolytic compatibility of semiconductor polymers, copolymer Poly pyrrole/ Polyethyleneglycol (PPy/PEG) and Poly pyrrole (PPy) for their possible use as biomaterials. The polymers were synthesized by plasma between 10 and 100 W, with discharges of splendor RF to 13.5 MHz with resistive coupling. The hydrolytic affinity was evaluated calculating the contact angle with solutions of NaCl, NaCl-MgSO{sub 4} and Krebs-Ringer. The results show a hydrophilicity increment due to the increase of the surface ruggedness with the synthesis energy. On the contrary, the crystallinity diminishes when increasing the power in PPy and it stays approximately constant in PPy/PEG. The electric conductivity presents a growth from 2 to 4 magnitude orders in function of the water content in the polymers. (Author)

  15. Label-free impedimetric biosensor for Salmonella Typhimurium detection based on poly [pyrrole-co-3-carboxyl-pyrrole] copolymer supported aptamer.

    Sheikhzadeh, E; Chamsaz, M; Turner, A P F; Jager, E W H; Beni, V

    2016-06-15

    The Gram-negative bacterium, Salmonella Typhimurium (S. Typhimurium) is a food borne pathogen responsible for numerous hospitalisations and deaths all over the world. Conventional detection methods for pathogens are time consuming and labour-intensive. Hence, there is considerable interest in faster and simpler detection methods. Polypyrrole-based polymers, due to their intrinsic chemical and electrical properties, have been demonstrated to be valuable candidates for the fabrication of chemo/biosensors and functional surfaces. Similarly aptamers have been shown to be good alternatives to antibodies in the development of affinity biosensors. In this study, we report on the combination of poly [pyrrole-co-3-carboxyl-pyrrole] copolymer and aptamer for the development of a label-less electrochemical biosensor suitable for the detection of S. Typhimurium. Impedimetric measurements were facilitated by the effect of the aptamer/target interaction on the intrinsic conjugation of the poly [pyrrole-co-3-carboxyl-pyrrole] copolymer and subsequently on its electrical properties. The aptasensor detected S. Typhimurium in the concentration range 10(2)-10(8)CFUmL(-1) with high selectivity over other model pathogens and with a limit of quantification (LOQ) of 100CFUmL(-1) and a limit of detection (LOD) of 3CFUmL(-1). The suitability of the aptasensor for real sample detection was demonstrated via recovery studies performed in spiked apple juice samples. We envisage this to be a viable approach for the inexpensive and rapid detection of pathogens in food, and possibly in other environmental samples. PMID:26836649

  16. A C2-symmetric ratiometric fluorescence and colorimetric anion sensor based on pyrrole derivative

    A C2-symmetric fluorescence and colorimetric anion sensor (1) based on pyrrole derivative was designed and synthesized according to binding site-signaling subunit approach. The compound 1 was easily prepared by reaction of pyrrole-2,5-dicarboxaldehyde with 4-nitrophenylhydrazine in ethanol (yield=78%). In DMSO, the sensor 1 exhibited a visible color change from red to brown upon exposure to anions such as AcO- and F-; however, no obvious color changes were observed when the other tested anions (e. g. H2PO4-, Cl-, Br- and I-) were added. There was a significant redshift (Δλmax=160 nm) in UV-vis spectrum during UV-vis spectral titrations. In particular, the sensor 1 showed ratiometric fluorescence responses to anions. - Highlights: → C2-symmetric fluorescence and colorimetric anion sensor based on pyrrole derivative was designed and synthesized according to binding site-signaling subunit approach. → The sensor was easily prepared by reaction of pyrrole-2,5-dicarboxaldehyde with 4-nitrophenylhydrazine in ethanol (yield=78%). → In DMSO, the sensor exhibited a visible color change from red to brown upon exposure to anions such as AcO- and F-, however, no obvious color changes were observed when the other anions tested (e. g. H2PO4-, Cl-, Br- and I-) were added. → The sensor showed ratiometric fluorescence responses to anions.

  17. Self-Assembly of Dimeric Tetrathiafulvalene-Calix 4 pyrrole: Receptor for 1,375-Trinitrobenzene

    Nielsen, K. A.; Stein, P. C.

    2011-01-01

    The synthesis and binding properties of a tetrathiafulvalene (TTF)-calix[4]pyrrole receptor 2 appended with one 3,5-dinitrobenzoate guest moiety are reported. The preliminary studies revealed that the receptor is self-compiexing into a dimer receptor 2 center dot 2. The self-complexation of the...

  18. Identification of a new electron-transfer relaxation pathway in photoexcited pyrrole dimers

    Neville, Simon P.; Kirkby, Oliver M.; Kaltsoyannis, Nikolas; Worth, Graham A.; Fielding, Helen H.

    2016-04-01

    Photoinduced electron transfer is central to many biological processes and technological applications, such as the harvesting of solar energy and molecular electronics. The electron donor and acceptor units involved in electron transfer are often held in place by covalent bonds, π-π interactions or hydrogen bonds. Here, using time-resolved photoelectron spectroscopy and ab initio calculations, we reveal the existence of a new, low-energy, photoinduced electron-transfer mechanism in molecules held together by an NH⋯π bond. Specifically, we capture the electron-transfer process in a pyrrole dimer, from the excited π-system of the donor pyrrole to a Rydberg orbital localized on the N-atom of the acceptor pyrrole, mediated by an N-H stretch on the acceptor molecule. The resulting charge-transfer state is surprisingly long lived and leads to efficient electronic relaxation. We propose that this relaxation pathway plays an important role in biological and technological systems containing the pyrrole building block.

  19. A Facile Synthesis of Polysubstituted Pyrroles by One-Pot Three-Component Reaction

    Anaraki-Ardakani, Hossein; Noei, Maziar; Karbalaei-Harofteh, Mina; Zomorodbakhsh, Shahab

    2012-01-01

    A new and efficient one-pot synthesis of polysubstituted pyrrole derivatives by three-component reaction between dialkyl acetylenedicarboxylates, triphenylphosphine, 2-aminopyridin derivatives in the presence of arylglyoxals is described. The reactions were performed in dichloromethane at room temperature and neutral conditions and afforded high yields of products.

  20. Synthesis of Dihydropyrrolizine and Tetrahydroindolizine Scaffolds from Pyrroles by Titanocene(III) Catalysis.

    Hildebrandt, Sven; Gansäuer, Andreas

    2016-08-01

    A synthetic approach to dihydropyrrolizine and tetrahydroindolizine scaffolds from pyrroles has been developed. The key step, a titanocene(III)-catalyzed radical arylation that proceeds by C-H functionalization is atom-economical and tolerates a large variety of functional groups. The reaction is therefore attractive for the swift assembly of functional and structural diversity. PMID:27383638

  1. Clauson Kaas Pyrrole Synthesis Catalyzed by Acidic Ionic Liquid under Microwave Irradiation

    Cigdem Yolacan; Feray Aydogan

    2013-01-01

    A new procedure to synthesize the N-substituted pyrrole derivatives by Clauson Kaas reaction catalyzed by acidic ionic liquid under microwave irradiation was developed. This procedure provides several advantages such as high yield, clean product formation, and short reaction time.

  2. Desorption and photopolymerization behavior of mixed and multilayered styrene-pyrrole nanofilms

    The molecular arrangement and polymerization of adsorbed styrene-pyrrole films were explored using two different dosing schemes: simultaneous dosing to form an intimately mixed film of the two monomers and sequential dosing to form films with distinct layers of styrene and pyrrole. It was found that the desorption of pyrrole was delayed until 175 K when either simultaneously dosed with styrene or in the presence of an overlying styrene layer, whereas it normally desorbs at 165 K when dosed alone. No such effects were observed with styrene in any dosing configuration. The polymerization rate of pyrrole was unaffected in the films when present as the top layer and was observed to decrease by 50% when beneath a styrene layer. Moreover, the rate of polymerization increased by two orders of magnitude in the case of the intimately mixed film. The rate of styrene polymerization was not found to change in any of the explored geometries. These effects are explained by considering the proximity of the components and the potential for screening UV radiation based on their molecular structure

  3. Non-adiabatic dynamics of pyrrole: Dependence of deactivation mechanisms on the excitation energy

    Barbatti, M.; Pittner, Jiří; Pederzoli, Marek; Werner, U.; Mitrić, R.; Bonačić-Koutecký, V.; Lischka, H.

    2010-01-01

    Roč. 375, č. 1 (2010), s. 26-34. ISSN 0301-0104 R&D Projects: GA AV ČR IAA400400810 Institutional research plan: CEZ:AV0Z40400503 Keywords : non-adiabatic dynamics * ultrafast phenomena * pyrrole Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.017, year: 2010

  4. Ferrocene-functionalized 4-(2,5-Di(thiophen-2-yl)-1H-pyrrol-1-yl)aniline: a novel design in conducting polymer-based electrochemical biosensors.

    Ayranci, Rukiye; Demirkol, Dilek Odaci; Ak, Metin; Timur, Suna

    2015-01-01

    Herein, we report a novel ferrocenyldithiophosphonate functional conducting polymer and its use as an immobilization matrix in amperometric biosensor applications. Initially, 4-(2,5-di(thiophen-2-yl)-1H-pyrrol-1-yl)amidoferrocenyldithiophosphonate was synthesized and copolymerized with 4-(2,5-di(thiophen-2-yl)-1H-pyrrol-1-yl)benzenamine at graphite electrodes. The amino groups on the polymer were utilized for covalent attachment of the enzyme glucose oxidase. Besides, ferrocene on the backbone was used as a redox mediator during the electrochemical measurements. Prior to the analytical characterization, optimization studies were carried out. The changes in current signals at +0.45 V were proportional to glucose concentration from 0.5 to 5.0 mM. Finally, the resulting biosensor was applied for glucose analysis in real samples and the data were compared with the spectrophotometric Trinder method. PMID:25591169

  5. Pyrrolo[3,2-b]pyrrole-Based Copolymers as Donor Materials for Organic Photovoltaics

    A new accepter unit, pyrrolo[3,2-b]pyrrole-2,5-dione, was prepared and utilized for the synthesis of the conjugated polymers containing electron donor-acceptor pair for OPVs. Pyrrolo[3,2-b]pyrrole-2,5-dione unit, regioisomer of the known pyrrolo[3,4-c]pyrrole-1,4-dione, is originated from the structure of stable synthetic pigment. The new conjugated polymers with 1,4-diphenylpyrrolo[3,2-b]pyrrole-2,5-dione, thiophene and carbazole were synthesized using Suzuki polymerization to generate P1 and P2. The solid films of P1 and P2 show absorption bands with maximum peaks at about 377, 554 and 374, 542 nm and the absorption onsets at 670 and 674 nm, corresponding to band gaps of 1.85 and 1.84 eV, respectively. To improve the hole mobility of the polymer with 1,4-bis(4-butylphenyl)-pyrrolo[3,2-b]-pyrrole-2,5-dione unit, which was previously reported by us, the butyl group at the 4-positions of the N-substituted phenyl group was substituted with hydrogen and methyl group. The field-effect hole mobility of P2 is 9.6 Χ 10-5 cm2/Vs. The device with P2:PC71BM (1:2) showed VOC value of 0.84 V, JSC value of 5.10 mA/cm2, and FF of 0.33, giving PCE of 1.42%

  6. A new titanium biofunctionalized interface based on poly(pyrrole-3-acetic acid) coating: proliferation of osteoblast-like cells and future perspectives.

    De Giglio, Elvira; Cometa, Stefania; Calvano, Cosima-Damiana; Sabbatini, Luigia; Zambonin, Pier Giorgio; Colucci, Silvia; Benedetto, Adriana Di; Colaianni, Graziana

    2007-09-01

    In recent years, many procedures based on surface modification have been suggested to improve the biocompatibility and biofunctionality of orthopedic titanium-based implants. In this contest, the development of a new titanium-based biomaterial that could be covalently modified with biologically active molecules (i.e., RGD-peptides, growth factors, etc.) able to improve osteoblasts response was investigated. The strategy followed was based on a preliminary coating of the implant material by an adherent thin polymer film to which bioactive molecules could be grafted exploiting the polymer surface chemical reactivity. In this work, we focused our attention on pyrrole-3-acetic acid (Py-3-acetic), a pyrrole with carboxylic acid substituent, whose electrosynthesis and characterization on titanium substrates were already accomplished and whose potentialities in the design of new biocompatible surfaces are well evident. As first step, the biocompatibility of the electrochemically grown PPy-3-acetic films was investigated performing in vitro tests (adhesion and proliferation) with mouse bone marrow cells. Successively, the availability and reactivity of surface carboxylic groups were tested through the grafting of an aminoacidic residue to PPy-3-acetic films. PMID:17483896

  7. A soluble conducting polymer of 2,5-di(thiophen-2-yl)-1-p-tolyl-1H-pyrrole and its electrochromic device

    A monomer 2,5-di(thiophen-2-yl)-1-p-tolyl-1H-pyrrole was synthesized via reaction of 1,4-di(2-thienyl)-1,4-butanedione and p-toluidine in the presence of catalytical amount of p-toluenesulfonic acid. Chemical polymerization of the monomer yielded a soluble polymer. The average molecular weight was determined by gel permeation chromatography as number average molecular weight (Mn) 2.5 x 103 g/mol. The monomer was also electrochemically polymerized in the presence of LiClO4, NaClO4 (1:1) as the supporting electrolyte in acetonitrile. Cyclic Voltammetry, Fourier Transform Infra Red, Nuclear Magnetic Resonance, Scanning Electron Microscopy and Ultraviolet-Visible Spectroscopy were employed for the characterization of the polymer. Spectroelectrochemistry analysis of homopolymer revealed an electronic transition at 428 nm which corresponds to π-π* transition. Switching ability of the homopolymer was evaluated by kinetic studies upon measuring the percent transmittance (%T) at the maximum contrast point, indicating that poly(2,5-di(thiophen-2-yl)-1-p-tolyl-1H-pyrrole) is a suitable material for electrochromic devices

  8. Preparation and evaluation of Pd/polymeric pyrrole-sodium lauryl sulfonate/foam-Ni electrode for 2,4-dichlorophenol dechlorination in aqueous solution

    Polymeric pyrrole-sodium lauryl sulfonate (PPy-SLS) composite film was applied to the preparation of palladium/foam-nickel (Pd/foam-Ni) electrode. The prepared Pd/PPy-SLS/foam-Ni electrode was characterized by cyclic voltammetry (CV), scanning electron microscope (SEM), X-ray diffraction (XRD), inductively coupled plasma-atomic emission spectroscopy (ICP-AES), and X-ray photoelectron spectroscopy (XPS). The addition of SLS improved the polymerization of pyrrole to form PPy-SLS film, which was conducive to prepare small Pd microparticles and led to the lower Pd loading, 0.85 mg cm−2. The composite electrode was used for electrochemically reductive dechlorination of 2,4-dichlorophenol (2,4-DCP) in aqueous solution. The influences of dechlorination current and initial pH value on the conversion efficiency and current the efficiency of 2,4-DCP dechlorination were studied. Complete dechlorination could be achieved on the Pd/PPy-SLS/foam-Ni electrode at ambient temperature under the condition of dechlorination current of 5 mA and initial pH value of 2.5 within 50 min. The electrode exhibits promising potential for dechlorination with high catalytic activity, good stability and low cost

  9. Biofabrication Using Pyrrole Electropolymerization for the Immobilization of Glucose Oxidase and Lactate Oxidase on Implanted Microfabricated Biotransducers

    Christian N. Kotanen

    2014-03-01

    Full Text Available The dual responsive Electrochemical Cell-on-a-Chip Microdisc Electrode Array (ECC MDEA 5037 is a recently developed electrochemical transducer for use in a wireless, implantable biosensor system for the continuous measurement of interstitial glucose and lactate. Fabrication of the biorecognition membrane via pyrrole electropolymerization and both in vitro and in vivo characterization of the resulting biotransducer is described. The influence of EDC-NHS covalent conjugation of glucose oxidase with 4-(3-pyrrolyl butyric acid (monomerization and with 4-sulfobenzoic acid (sulfonization on biosensor performance was examined. As the extent of enzyme conjugation was increased sensitivity decreased for monomerized enzymes but increased for sulfonized enzymes. Implanted biotransducers were examined in a Sprague-Dawley rat hemorrhage model. Resection after 4 h and subsequent in vitro re-characterization showed a decreased sensitivity from 0.68 (±0.40 to 0.22 (±0.17 µA·cm−2·mM−1, an increase in the limit of detection from 0.05 (±0.03 to 0.27 (±0.27 mM and a six-fold increase in the response time from 41 (±18 to 244 (±193 s. This evidence reconfirms the importance of biofouling at the bio-abio interface and the need for mitigation strategies to address the foreign body response.

  10. Direct Arylation of Pyrroles via Indirect Electroreductive C-H Functionalization Using Perylene Bisimide as an Electron-Transfer Mediator.

    Sun, Guoquan; Ren, Shuya; Zhu, Xinhai; Huang, Manna; Wan, Yiqian

    2016-02-01

    The indirect electroreductive coupling of aryl halides and pyrroles was successfully conducted using a catalytic amount of perylene bisimide as a mediator in 1-ethyl-3-methylimidazolium bis((trifluoromethyl)sulfonyl)imide ([EMIM]NTf2)/DMSO. PMID:26800089

  11. Use of Graphite Oxide and Graphene Oxide as Catalysts in the Synthesis of Dipyrromethane and Calix[4]pyrrole

    Sweta Mishra

    2011-08-01

    Full Text Available Graphite oxide and graphene oxides have been used as solid catalysts for the synthesis of 5,5-dialkyldipyrromethanes and calix[4]pyrroles in organic and aqueous solutions at room temperature.

  12. 3-/3,5-Pyrrole-substituted BODIPY derivatives and their photophysical and electrochemical studies

    KARTHIKA J KADASSERY; AKANKSHA NIMESH; SANOJ RAJ; NEERAJ AGARWAL

    2016-09-01

    Nucleophilic substitution on 3-bromo/3,5-dibromo-4,4'-difluoro-8-(aryl)-4-bora-3a,4a-diaza-sindacene (BODIPY), substituted with anisyl or thienyl at meso positions, with neat pyrrole afforded the mono and di-pyrrole substituted BODIPYs 1–4 in good yields. Large bathochromic shifts, upto ∼180 nm in absorption maxima (581–682 nm), and fluorescence maxima (606–695 nm) were observed for these BODIPYs. Absorption and fluorescence properties were studied in different solvents to compare the effect of mono and di substitution on BODIPY. The Lippert-Mataga equations were used which predict strong polarization of monosubstituted BODIPYs. Electrochemical studies were carried out to find the oxidation potential and HOMO energy levels were calculated. Theoretical studies of 1–4 provide the insight on the electron density distribution in 1–4. Theoretical and experimental photo-physical studies in different solvents were correlated to findthe substituent effects on BODIPY.

  13. The electropolymerization of pyrrole at a CuNi electrode: corrosion protection properties

    Fenelon, Anna M.; Breslin, Carmel B

    2003-12-01

    Pyrrole was successfully electropolymerized at a copper-nickel electrode in a near-neutral sodium oxalate solution containing Cu{sup 2+} cations to generate a homogenous and adherent polypyrrole film. The presence of the Cu{sup 2+} ions increased both the rate of the electropolymerization reaction and the adherence of the polymer at the CuNi interface. In the absence of these cations, oxidation of the electrode occurred generating a nickel-rich layer that was not sufficiently conducting, under the electropolymerization conditions employed, to facilitate the electron-transfer reaction and the electropolymerization of pyrrole. These films remained stable and exhibited significant corrosion protection properties in acidified and neutral 0.1 mol dm{sup -3} NaCl solutions even on polarization of the electrodes to high anodic potentials.

  14. New pentasubstituted pyrrole hybrid atorvastatin-quinoline derivatives with antiplasmodial activity.

    Carvalho, Rita C C; Martins, Wagner A; Silva, Tayara P; Kaiser, Carlos R; Bastos, Mônica M; Pinheiro, Luiz C S; Krettli, Antoniana U; Boechat, Núbia

    2016-04-15

    Cerebral malaria is caused by Plasmodium falciparum. Atorvastatin (AVA) is a pentasubstituted pyrrole, which has been tested as an adjuvant in the treatment of cerebral malaria. Herein, a new class of hybrids of AVA and aminoquinolines (primaquine and chloroquine derivatives) has been synthesized. The quinolinic moiety was connected to the pentasubstituted pyrrole from AVA by a linker group (CH2)n=2-4 units. The activity of the compounds increased with the size of the carbons chain. Compound with n=4 and 7-chloroquinolinyl has displayed better activity (IC50=0.40μM) than chloroquine. The primaquine derivative showed IC50=1.41μM, being less toxic and more active than primaquine. PMID:26988303

  15. Dichloridobis(4-pyridylmethyl 1H-pyrrole-2-carboxylate-κNzinc

    Guilong Zhang

    2012-03-01

    Full Text Available In the title molecule, [ZnCl2(C11H10N2O22], the ZnII ion, situated on a twofold axis, is in a distorted tetrahedral coordination environment formed by two chloride anions and two pyridine N atoms of the two organic ligands. In the pyrrole-2-carboxylate unit, the pyrrole N—H group and the carbonyl group point approximately in the same direction. The dihedral angle between the two pyridine rings is 54.8 (3°. The complex molecules are connected into chains extending along [101] by N—H...Cl hydrogen bonds. The chains are further assembled into (-101 layers by C—H...O and C—H...Cl interactions.

  16. Pyrrole Azocrown Ethers. Synthesis, Complexation, Selective Lead Transport and Ion-Selective Membrane Electrode Studies

    Luboch, Elzbieta; Wagner-Wysiecka, Ewa; Fainerman-Melnikova, Marina; Lindoy, Leonard F.; Biernat, Jan F.

    2006-01-01

    Abstract New 21-membered lipophilic crown ethers, each incorporating a pyrrole unit and two azo groups as macrocyclic ring components, have been synthesized. The complexation behavior of these and two further macrocycles has been investigated in acetonitrile. These ligand systems have been employed as ionophores in transport experiments involving the competitive transport behavior of an equimolar mixture of Co2+, Ni2+, Cu2+, Zn2+, Cd2+, Ag+ and Pb2+ across a water (pH 4.9)/chlorof...

  17. A joint experimental and computational investigation on the thermochemistry of (nitrophenyl)pyrroles

    Santos, Ana Filipa L.O.M. [Centro de Investigacao em Quimica, Department of Chemistry, Faculty of Science, University of Porto, Rua do Campo Alegre, 687, P-4169-007 Porto (Portugal); Ribeiro da Silva, Manuel A.V., E-mail: risilva@fc.up.p [Centro de Investigacao em Quimica, Department of Chemistry, Faculty of Science, University of Porto, Rua do Campo Alegre, 687, P-4169-007 Porto (Portugal)

    2010-08-15

    This paper reports the standard (p{sup o} = 0.1 MPa) molar enthalpies of formation, in the gaseous phase, {Delta}{sub f}H{sub m}{sup 0}(g), at T = 298.15 K, of 1-(2-nitrophenyl)pyrrole and of 1-(4-nitrophenyl)pyrrole as (235.7 {+-} 2.7) kJ . mol{sup -1} and (205.5 {+-} 2.5) kJ . mol{sup -1}, respectively. These values were derived from experimental thermodynamic parameters, namely from the standard (p{sup o} = 0.1 MPa) molar enthalpies of formation, in the crystalline phase, {Delta}{sub f}H{sub m}{sup 0}(cr), at T = 298.15 K, obtained from the standard molar enthalpies of combustion, {Delta}{sub c}H{sub m}{sup 0}, measured by static-bomb combustion calorimetry, and from the standard molar enthalpies of sublimation, at T = 298.15 K, determined from the temperature-vapour pressure dependence, obtained by the Knudsen mass loss effusion method. Additionally, the gas-phase enthalpies of formation were estimated by G3(MP2)//B3LYP calculations, using several gas-phase working reactions, and were compared with the experimental determined ones. Experimental and theoretical results are in very good agreement and show that 1-(4-nitrophenyl)pyrrole is thermodynamically more stable than the 2-isomer. This composite approach was also used to estimate the gas-phase enthalpy of formation of the 1-(3-nitrophenyl)pyrrole.

  18. Design and synthesis of hepatoselective, pyrrole-based HMG-CoA reductase inhibitors.

    Pfefferkorn, Jeffrey A; Song, Yuntao; Sun, Kuai-Lin; Miller, Steven R; Trivedi, Bharat K; Choi, Chulho; Sorenson, Roderick J; Bratton, Larry D; Unangst, Paul C; Larsen, Scott D; Poel, Toni-Jo; Cheng, Xue-Min; Lee, Chitase; Erasga, Noe; Auerbach, Bruce; Askew, Valerie; Dillon, Lisa; Hanselman, Jeffrey C; Lin, Zhiwu; Lu, Gina; Robertson, Andrew; Olsen, Karl; Mertz, Thomas; Sekerke, Catherine; Pavlovsky, Alexander; Harris, Melissa S; Bainbridge, Graeme; Caspers, Nicole; Chen, Huifen; Eberstadt, Matthias

    2007-08-15

    This manuscript describes the design and synthesis of a series of pyrrole-based inhibitors of HMG-CoA reductase for the treatment of hypercholesterolemia. Analogs were optimized using structure-based design and physical property considerations resulting in the identification of 44, a hepatoselective HMG-CoA reductase inhibitor with excellent acute and chronic efficacy in a pre-clinical animal models. PMID:17574412

  19. 2-(2-hydroxyethyl)-1H,3H-benzo[c]pyrrol-1-one

    Urban, Jiří; Fábry, Jan; Zuman, P.; Ludvík, Jiří; Císařová, I.

    2007-01-01

    Roč. 63, - (2007), o4137-o4138. ISSN 1600-5368 R&D Projects: GA MŠk 1P05ME785 Institutional research plan: CEZ:AV0Z40400503; CEZ:AV0Z10100520 Keywords : 2-(2-hydroxyethyl)-1H,3H-benzo[c]pyrrol-1-one * hydrogen bonds * interactions Subject RIV: CG - Electrochemistry Impact factor: 0.508, year: 2007

  20. tert-Butyl 2-borono-1H-pyrrole-1-carboxylate

    Zheng Zhong

    2009-04-01

    Full Text Available In the crystal structure of the title compound, C9H14BNO4, the boronic acid group and carbamate groups are nearly co-planar with the pyrrole ring, making dihedral angles of 0.1 (2 and 2.2 (2°, respectively. Intramolecular and intermolecular O—H...O hydrogen bonds help to stabilize the structure, the latter interaction leading to inversion dimers..

  1. Interaction of derived polymers from pyrrole with biocompatible solutions; Interaccion de polimeros derivados de pirrol con soluciones biocompatibles

    Lopez G, O. G.

    2010-07-01

    This work presents a study about the synthesis by plasma, the electric properties and superficial interaction of polymers derived from pyrrole doped with Iodine with potential use as bio material. Poly-pyrrole is a semiconductor and biocompatible polymer with potential application in the development of artificial muscles and implants where the electric interaction between cells and material is an important variable. The syntheses were made at 13.5 MHz in a glass tubular reactor of 1500 cm{sup 3} with electrodes of 6.5 cm diameter and stainless steel flanges. An electrode was connected to the RF terminal of the power supply that is combined with a matching coupling resistance. The monomer and dopant used in this work were pyrrole and Iodine respectively, in closed containers. They were vaporized and injected separately into the reactor at room temperature and 0.1 mbar. The vapors of the reagents mixed freely in the reactor. The synthesis time was 240 min at 40, 60, 80 and 100 W. The polymers were obtained as thin films adhered to the reactor walls. The films were washed and swollen with distilled water and removed from the reactor walls with a small spatula. The polymers were irradiated with gamma rays at 18 and 22 KGy. Due to the fact that the doses are cumulative, the final dose applied was 40 KGy. The polymers characterization was carried out by Fourier Transform Infrared Spectroscopy, thermogravimetric analysis (TGA), scanning electron microscopy, contact angle, electrical conductivity and X-ray diffraction. The analyses indicates that the polymers have very similar structure in almost the entire power range, showing C-O, C=C, C-H, O-H, N-H bonds with a predominantly amorphous structure. The TGA analyses showed that the material has 4 or 5 loses of material. The first one starts after that 115 C except for the material irradiated at 40 KGy, this one begins in 87 C, the second one is in the interval of 196 and 295 C, the third one between 311 and 500 C, and the

  2. Electrodeposition of (pyrrole-co-phenol) on steel surfaces in mixed electrolytes of oxalic acid and DBSA

    Poly (pyrrole-co-phenol) (co-PyPh) was synthesised using cyclic voltammetry in the mixture of dodecyl benzene sulphonic acid (DBSA) with oxalic acid solution on steel electrodes. The morphology and compositions were characterized by Field Emission Scanning Electron Microscopy (FESEM), Fourier Transform Infrared Spectroscopy (FTIR) techniques and Energy-dispersive X-ray spectroscopy (EDX). Electrode/co-PyPh/electrolyte system was studied in 0.1 M NaCl solutions by Electrochemical Impedance Spectroscopy (EIS). The Warburg impedance observed in mid frequency region is an evidence of the effective barrier behaviour of coating. The results of EDX indicate that the content of doped sulphur can influence the morphology of co-PyPh. Three dissimilar morphologies of co-PyPh and different amount of doped sulphur in co-PyPh are observed. The existence of phenol monomer leads to a decrease in the amount of doped sulphur in co-PyPh compared with synthesised polypyrrole (PPy) in the same environment.

  3. A soluble conducting polymer: 1-Phenyl-2,5-di(2-thienyl)-1H-pyrrole and its electrochromic application

    Tarkuc, S. [Department of Chemistry, Middle East Technical University, 06531 Ankara (Turkey); Sahmetlioglu, E. [Department of Chemistry, Middle East Technical University, 06531 Ankara (Turkey); Department of Chemistry, Nigde University, 51100 Nigde (Turkey); Tanyeli, C. [Department of Chemistry, Middle East Technical University, 06531 Ankara (Turkey); Akhmedov, I.M. [Department of Chemistry, Middle East Technical University, 06531 Ankara (Turkey); Toppare, L. [Department of Chemistry, Middle East Technical University, 06531 Ankara (Turkey)]. E-mail: toppare@metu.edu.tr

    2006-07-28

    A thiophene-functionalized monomer 1-phenyl-2,5-di(2-thienyl)-1H-pyrrole (PTP) was synthesized. The chemical polymerization of PTP (CPTP) was realized by using FeCl{sub 3} as the oxidant. The structures of both the monomer and the soluble polymer (CPTP) were investigated by Nuclear Magnetic Resonance ({sup 1}H and {sup 13}C NMR) and Fourier Transform Infrared (FTIR). The average molecular weight of the chemically synthesized polymer was determined by gel permeation chromatography (GPC) as Mn = 7.2 x 10{sup 3}. The electrochemical oxidative polymerization of PTP was carried out via constant-potential electrolysis. Characterizations of the resulting polymer were done by cyclic voltammetry (CV), FTIR, Scanning Electron Microscopy (SEM) and UV-vis Spectroscopy. The conductivity of sample was measured by four-probe technique. Moreover, the spectroelectrochemical and electrochromic properties of the polymer film were investigated. Spectroelectrochemical analysis of P(PTP) revealed electronic transitions at 413, 577 and 884 nm corresponding to {pi}-{pi}* transition, polaron, and bipolaron band formations, respectively. Kinetic studies evaluated the switching ability of the P(PTP); the percent transmittance T% was found as 27%. The homopolymer of PTP was used to construct dual-type polymer electrochromic devices (ECDs) against poly(3,4-ethylenedioxythiophene) (PEDOT). Spectroelectrochemistry, electrochromic switching and open circuit stability of the devices were investiga0009t.

  4. A soluble conducting polymer: 1-Phenyl-2,5-di(2-thienyl)-1H-pyrrole and its electrochromic application

    A thiophene-functionalized monomer 1-phenyl-2,5-di(2-thienyl)-1H-pyrrole (PTP) was synthesized. The chemical polymerization of PTP (CPTP) was realized by using FeCl3 as the oxidant. The structures of both the monomer and the soluble polymer (CPTP) were investigated by Nuclear Magnetic Resonance (1H and 13C NMR) and Fourier Transform Infrared (FTIR). The average molecular weight of the chemically synthesized polymer was determined by gel permeation chromatography (GPC) as Mn = 7.2 x 103. The electrochemical oxidative polymerization of PTP was carried out via constant-potential electrolysis. Characterizations of the resulting polymer were done by cyclic voltammetry (CV), FTIR, Scanning Electron Microscopy (SEM) and UV-vis Spectroscopy. The conductivity of sample was measured by four-probe technique. Moreover, the spectroelectrochemical and electrochromic properties of the polymer film were investigated. Spectroelectrochemical analysis of P(PTP) revealed electronic transitions at 413, 577 and 884 nm corresponding to π-π* transition, polaron, and bipolaron band formations, respectively. Kinetic studies evaluated the switching ability of the P(PTP); the percent transmittance T% was found as 27%. The homopolymer of PTP was used to construct dual-type polymer electrochromic devices (ECDs) against poly(3,4-ethylenedioxythiophene) (PEDOT). Spectroelectrochemistry, electrochromic switching and open circuit stability of the devices were investigated

  5. Preparation of thin α-particle sources using poly-pyrrole films functionalized by a chelating agent

    This work takes place in the scope of analysis of the α-particle emitting elements U, Pu and Am present in compound environmental matrix like sols and sediments. The samples diversity and above all the α-ray characteristics require the analyst to implement a sequence of chemical steps in which the more restricting is the actinides concentration in a uniform and thin layer en allowing an accurately measure of alpha activity. On this account, we studied a new technique for radioactive sources preparation based on tow steps: preparation of a thin film as source support; incorporation of radioactive elements by a chelating extraction mechanism. The thin films were obtained through electro-polymerization of pyrrole monomer functionalized by an chelating ligand able to extract actinides from concentrated acidic solutions. Polymerization conditions of this monomer were perfected, then obtained films were characterized from a physico-chemical point of view. We point out their extracting properties were comparable to (retention capacity, distribution coefficient) to those of usual ion-exchange resins. The underscore of uranyl and americium nitrate complexes formed in the thin layer allowed to calculate the extraction constants in case acid extraction is negligible. Thanks to this results, the values of the coefficients distribution DU and DAm could be provided for all nitric solutions in which acid extraction is negligible. Optimal actinides retention conditions in the polymer were defined and used to settle a protocol for plutonium analysis in environmental samples. (author)

  6. Electrochromic and electrochemical properties of 3-pyridinyl and 1,10-phenanthroline bearing poly(2,5-di(2-thienyl)-1H-pyrrole) derivatives

    Hwang, Jaeyoung; Ik Son, Jung; Shim, Yoon-Bo [Department of Chemistry, Pusan National University, Keumjeong-ku, Busan 609-735 (Korea)

    2010-07-15

    This study examined a highly efficient synthetic route and characterization of two derivatives of 2,5-di(2-thienyl)-1H-pyrrole that incorporated 3-pyridinyl and 1,10-phenanthroline moieties in the central pyrrole ring. The electrically conductive polyPTPy and polyPhenTPy films were synthesized through electropolymerization on a glassy carbon electrode in a 0.1 M TBAP/dichloromethane solution. The polymer films were characterized using cyclic voltammetry (CV), in situ conductivity measurements, and in situ spectroelectrochemistry. The redox peaks of the polyPTPy and polyPhenTPy films were observed at 0.96/0.66 and 0.89/0.73 V, respectively. The maximum conductivities of polyPTPy and polyPhenTPy were 6.5 x 10{sup -2} and 9.2 x 10{sup -2} S/cm at 1.4 V. The spectroelectrochemical analysis showed that the polyPTPy film was brownish-yellow color ({lambda}{sub max}=430 nm) in the neutral state and dark blue (1.4 V) in the fully oxidized state. Similarly, polyPhenTPy was greenish-yellow color ({lambda}{sub max}=451 nm) in the neutral state and light blue (1.4 V) in the fully oxidized state. The polymer films exhibited a fast optical switching time within 1.0 s. The electrochemical and spectroelectrochemical characterizations of these films revealed that the materials were highly electroactive and robust in terms of electrochromics. (author)

  7. Spectral, IR and magnetic studies of Mn(II), Co(II), Ni(II) and Cu(II) complexes with pyrrole-2-carboxyaldehyde thiosemicarbazone (L)

    Chandra, Sulekh; Kumar, Anil

    2007-11-01

    Mn(II), Co(II), Ni(II) and Cu(II) complexes are synthesized with thiosemicarbazone (L) derived from pyrrole-2-carboxyaldehyde. These complexes are characterized by elemental analysis, molar conductance, magnetic susceptibility measurement, mass, IR, electronic and EPR spectral studies. The molar conductance measurement of the complexes in DMSO indicates that the complexes are non-electrolyte except Co(L) 2(NO 3) 2 and Ni(L) 2(NO 3) 2 complexes which are 1:2 electrolyte. All the complexes are of high-spin type. On the basis of spectral studies an octahedral geometry may be assigned for Mn(II), Co(II) and Ni(II) complexes except Co(L) 2(NO 3) 2 and Ni(L) 2(NO 3) 2 which are of tetrahedral geometry. A tetragonal geometry may be suggested for Cu(II) complexes.

  8. Biological activity of two new pyrrole derivatives against stored-product species: influence of temperature and relative humidity.

    Boukouvala, M C; Kavallieratos, N G; Athanassiou, C G; Hadjiarapoglou, L P

    2016-08-01

    Members of the pyrrole group are likely to have interesting properties that merit additional investigation as insecticides at the post-harvest stages of agricultural commodities. In the present work, the insecticidal effect of two new pyrrole derivatives, ethyl 3-(benzylthio)-4,6-dioxo-5-phenyl-2,4,5,6-tetrahydropyrrolo[3,4-c]pyrrole-carboxylate (3i) and isopropyl 3-(benzylthio)-4,6-dioxo-5-phenyl-2,4,5,6-tetrahydropyrrolo[3,4-c]pyrrole-carboxylate (3k) were studied as stored-wheat protectants against two major stored-product insect species, the confused flour beetle, Tribolium confusum Jaquelin du Val adults and larvae and the Mediterranean flour moth, Ephestia kuehniella Zeller larvae at different doses (0.1, 1 and 10 ppm), exposure intervals (7, 14 and 21 days), temperatures (20, 25 and 30°C) and relative humidity (55 and 75%) levels. For T. confusum adults, in the case of the pyrrole derivative 3i, mortality was low and it did not exceed 32.2% in wheat treated with 10 ppm 3i at 30°C and 55% relative humidity. Progeny production was very low (insecticidal effect, but this effect is moderated by the exposure, the target species, the temperature and the relative humidity. PMID:27087458

  9. Quantification of CH-π Interactions Using Calix[4]pyrrole Receptors as Model Systems

    Gemma Aragay

    2015-09-01

    Full Text Available We describe the use of two series of aryl-extended calix[4]pyrrole receptors bearing two and four electronically tunable phenyl groups, respectively, in their meso-positions as model systems for the quantification of CH-π interactions in solution. The “four-wall” and the “two-wall” receptors formed thermodynamically stable 1:1 complexes in acetonitrile solution with both trimethylamine N-oxide and trimethylphosphine P-oxide as guests. The complexes were mainly stabilized by the formation of four convergent hydrogen bonds between the oxygen atom of the guests and the pyrrole NHs of the host. In general, the N-oxide produced thermodynamically more stable hydrogen bonding interactions than the P-oxide. Upon guest binding, the receptors adopted the cone conformation and the methyl groups of the included guests engaged in CH-π interactions with the aromatic walls. We show that the modification of the electronic properties of the aromatic surfaces, in any of the receptor series, did not have a significant impact in the measured binding affinities for a given guest. However, the larger binding affinities determined for the “four-wall” receptors in comparison to the “two-wall” counterparts supported the importance of CH-π interactions on guest complexation. The strength of the CH-π interactions present in the inclusion complexes was quantified employing the octamethyl calix[4]pyrrole as reference. We determined an average magnitude of ~1 kcal·mol−1 for each CH-π interaction. The CH-π interactions featured a reduced electrostatic nature and thus dispersion forces were assigned as main contributors of their strength.

  10. Electrochemical polymerization of pyrrole over AZ31 Mg alloy for biomedical applications

    Highlights: ► Polymerization of pyrrole over AZ31 Mg was carried out using cyclic voltammetry. ► Pyrrole concentration was optimized to accomplish the adherent and uniform coating. ► Effect of monomer concentration on the surface morphology was discussed. ► Corrosion resistance of AZ31 Mg in SBF was studied as a function of Py concentration. ► PPy coated AZ31 Mg alloy exhibited enhanced corrosion resistance at 0.25 M of Py. -- Abstract: Electrochemical polymerization of pyrrole (Py) from aqueous salicylate solution over AZ31 Mg alloy was carried out using cyclic voltammetry (CV). The effect of monomer concentration on the surface and electrochemical corrosion in simulated body fluid (SBF) were analysed. Attenuated total reflection-infrared (ATR-IR) spectra showed the characteristic ring stretching peaks for polypyrrole (PPy). Scanning electron microscopy (SEM) and atomic force microscopy (AFM) studies exhibited typical cauliflower morphology with rough surface for PPy coated AZ31 Mg alloy. Open circuit potential measurement and potentiodynamic polarization studies revealed that the coating prepared using 0.25 M of Py had positive shift of about 120 mV in corrosion potential and lower corrosion current density (0.03 mA/cm2) compared to other concentrations and uncoated AZ31 Mg alloy (0.25 mA/cm2). Electrochemical impedance spectroscopic (EIS) studies of uncoated and PPy coated Mg alloy in SBF revealed three-time constants behaviour with about one order of increment in impedance value for 0.25 M of Py

  11. Sustainable Pathways to Pyrroles through Iron-Catalyzed N-Heterocyclization from Unsaturated Diols and Primary Amines.

    Yan, Tao; Barta, Katalin

    2016-09-01

    Pyrroles are prominent scaffolds in pharmaceutically active compounds and play an important role in medicinal chemistry. Therefore, the development of new, atom-economic, and sustainable catalytic strategies to obtain these moieties is highly desired. Direct catalytic pathways that utilize readily available alcohol substrates have been recently established; however, these approaches rely on the use of noble metals such as ruthenium or iridium. Here, we report on the direct synthesis of pyrroles using a catalyst based on the earth-abundant and inexpensive iron. The method uses 2-butyne-1,4-diol or 2-butene-1,4-diol that can be directly coupled with anilines, benzyl amines, and aliphatic amines to obtain a variety of N-substituted pyrroles in moderate-to-excellent isolated yields. PMID:27493031

  12. Thermal Diffusivity Measurement of Poly pyrrole-Chitosan Composite by Photoacoustic Technique

    Thermal diffusivity is a physical quantity that represents an intrinsic property for a material and indicates how fast heat propagates through a sample. The photoacoustic (PA) technique has recently been recognized as a powerful and reliable experimental technique in measuring thermal diffusivity. This effect is described as the periodic heating generated in the sample by a nonradiative deexcitation process due to the absorption of a modulated light source [1]. In present work, the conducting polymer composite films of poly pyrrole-chitosan (PPy- CHI) were synthesized by electrochemical polymerization method. The electrical conductivity and thermal diffusivity of composite film were studied as a function of electro polymerization conditions. (author)

  13. Gliclazide impurity F: N-[(perhydrocyclopenta[c]pyrrol-2-ylaminocarbonyl]-o-toluenesulfonamide

    Di Wu

    2012-02-01

    Full Text Available The title compound, C15H21N3O3S, is known to be an impurity of gliclazide [systematic name: N-(hexahydro-1H-cyclopenta[c]pyrrol-2-ylcarbamoyl-4-methylbenzenesulfonamide], a sulfonylurea antidiabetic drug. Gliclazide has a p-tolyl group substituting the sulfonamide functionality, while the title molecule contains an o-tolyl group. Both five-membered fused rings adopt envelope conformations. In the crystal, N—H...O hydrogen bonds are formed between HN(C=ONH groups, building centrosymmetric dimers. These dimers are further linked through N—H...O(sulfonyl contacts, forming chains in [100].

  14. Low frequency ac conduction and dielectric relaxation in poly(N-methyl pyrrole)

    Amarjeet K Narula; Ramadhar Singh; Subhas Chandra

    2000-06-01

    The ac conductivity and dielectric constant of poly(N-methyl pyrrole) thin films have been investigated in the temperature range 77–350 K and in the frequency range 102–106 Hz. The well defined loss peaks have been observed in the temperature region where measured ac conductivity approaches dc conductivity. These loss peaks are associated with the hopping of the charge carriers. The frequency and temperature dependence of ac conductivity have been qualitatively explained by considering the contribution from two mechanisms; one giving a linear dependence of conductivity on frequency and other having distribution of relaxation times giving rise to broad dielectric loss peak.

  15. Biosynthesis, asymmetric synthesis, and pharmacology, including cellular targets, of the pyrrole-2-aminoimidazole marine alkaloids

    Al-Mourabit, A.; Zancanella, M.A.; Tilvi, S.; Romo, D.

    O O proline ornithine arginine histidine lysine simple precursors c o mp le x mo no m e r s , d i mer s a n d t e t r a m e rs reactive intermediates H N O stylissadine A O NH Br Br NH O HN Br Br N O HN NH 2 N HN H 2 N OH N H O NH Br Br NH O HN... biosynthetic studies, still leaves the question unanswered. Based on some synthetic studies and the isolation of a C 11 N 5 diketopiperazine, verpacamide C (18), Al-Mourabit and coworkers proposed proline or arginine as early precursors for both the pyrrole...

  16. Diethyl 2-amino-5-[(E-(1-methyl-1H-pyrrol-2-ylmethylideneamino]thiophene-3,4-dicarboxylate

    Stéphane Dufresne

    2010-12-01

    Full Text Available The structure of the title compound, C16H19N3O4S, shows the planes described by the thiophene and the pyrroles are twisted by 17.06 (4°. Additionally, the structure shows the azomethine bond adopts the E configuration, while the pyrrole is disordered as a heterocycle flip [occupancy ratio 0.729 (5:0.271 (5]. The three-dimensional network is well packed and involves N–H...O hydrogen bonding and π–π stacking [centroid–centroid distance = 4.294 (8 Å].

  17. Ethyl (2E-2-cyano-3-(1-methyl-1H-pyrrol-2-ylprop-2-enoate

    Abdullah M. Asiri

    2011-09-01

    Full Text Available The 15 non-H atoms of the title compound, C11H12N2O2, are approximately coplanar, the r.m.s. deviation being 0.145 Å. The major deviation from coplanarity is seen in a twist between the ethene (E configuration and pyrrole rings [C—C—N—C torsion angle = −8.26 (18°]. The carbonyl O and cyano N atoms are syn to each other. In the crystal, supramolecular linear tapes linked by C—H...O and C—H...N interactions are further connected by C—H...π(pyrrole interactions.

  18. Synthesis of furans and pyrroles via migratory and double migratory cycloisomerization reactions of homopropargylic aldehydes and imines

    Shiroodi, Roohollah Kazem; Vera, Claudia I. Rivera; Dudnik, Alexander S.; Gevorgyan, Vladimir

    2015-01-01

    A novel gold-catalyzed divergent sysnthesis of furans and pyrroles employing readily available homopropargylic aldehydes and imines have been developed. The regiochemical outcome of this reaction is dependent on the substituent on the terminal alkyne of substrate. Thus, substrates possessing alkyl and aryl substituent at the alkyne moiety produce 2,3,5-substituted furans and pyrroles via a migratory cycloisomerizaton reaction. Whereas, their silicon analogues are capable to undergo a double migratory process leading to 2,3,4-substituted heterocycles. PMID:26185336

  19. Polymers and copolymers of pyrrole and thiophene as electrodes in lithium cells

    Pinto, M.I.S. de; Mishima, H.T.; Mishima, B.A.L. de [Universidad Nacional de Santiago del Estero (Argentina). Inst. de Cs. Quimicas

    1997-07-01

    The performance of pyrrole and thiophene polymer electrodes in lithium cells has been examined in the lithium perchlorate-propylene carbonate electrolyte by cyclic voltammetry. Polypyrrole films were synthesized in `wet` and `dry` conditions; pyrrole and thiophene copolymers were prepared at different potentials and bilayers were prepared by sequential deposition of polythiophene (PTh) and polypyrrole (PPy) films. The polymers were cycled between 2.0V and 4.0V in the lithium cells. The effects of disconnecting the electrodes from the cell on the behaviour of the polymers regarding doping and coulombic efficiency were also studied. The cycling performance of the `wet` PPy is better than `dry` PPy, bilayer PTg/PPy and copolymers. No mixed behaviour was observed for a bilayer where the inner layer was polythiophene and the outer layer was polypyrrole with a thickness PP6/Pth ratio equal to ten. The copolymer prepared at 3.9V vs Li/Li{sup +} showed the higher energy capacity in Wh kg{sup -1} calculated from the anodic charge. (Author)

  20. Electrochemical Detection of Clenbuterol in Pig Liver at Pyrrole-DNA Modified Boron-doped Diamond Electrode

    WU Jing; LI Xiao-li; WU Xu-mei; HUAN Shuang-yan; SHEN Guo-li; YU Ru-qin

    2005-01-01

    The direct detection of clenbuterol(CL) in pig liver without any extraction separation at a pyrrole-DNA modified boron-doped diamond(BDD) electrode is reported. The pyrrole-DNA modified BDD electrode has a strong electrocatalytic effect on the redox reaction of CL. One oxidization and two reduction peaks of CL appear at 340.2, 299.8 and 166.6 mV(versus SCE), respectively. The pyrrole polymer alone cannot electrocatalyze the above reaction at a BDD electrode; the electrocatalytic effect of a BDD electrode modified with DNA membrane is unsufficient for the analytical detection of CL; the replacement of boron-doped diamond by glass carbon makes the electrocatalytic reaction impossible; the redox process is pH dependent. The influences of various experimental parameters on the pyrrole-DNA modified BDD electrode were investigated. A sensitive cyclic voltammetric response for CL was obtained in a linear range from 3.4×10-6 to 5×10-4 mol/L with a detection limit of 8.5×10-7 mol/L. A mean recovery of 102.7% of CL in the pig liver sample solution and a reproducibility of 3.2% were obtained.

  1. Molecular distributions and geochemical implications of pyrrolic nitrogen compounds in the Permian Phosphoria Formation derived oils of Wyoming

    Silliman, J.E.; Li, M.; Yao, H. [Geological Survey of Canada, Calgary, Alberta (Canada); Hwang, R. [Chevron Petroluem Technology Company, Richmond, CA (United States)

    2002-05-01

    Crude oils from the Laramide structures of Wyoming were studied with respect to their geochemical compositions. The sampling areas include the Greater Green River, Wind River and Big Horn basins, and the Casper Arch region. Based on pristane/phytane ratio and various hopane and sterane parameters, the Permian Phosphoria Formation derived oils can be readily differentiated from oils with different origins. Within the Phosphoria Formation derived oils, three subgroups can be identified using T{sub s}/(T{sub s} + T{sub m}) and diasterane/regular sterane ratios, corresponding to sources with subtle variation in organic facies and/or thermal maturity of the Phosphoria Formation. Differences in source organic input, depositional environments, and thermal maturity were observed to greatly influence the saturated hydrocarbon compositions of the Permian Phosphoria Formation derived oils. However, the distributions of pyrrolic nitrogen compounds in these oils do not appear as diagnostic as the conventional hydrocarbon parameters commonly used as indicators of these geological factors. This fact may be related to the more significant role of oil migration in the modification of pyrrolic nitrogen compound distributions in foreland basins as compared to that in rift basins. The recognition of possible source and maturity effects on pyrrolic nitrogen compounds suggests that all of these factors should be taken into proper consideration before the pyrrolic nitrogen compounds are used as indicators for any specific geological process. (Author)

  2. One electron vs. two electron electrochemical and chemical oxidation of electron-donor substituted diketo-pyrrolo-pyrroles

    Luňák jr., S.; Eliáš, Z.; Mikysek, T.; Vyňuchal, J.; Ludvík, Jiří

    2013-01-01

    Roč. 106, SEP 2013 (2013), s. 351-359. ISSN 0013-4686 Grant ostatní: GA ČR(CZ) CZ.1.07/2.3.00/30.0021 Institutional support: RVO:61388955 Keywords : Diketo-pyrrolo-pyrroles * electrochemistry * Absorption spectra Subject RIV: CG - Electrochemistry Impact factor: 4.086, year: 2013

  3. Synthesis of conducting copolymers of thiophene capped poly(ethylene oxide) with pyrrole and thiophene

    Thiophene capped poly(ethylene oxide) (PEO) was synthesized. Copolymerisations of PEO with pyrrole (Py) and thiophene (Th) were achieved in water-sodium dodecyl sulfate (SDS) and acetonitrile (AN)-tetrabutylammonium tetrafluoroborate (TBAFB) solvent electrolyte couples via constant potential electrolyses. Characterisations of the samples were performed by NMR, cyclic voltammetry (CV), FT-IR, scanning electron microscopy (SEM). Electrical conductivities were measured by the four-probe technique. PEO-co-PTh film which was synthesized on ITO-glass in boron fluoride-ethyl ether (BFEE) found to exhibit electrochromic behaviour and it electrochemically switches between blue oxidized and red reduced states. Optical analyses were carried out to investigate the electronic structure of PEO-co-PTh electrochromic copolymer

  4. Emission and absorption of light in poly pyrrole synthesized by plasma

    The poly pyrrole structure (PPy) consists of heterocyclic rings with conjugation that it depends on the intensity of the electric field applied during the synthesis, and its luminescence is related with the π-π* transitions of that conjugation. To irradiate with light of different wavelengths, the results indicate that the polymer absorbs in the interval from 290 to 700 nm and it emits between 450 and 470 nm. The basal conductivity of the polymers, without electromagnetic excitation, it was measured in 10-15 S/cm, however, to interact with visible light it is increased approximately 10 times and when excite with UV light it is increased up to 3 magnitude orders. (Author)

  5. Supramolecular biosensors based on electropolymerised pyrrole-cyclodextrin modified surfaces for antibody detection.

    Wajs, Ewelina; Fernández, Núria; Fragoso, Alex

    2016-06-01

    The self-assembly of an adamantane-appended polymer bearing an antigen fragment on a polypyrrole-cyclodextrin modified surface provides a highly sensitive immunosensor with low limits of detection for celiac disease related targets. The pyrrole-carboxylic acid films were formed on the surface of gold electrodes by electropolymerisation and followed by covalent attachment of cyclodextrin units. Surface plasmon resonance measurements confirmed the role of the host/guest interactions between adamantane moieties and β-cyclodextrin hosts in the formation of the supramolecular sensor interface. Furthermore, this novel electrochemical supramolecular platform was effective in the amperometric detection of anti-gliadin antibodies in spiked serum samples with very good signal recovery. PMID:27097527

  6. ELECTRICALLY CONDUCTIVE COMPOSITE PREPARED BY ELECTROCHEMICAL POLYMERIZATION OF PYRROLE IN POLY- (p- PHENYLENE TEREPHTHALAMIDE ) MATRIX

    BI Xiantong; PEI Qibing; HAN Baozhen; BAO Jingshen

    1991-01-01

    The preparation of PPy/PPTA conductive composite films by electrochemical method is presented.The first step is to cast a thin layer of poly (p-phenylene-terephthalamide)(PPTA)on a slice of Pt working electrode. The second step is to electrochemically polymerize pyrrole on the PPTA/Pt working electrode. Both of the electrical conductivity and the mechanical properties of the PPy/PPTA composite film are better than those of the pure PPy film, and the film has excellent flexibility at low temperature, even in liquid nitrogen.The SEM picture of the cross-section of PPy/PPTA composite film showed that the two components were well mixed.Cyclic voltammograms of PPy/PPTA film in aqueous solution showed that the conductive films could be reduced and reoxidized.

  7. Outer-Sphere Mechanism in the Oxidation of Pyrrole-2- Carboxaldehyde by Hexacyanoferrate (III Complex.

    Abd-Alhakeem H. Abu-Nawwas

    2014-01-01

    Full Text Available The kinetics and mechanism of base-catalyzed oxidation of pyrrole-2-carboxaldehyde with hexacyanoferrate (III is reported. The reaction showed first order with respect to aldahyde , alkali and hexaeyanoferrate(III. The kinetic data suggest that the oxidation involves the formation of an anion of the substrate undergoes oxidation with hexaeyanoferrate(III via outer sphere mechanism process. The free radical thus produced is further oxidized to form the final products. A suitable mechanism was proposed and rate law was derived as − d[Fe CN 6 ] 3− = 2k1k2 RC(OH2 [Fe CN 6 ] 3−[OH−] k−1 H2O

  8. Crystal structure of 1-benzyl-4-formyl-1H-pyrrole-3-carb-oxamide.

    Zhong, Qi-Di; Hu, Sheng-Quan; Yan, Hong

    2016-02-01

    In the title compound, C13H12N2O2 (I), the mean planes of the pyrrole and benzyl rings are approximately perpendicular, forming a dihedral angle of 87.07 (4) °. There is an intra-molecular N-H⋯O hydrogen bond forming an S(7) ring motif. In the crystal, mol-ecules are linked via a pair of N-H⋯O hydrogen bonds forming inversion dimers. C-H⋯O hydrogen bonds link the dimers into chains along direction [10-1]. The chains are further linked by weak C-H⋯π inter-actions forming layers parallel to the ac plane. PMID:26958371

  9. Tumor Repression of VCaP Xenografts by a Pyrrole-Imidazole Polyamide.

    Amanda E Hargrove

    Full Text Available Pyrrole-imidazole (Py-Im polyamides are high affinity DNA-binding small molecules that can inhibit protein-DNA interactions. In VCaP cells, a human prostate cancer cell line overexpressing both AR and the TMPRSS2-ERG gene fusion, an androgen response element (ARE-targeted Py-Im polyamide significantly downregulates AR driven gene expression. Polyamide exposure to VCaP cells reduced proliferation without causing DNA damage. Py-Im polyamide treatment also reduced tumor growth in a VCaP mouse xenograft model. In addition to the effects on AR regulated transcription, RNA-seq analysis revealed inhibition of topoisomerase-DNA binding as a potential mechanism that contributes to the antitumor effects of polyamides in cell culture and in xenografts. These studies support the therapeutic potential of Py-Im polyamides to target multiple aspects of transcriptional regulation in prostate cancers without genotoxic stress.

  10. Depopulation of Single-Phthalocyanine Molecular Orbitals upon Pyrrolic-Hydrogen Abstraction on Graphene.

    Néel, Nicolas; Lattelais, Marie; Bocquet, Marie-Laure; Kröger, Jörg

    2016-02-23

    Single-molecule chemistry with a scanning tunneling microscope has preponderantly been performed on metal surfaces. The molecule-metal hybridization, however, is often detrimental to genuine molecular properties and obscures their changes upon chemical reactions. We used graphene on Ir(111) to reduce the coupling between Ir(111) and adsorbed phthalocyanine molecules. By local electron injection from the tip of a scanning tunneling microscope the two pyrrolic H atoms were removed from single phthalocyanines. The detachment of the H atom pair induced a strong modification of the molecular electronic structure, albeit with no change in the adsorption geometry. Spectra and maps of the differential conductance combined with density functional calculations unveiled the entire depopulation of the highest occupied molecular orbital upon H abstraction. Occupied π states of intact molecules are proposed to be emptied via intramolecular electron transfer to dangling σ states of H-free N atoms. PMID:26812093

  11. Theoretical and Experimental Study of Proton Transfer Reaction Dynamics in Pyrrole 2-Caboxyldehyde

    Chowdhury, Papia; Pathak, Anirban

    2009-01-01

    Photophysical and photochemical dynamics of ground state and excited state proton transfer reaction is reported for Pyrrole 2-Caboxyldehyde (PCL). Steady state absorption and emission measurements are conducted in this five member heterocyclic system (PCL). The theoretical investigation is done by using different quantum mechanical methods (e.g. Hartree Fock, DFT, MP2, CCSD etc.). The reaction pathway and two dimensional potential energy surfaces are computed in various level of theory. A transition state is also reported in gas phase and reaction filed calculation. It is established that PCL forms different emitting species in different media. A large Stokes shifted emission band, which is attributed to species undergoing excited state intramolecular proton transfer, is observed in hydrocarbon solvent. Intermolecular proton transfer is observed in hydroxylic polar solvent. Experimental observations yield all possible signatures of intramolecular and intermolecular proton transfer in excited state of PCL. The...

  12. Gamma irradiation effect on polymers derived of pyrrole synthesized by plasma

    This work studies the effect of gamma irradiation at doses of 50, 100, 200, 400 and 800 kGy on polymers obtained from pyrrole synthesized by plasma. The evolution of the structure was studied by Fourier transform infrared spectroscopy (Ftir) and X-ray photoelectron spectroscopy (XPS). The Ftir spectra show that poly pyrroles have N-H, C-H, C=O, triple and consecutive double bonds in their structure. The irradiated polymers show the same chemical groups in their structure without significant changes. Nevertheless, a more detailed analysis by XPS allows the identification of superficial chemical states, such as: C=CH-C, C=CC-C, C-NH-C, C-NC-C, etc., and shows that most of these states are present in all polymers but with different participation. One possible mechanism indicates that as the irradiation dose increases, dehydrogenation processes are performed increasing fragmentation, crosslinking and formation of multiple bonds. The fragmentation and thermal degradation were studied by thermogravimetric analysis, indicating that the loss of moisture and light compounds formed during gamma irradiation occurs in the firsts 100 grades C. The main degradation of all polymers occurs from 150 to 700 grades C, suggesting that the thermal stability is independent of the irradiation dose in the interval studied. Morphology was studied using scanning electron microscopy techniques. Before irradiation, the polymer presented a uniform and practically smooth surface, however, after gamma irradiation, the applied energy increased roughness and macro fragmentation. The roughness and functional groups on the surface reduced the contact angle with water as the irradiation dose increased. However, the polymers are hydrophilic, because for all doses that contact angle is smaller than 90 grades C. Electrical conductivity was calculated respect to temperature in the interval from 25 to 100 grades C. Conductivity increases with temperature and is slightly greater in the irradiated polymers

  13. Optoelectrochemical properties of the copolymer of 2,5-di(4-methylthiophen-2-yl)-1-(4-nitrophenyl)-1H-pyrrole monomer with 3,4-ethylenedioxythiophene

    Ak, Metin [Department of Chemistry, Middle East Technical University, 06531, Ankara (Turkey); Department of Chemistry, Faculty of Art and Sciences, Pamukkale University, 20017 Denizli (Turkey)], E-mail: metinak@pau.edu.tr; Tanyeli, Cihangir [Department of Chemistry, Middle East Technical University, 06531, Ankara (Turkey)], E-mail: tanyeli@metu.edu.tr; Akhmedov, Idris M. [Department of Chemistry, Middle East Technical University, 06531, Ankara (Turkey)], E-mail: idrism@chem.metu.edu.tr; Toppare, Levent [Department of Chemistry, Middle East Technical University, 06531, Ankara (Turkey)], E-mail: toppare@metu.edu.tr

    2008-04-30

    Copolymer of 2,5-di(4-methylthiophen-2-yl)-1-(4-nitrophenyl)-1H-pyrrole (MTNP) with 3,4-ethylene dioxythiophene (EDOT) was electrochemically synthesized and characterized via cyclic voltammetry, Fourier Transform Infrared spectroscopy, Scanning Electron Microscopy, conductivity measurements. Spectroelectrochemical investigations showed that resulting copolymer film has distinct electrochromic properties. It has five different colors (dark purple, red, light grey, green, blue). At the neutral state {lambda}{sub max} due to the {pi}-{pi}* transition was found to be 500 nm and E{sub g} was calculated as 1.71 eV. Double potential step chronoamperometry experiment shows that copolymer film has good stability, fast switching time (1.1 s) and high optical contrast (30%). Electrochromic device based on P(MTNP-co-EDOT) and PEDOT was constructed and characterized. Oxidized state of the device shows dark purple color with a blue color reduced state. At interval potentials device has good transparency and colors of the device are yellow and grey. Maximum contrast and switching time of the device were measured as 23% and 1.1 s at 650 nm.

  14. Optoelectrochemical properties of the copolymer of 2,5-di(4-methylthiophen-2-yl)-1-(4-nitrophenyl)-1H-pyrrole monomer with 3,4-ethylenedioxythiophene

    Copolymer of 2,5-di(4-methylthiophen-2-yl)-1-(4-nitrophenyl)-1H-pyrrole (MTNP) with 3,4-ethylene dioxythiophene (EDOT) was electrochemically synthesized and characterized via cyclic voltammetry, Fourier Transform Infrared spectroscopy, Scanning Electron Microscopy, conductivity measurements. Spectroelectrochemical investigations showed that resulting copolymer film has distinct electrochromic properties. It has five different colors (dark purple, red, light grey, green, blue). At the neutral state λmax due to the π-π* transition was found to be 500 nm and Eg was calculated as 1.71 eV. Double potential step chronoamperometry experiment shows that copolymer film has good stability, fast switching time (1.1 s) and high optical contrast (30%). Electrochromic device based on P(MTNP-co-EDOT) and PEDOT was constructed and characterized. Oxidized state of the device shows dark purple color with a blue color reduced state. At interval potentials device has good transparency and colors of the device are yellow and grey. Maximum contrast and switching time of the device were measured as 23% and 1.1 s at 650 nm

  15. Catalytic formal [2+2+1] synthesis of pyrroles from alkynes and diazenes via TiII/TiIV redox catalysis

    Gilbert, Zachary W.; Hue, Ryan J.; Tonks, Ian A.

    2016-01-01

    Pyrroles are structurally important heterocycles. However, the synthesis of polysubstituted pyrroles is often challenging. Here, we report a multicomponent, Ti-catalysed formal [2+2+1] reaction of alkynes and diazenes for the oxidative synthesis of penta- and trisubstituted pyrroles: a nitrenoid analogue to classical Pauson-Khand-type syntheses of cyclopentenones. Given the scarcity of early transition-metal redox catalysis, preliminary mechanistic studies are presented. Initial stoichiometric and kinetic studies indicate that the mechanism of this reaction proceeds through a formally TiII/TiIV redox catalytic cycle, in which an azatitanacyclobutene intermediate, resulting from [2+2] alkyne + Ti imido coupling, undergoes a second alkyne insertion followed by reductive elimination to yield pyrrole and a TiII species. The key component for catalytic turnover is the reoxidation of the TiII species to a TiIV imido via the disproportionation of an η2-diazene-TiII complex.

  16. Zur Reaktion von Pyroglutaminsäure-Derivaten mit Phosphorpentachlorid - Darstellung chlorierter Pyrrol-2-carbonsäure-Derivate (Aminosäuren ; 9)

    Effenberger, Franz; Müller, Wolfgang; Isak, Heinz

    1987-01-01

    N-Benzyl-5-oxoprolinester 5 werden mit PCl5 über verschiedene chlorierte Zwischenstufen zu N-Benzyl-4,5-dichlor-1H-pyrrol-2-carbonsäureestern 6 chloriert, während N-Benzhydryl- L-3 und N-Acyl-5-oxoprolinester L-4 mit PCl5 unter Abspaltung des N-Substituenten L-4,4,5-Trichlor-3,4-dihydro-2H-pyrrol-2-carbon-säureester 18 bilden, die mit Base in die 4,5-Dichlor-1H-pyrrol-2-carbonsäureester 20 übergehen. Diese Umsetzungen stellen die beste Methode zur Herstellung von 4,5-Dichlor-1H-pyrrol-2-carbo...

  17. Ruthenium(II)-catalyzed synthesis of pyrrole- and indole-fused isocoumarins by C-H bond activation in DMF and water

    Singh, K.S.; Sawant, S.G.; Dixneuf, P.H.

    isocoumarin derivatives. These catalytic reactions can be performed in DMF and competively in water. COMMUNICATION Keisham S. Singh*,Sneha G. Sawant, Pierre H. Dixneuf * Page No. – Page No. Ruthenium(II) catalysed synthesis of pyrrole...

  18. Organocatalytic asymmetric Henry reaction of 1H-pyrrole-2,3-diones with bifunctional amine-thiourea catalysts bearing multiple hydrogen-bond donors.

    Zhang, Ming-Liang; Yue, Deng-Feng; Wang, Zhen-Hua; Luo, Yuan; Xu, Xiao-Ying; Zhang, Xiao-Mei; Yuan, Wei-Cheng

    2016-01-01

    For the first time, a catalytic asymmetric Henry reaction of 1H-pyrrole-2,3-diones was achieved with a chiral bifunctional amine-thiourea as a catalyst possessing multiple hydrogen-bond donors. With this developed method, a range of 3-hydroxy-3-nitromethyl-1H-pyrrol-2(3H)-ones bearing quaternary stereocenters were obtained in acceptable yield (up to 75%) and enantioselectivity (up to 73% ee). PMID:26977188

  19. Strikingly different luminescent properties arising from single crystals grown from solution or from the vapor phase in a diketo-pyrrolo-pyrrole analog

    Imoda, Tomohiko; Mizuguchi, Jin

    2007-01-01

    The title compound di-cyano-pyrrolo-pyrrole (DCPP) is an analog of diketo-pyrrolo-pyrrole (DPP) known as a red pigment on the market. Brilliant orange photoluminescence has been observed in crystals of DCPP recrystallized from solution (crystal I); whereas the luminescence was quite weak in single crystals grown from the vapor phase (crystal II). To elucidate the difference in luminescent properties, a series of structural analysis together with thermal analysis has been carried out on crysta...

  20. CHANGES OF STRUCTURE AND PROPERTIES OF POLY (ETHYLENE TEREPHTHALATE)CAUSED BY IN-SITU POLYMERIZATION OF PYRROLE

    HE Jiasong; FENG Zhihai

    1991-01-01

    Conductive polymer composites based on crystalline polymer matrix have been prepared by using an in-situ polymerization process of pyrrole in amorphous poly (ethylene terephthalate) (PET) film.The DSC and WAXD measurement and SEM observation show that liquid-induced crystallization of PET matrix has occurred during the preparation of composite films. Depending upon the equilibrium degree of swelling and crystallinity, the limited depth of penetration of pyrrole molecules results in a skin-core structure of the composite film. The skin layer containing charge transfer intercalated polypyrrole has a surface resistance of 3.5 × 104 Ω. Rigid and heat-resistant polypyrrole molecules formed in PET film increase the tensile modulus and, especially, the rigidity of PET at elevated temperatures. However, they decrease the tensile strength and elongation at break, and impair the thermal ductility of PET.

  1. Highly enantioselective synthesis of beta-heteroaryl-substituted dihydrochalcones through Friedel-Crafts alkylation of indoles and pyrrole.

    Wang, Wentao; Liu, Xiaohua; Cao, Weidi; Wang, Jun; Lin, Lili; Feng, Xiaoming

    2010-02-01

    A highly enantioselective Friedel-Crafts (F-C) alkylation of indoles and pyrrole with chalcone derivatives catalyzed by a chiral N,N'-dioxide-Sc(OTf)(3) complex has been developed that tolerates a wide range of substrates. The reaction proceeds in moderate to excellent yields and high enantioselectivities (85-92 % enantiomeric excess) using 2 mol % (for indole) or 0.5 mol % (for pyrrole) catalyst loading, which showed the potential value of the catalyst system. Meanwhile, a strong positive nonlinear effect was observed. On the basis of the experimental results and previous reports, a possible working model is proposed to explain the origin of the activation and asymmetric induction. PMID:20013964

  2. Green Synthesis of Ag and Pd Nanospheres, Nanowires, and Nanorods Using Vitamin B2: Catalytic Polymerisation of Aniline and Pyrrole

    Mallikarjuna N. Nadagouda

    2008-01-01

    Full Text Available For the first time, we report green chemistry approach using vitamin B2 in the synthesis of silver (Ag and palladium (Pd, nanospheres, nanowires, and nanorods at room temperature without using any harmful reducing agents, such as sodium borohydride (NaBH4 or hydroxylamine hydrochloride and any special capping or dispersing agent. Vitamin B2 was used as reducing agent as well as capping agent due to its high-water solubility, biodegradability, and low-toxicity compared with other reducing agents. The average particle size of nanoprticle was found to be Ag (average size 6.1±0.1 nm and Pd (average size 4.1±0.1 nm nanoparticles in ethylene glycol and Ag (average size 5.9±0.1 nm, and average size 6.1±0.1 nanoparticles in acetic acid and NMP, respectively. The formation of noble multiple shape nanostructures and their self assembly were dependent on the solvent employed for the preparation. When water was used as solvent media, Ag and Pd nanoparticles started to self-assemble into rod-like structures and in isopropanol Ag and Pd nanoparticles yielded wire-like structures with a thickness in the range of 10 to 20 nm and several hundred microns in length. In acetone and acetonitrile medium, the Ag and Pd nanoparticles are self-assembled into a regular pattern making nanorod structures with thicknesses ranging from 100 to 200 nm and lengths of a few microns. The so-synthesized nanostructures were characterized using scanning electron microscopy (SEM, transmission electron microscopy (TEM, energy dispersive X-ray (EDX analysis, and UV spectroscopy. The ensuing Ag and Pd nanoparticles catalyzed the reactions of aniline and pyrrole to generate polyaniline and polypyrrole nanofibers and may find various technological and biological applications. This single-step greener approach is general and can be extended to other noble metals and transition metal oxides.

  3. Copper-Catalyzed Coupling of 2-Siloxy-1-alkenes and Diazocarbonyl Compounds: Approach to Multisubstituted Furans, Pyrroles, and Thiophenes.

    Tan, Wei Wen; Yoshikai, Naohiko

    2016-07-01

    We report herein copper(II)-catalyzed cyclization reactions of silyl enol ethers derived from methyl ketones with α-diazo-β-ketoesters or α-diazoketones to afford 2-siloxy-2,3-dihydrofuran derivatives or 2,3,5-trisubstituted furans, respectively, under mild conditions. The former cyclization products serve as versatile 1,4-diketone surrogates, allowing facile preparation of 2,3,5-trisubstituted furans, pyrroles, and thiophenes. PMID:27259097

  4. Direct detection of pyridine formation by the reaction of CH (CD) with pyrrole: a ring expansion reaction

    Soorkia, Satchin; Taatjes, Craig A.; Osborn, David L.; Selby, Talitha M.; Trevitt, Adam J.; Wilson, Kevin R.; Leone, Stephen R.

    2010-03-16

    The reaction of the ground state methylidyne radical CH (X2Pi) with pyrrole (C4H5N) has been studied in a slow flow tube reactor using Multiplexed Photoionization Mass Spectrometry coupled to quasi-continuous tunable VUV synchrotron radiation at room temperature (295 K) and 90 oC (363 K), at 4 Torr (533 Pa). Laser photolysis of bromoform (CHBr3) at 248 nm (KrF excimer laser) is used to produce CH radicals that are free to react with pyrrole molecules in the gaseous mixture. A signal at m/z = 79 (C5H5N) is identified as the product of the reaction and resolved from 79Br atoms, and the result is consistent with CH addition to pyrrole followed by Helimination. The Photoionization Efficiency curve unambiguously identifies m/z = 79 as pyridine. With deuterated methylidyne radicals (CD), the product mass peak is shifted by +1 mass unit, consistent with the formation of C5H4DN and identified as deuterated pyridine (dpyridine). Within detection limits, there is no evidence that the addition intermediate complex undergoes hydrogen scrambling. The results are consistent with a reaction mechanism that proceeds via the direct CH (CD) cycloaddition or insertion into the five-member pyrrole ring, giving rise to ring expansion, followed by H atom elimination from the nitrogen atom in the intermediate to form the resonance stabilized pyridine (d-pyridine) molecule. Implications to interstellar chemistry and planetary atmospheres, in particular Titan, as well as in gas-phase combustion processes, are discussed.

  5. N-Heterocyclic carbene–palladium catalysts for the direct arylation of pyrrole derivatives with aryl chlorides

    Ismail Özdemir

    2013-02-01

    Full Text Available New Pd–NHC complexes have been synthesized and employed for palladium-catalyzed direct arylation of pyrrole derivatives by using electron-deficient aryl chlorides as coupling partners. The desired coupling products were obtained in moderate to good yields by using 1 mol % of these air-stable palladium complexes. This is an advantage compared to the procedures employing air-sensitive phosphines, which have been previously shown to promote the coupling of aryl chlorides with heteroarenes.

  6. Pyrrole PMOs, incorporating new N-heterocyclic compounds on an ethene-PMO through Diels–Alder reactions

    Esquivel, Dolores; De Canck, Els [Center for Ordered Materials, Organometallics and Catalysis, Department of Inorganic and Physical Chemistry, Ghent University, Krijgslaan 281-S3, 9000 Ghent (Belgium); Jiménez-Sanchidrián, César [Department of Organic Chemistry, Nanochemistry and Fine Chemistry Research Institute (IUIQFN), Faculty of Sciences, University of Córdoba, Campus de Rabanales, Marie Curie Building, Ctra. Nnal. IV, km 396, 14071 Córdoba (Spain); Romero-Salguero, Francisco J., E-mail: qo2rosaf@uco.es [Department of Organic Chemistry, Nanochemistry and Fine Chemistry Research Institute (IUIQFN), Faculty of Sciences, University of Córdoba, Campus de Rabanales, Marie Curie Building, Ctra. Nnal. IV, km 396, 14071 Córdoba (Spain); Van Der Voort, Pascal, E-mail: pascal.vandervoort@ugent.be [Center for Ordered Materials, Organometallics and Catalysis, Department of Inorganic and Physical Chemistry, Ghent University, Krijgslaan 281-S3, 9000 Ghent (Belgium)

    2014-11-14

    The ethenylene bridges on the walls of an ethenylene-bridged periodic mesoporous organosilica were successfully modified with a variety of pyrrole derivatives – pyrrole, methylpyrrole, dimethylpyrrole, trimethylpyrrole and 1-phenylpyrrole – through Diels–Alder reactions. X-ray diffraction measurements and N{sub 2} adsorption–desorption analysis confirmed the preservation of the ordering and mesoporosity of the parent material as well as the decoration of the pores with the surface Diels–Alder adducts. Moreover, other techniques such as DRIFT, {sup 13}C and {sup 29}Si nuclear magnetic resonances revealed the formation of the surface N-heterocyclic compounds at the parent ethenylene sites. - Highlights: • Chemical modification of the double bonds on an ethene-PMO through the Diels–Alder reaction. • A family of pyrrole derivatives act as dienes in the Diels–Alder reaction. • Well-ordering and mesoporosity are retained after the post-functionalization. • N-containing compounds on the surface of ethene-PMO are present after the Diels–Alder reaction.

  7. Theoretical and experimental studies on the electronic, optical, and structural properties of poly-pyrrole-2-carboxylic acid films

    Highlights: • Novel approach for preparing a functionalized polypyrrole film. • Comparative experimental and theoretical results – conjugated polymers. • Accurate electronic, structural, and optical properties obtained for poly-pyrrole-2-carboxylic acid films. • Proposal of mechanism of electropolymerization of pyrrole-2-carboxylic acid films. - Abstract: A theoretical approach is used here to explain experimental results obtained from the electrosynthesis of polypyrrole-2-carboxylic acid (PPY-2-COOH) films in nonaqueous medium. An analysis of the Fukui function (reactivity index) indicates that the monomer (pyrrole-2-carboxylic acid, PY-2-COOH), and dimers and trimers are oxidized in the C4 or C5 positions of the heterocyclic ring of the PY-2-COOH structure. After calculating the heat of formation using semiempirical Austin Model 1 post-Hartree–Fock parameterization for dimer species, both C4 and C5 positions adjacent to the aromatic rings of PPY-2-COOH were considered the most susceptible ones to oxidative coupling reactions. The ZINDO-S/CI semiempirical method was used to simulate the electronic transitions typically seen in the UV–VIS–NIR range in monomer and oligomers with different conjugation lengths. The use of an electrochemical quartz crystal microbalance provides sufficient information to propose a polymerization mechanism of PY-2-COOH based on molecular modeling and experimental results

  8. Pyrrole PMOs, incorporating new N-heterocyclic compounds on an ethene-PMO through Diels–Alder reactions

    The ethenylene bridges on the walls of an ethenylene-bridged periodic mesoporous organosilica were successfully modified with a variety of pyrrole derivatives – pyrrole, methylpyrrole, dimethylpyrrole, trimethylpyrrole and 1-phenylpyrrole – through Diels–Alder reactions. X-ray diffraction measurements and N2 adsorption–desorption analysis confirmed the preservation of the ordering and mesoporosity of the parent material as well as the decoration of the pores with the surface Diels–Alder adducts. Moreover, other techniques such as DRIFT, 13C and 29Si nuclear magnetic resonances revealed the formation of the surface N-heterocyclic compounds at the parent ethenylene sites. - Highlights: • Chemical modification of the double bonds on an ethene-PMO through the Diels–Alder reaction. • A family of pyrrole derivatives act as dienes in the Diels–Alder reaction. • Well-ordering and mesoporosity are retained after the post-functionalization. • N-containing compounds on the surface of ethene-PMO are present after the Diels–Alder reaction

  9. Investigations of poly(pyrrole)-coated cotton fabrics prepared in blends of anionic and cationic surfactants as flexible electrode

    Highlights: • Poly(pyrrole)-coated cotton fabrics were prepared in mixed surfactants. • The fabrics are soft, lightweight, mechanically robust, and highly electrical conductive. • Potential applications of the fabrics as flexible electrodes were tested. • The fabric electrodes exhibited high discharge capacity and excellent cycling performance. -- Abstract: In recent years, much effort has been dedicated to achieve lightweight, stretchable and flexible energy-storage devices for wearable electronics. Here we report an everyday cotton fabric coated with poly(pyrrole) as flexible electrodes. Poly(pyrrole) nanoparticles are synthesized on the fabrics via a simple chemical polymerization process with the mixed surfactants of cetyltrimethylammonium bromide (CTAB) and sodium dodecyl benzene sulfonate (SDBS) as soft template. A highly conductive fabric with surface resistance of 14 Ω/□ can be produced by changing surfactant concentration. Such a conductive textile shows outstanding flexibility and stretchability, and demonstrates strong adhesion between the PPy and the cellulose fiber. The fabric electrode exhibits a discharge capacity of 51.7 mAh g−1 with high cycling stability (negligible decay after 100 cycles)

  10. Vibrational spectra and electronic structure of 3-((1H-pyrrol-1-yl) methyl) naphthalen-2-ol - A computational insight on antioxidant active Mannich base

    Boobalan, Maria susai; Tamilvendan, D.; Amaladasan, M.; Ramalingam, S.; Venkatesa Prabhu, G.; Bououdina, M.

    2015-02-01

    The 3-((1H-pyrrol-1-yl) methyl) naphthalen-2-ol (IFTN) is a class of synthesized organic Mannich base compound having antioxidant property of biological importance. A meticulous normal mode vibrational analysis has been carried out by comparing and contrasting the experimentally recorded FT-IR and FT-Raman spectra with simulated spectra of IFTN. Similarly the calculated 1H and 13C NMR of IFTN were correlated with experimental findings to understand the shielding and deshielding nature hold in it. The following other electronic structure properties were calculated such as equilibrium geometrical parameters, natural bond orbital analysis (NBO), frontier molecular orbital (FMO) characterization, statistical thermochemical properties against a range of temperatures and molecular electrostatic potential (MEP) imprint was carried out along with various charges such as APT, ESP, Hirshfeld, natural and Mulliken. All these predicted properties unlock the nature of total behavior of IFTN in various dimensions. These could be Lewis, non-Lewis interaction along with their respective energies, contribution of fragmented moieties for various orders of HOMO and LUMO, temperature consequences on enthalpy, entropy, and heat capacity. In addition, the MEP leads to find electrophilic, nucleophilic reactive sites on IFTN molecular surface. The entire computational calculations has been made on HF/6-31+G/6-311++G(d,p) and B3LYP/6-31+G/6-311++G(d,p) model chemistries. A complete electronic structure observation has been achieved by this theoretical analysis.

  11. Synthesis, molecular structure and spectral analysis of ethyl 4-formyl-3,5-dimethyl-1H-pyrrole-2-carboxylate thiosemicarbazone: A combined DFT and AIM approach

    Singh, R. N.; Kumar, Amit; Tiwari, R. K.; Rawat, Poonam; Verma, Divya; Baboo, Vikas

    2012-05-01

    A new ethyl 4-formyl-3,5-dimethyl-1H-pyrrole-2-carboxylate thiosemicarbazone (EFDMPCT) has been synthesized and characterized by elemental analysis and FT-IR, 1H NMR, UV-Visible, DART-mass spectroscopy. Quantum chemical calculations have been performed by DFT level of theory using B3LYP functional and 6-31G (d,p) as basis set. The calculated 1H NMR chemical shifts using gauge including atomic orbitals (GIAO) approach are in good agreement with the observed chemical shifts. The electronic transitions within molecule have been interpreted using the time dependent density functional theory (TD-DFT). The calculated and experimental wavenumbers analyses confirm the existence of dimer. Topological parameters electron density, Laplacian of electron density, kinetic electron energy density, potential electron density and the total electron energy density at the bond critical points (BCP) analyzed using 'Atoms in Molecules' AIM theory reveals intra and inter molecular hydrogen bonding other weaker interactions in detail. The calculated intermolecular hydrogen bond energy of dimer is -12.2176 kcal/mol using AIM calculation. The results of AIM ellipticity confirm the existence of resonance assisted hydrogen bonds in dimer. The calculated thermodynamic parameters show that reaction is exothermic and non-spontaneous at room temperature. The local reactivity descriptors find the reactive sites within molecules have been calculated.

  12. Electrochromic properties of poly (1-(phenyl)-2,5-di(2-thienyl)-1H-pyrrole-co-3,4-ethylenedioxy thiophene) and its application in electrochromic devices

    Tarkuc, S.; Sahmetlioglu, E.; Tanyeli, C.; Akhmedov, I. M.; Toppare, L.

    2008-06-01

    Electrochemical copolymerization of 1-(phenyl)-2,5-di(2-thienyl)-1H-pyrrole (PTP) with 3,4-ethylenedioxy thiophene (EDOT) was carried out in acetonitrile (AN)/NaClO4/LiClO4 (0.1 M) solvent-electrolyte couple via potentiodynamic electrolysis. Characterizations of the resulting copolymer were performed via cyclic voltammetry (CV), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and spectroelectrochemical analysis. Spectroelectrochemical analyses show that the copolymer of PTP with EDOT has an electronic band gap (due to π to π∗ transition) of 1.9 eV at 480 nm, with a claret red in the fully reduced form and a blue color in the fully oxidized form. Via kinetic studies, the optical contrast (ΔT %) was found to be 8% for P(PTP-co-EDOT). Results showed that the time required to reach 95% of the ultimate transmittance was 1.7 s for the copolymer. The P(PTP-co-EDOT) film was used to construct a dual type polymer electrochromic device (ECDs) with poly(3,4-ethylenedioxy thiophene) (PEDOT). Spectroelectrochemistry, electrochromic switching and open circuit memory of the device were investigated.

  13. A concise synthesis of (+)-batzelladine B from simple pyrrole-based starting materials

    Parr, Brendan T.; Economou, Christos; Herzon, Seth B.

    2015-09-01

    Alkaloids, secondary metabolites that contain basic nitrogen atoms, are some of the most well-known biologically active natural products in chemistry and medicine. Although efficient laboratory synthesis of alkaloids would enable the study and optimization of their biological properties, their preparation is often complicated by the basicity and nucleophilicity of nitrogen, its susceptibility to oxidation, and its ability to alter reaction outcomes in unexpected ways--for example, through stereochemical instability and neighbouring group participation. Efforts to address these issues have led to the invention of a large number of protecting groups that temper the reactivity of nitrogen; however, the use of protecting groups typically introduces additional steps and obstacles into the synthetic route. Alternatively, the use of aromatic nitrogen heterocycles as synthetic precursors can attenuate the reactivity of nitrogen and streamline synthetic strategies. Here we use such an approach to achieve a synthesis of the complex anti-HIV alkaloid (+)-batzelladine B in nine steps (longest linear sequence) from simple pyrrole-based starting materials. The route uses several key transformations that would be challenging or impossible to implement using saturated nitrogen heterocycles and highlights some of the advantages of beginning with aromatic reagents.

  14. Efficient Synthesis of Peptide and Protein Functionalized Pyrrole-Imidazole Polyamides Using Native Chemical Ligation

    Brian M. G. Janssen

    2015-06-01

    Full Text Available The advancement of DNA-based bionanotechnology requires efficient strategies to functionalize DNA nanostructures in a specific manner with other biomolecules, most importantly peptides and proteins. Common DNA-functionalization methods rely on laborious and covalent conjugation between DNA and proteins or peptides. Pyrrole-imidazole (Py–Im polyamides, based on natural minor groove DNA-binding small molecules, can bind to DNA in a sequence specific fashion. In this study, we explore the use of Py–Im polyamides for addressing proteins and peptides to DNA in a sequence specific and non-covalent manner. A generic synthetic approach based on native chemical ligation was established that allows efficient conjugation of both peptides and recombinant proteins to Py–Im polyamides. The effect of Py–Im polyamide conjugation on DNA binding was investigated by Surface Plasmon Resonance (SPR. Although the synthesis of different protein-Py–Im-polyamide conjugates was successful, attenuation of DNA affinity was observed, in particular for the protein-Py–Im-polyamide conjugates. The practical use of protein-Py–Im-polyamide conjugates for addressing DNA structures in an orthogonal but non-covalent manner, therefore, remains to be established.

  15. Experimental and computational thermochemistry of 1-phenylpyrrole and 1-(4-methylphenyl)pyrrole

    Santos, Ana Filipa L.O.M. [Centro de Investigacao em Quimica, Department of Chemistry, Faculty of Science, University of Porto, Rua do Campo Alegre, 687, P-4169-007 Porto (Portugal); Ribeiro da Silva, Manuel A.V., E-mail: risilva@fc.up.p [Centro de Investigacao em Quimica, Department of Chemistry, Faculty of Science, University of Porto, Rua do Campo Alegre, 687, P-4169-007 Porto (Portugal)

    2010-06-15

    The standard (p{sup o} = 0.1 MPa) molar enthalpies of formation, in the crystalline phase, of 1-phenylpyrrole and 1-(4-methylphenyl)pyrrole, at T = 298.15 K, were derived from the standard molar energies of combustion in oxygen, measured by static-bomb combustion calorimetry. For these compounds, the standard molar enthalpies of sublimation, at T = 298.15 K, were determined from the temperature-vapour pressure dependence, obtained by the Knudsen mass-loss effusion method. Using estimated values for the heat capacity differences between the gas and the crystal phases of the studied compounds, the standard (p{sup o} = 0.1 MPa) molar enthalpies, entropies, and Gibbs energies of sublimation, at T = 298.15 K, were derived. From the experimental values, the standard molar enthalpies of formation, in the gaseous phase, at T = 298.15 K, were calculated. Additionally, the enthalpies of formation of both compounds were estimated using the composite G3(MP2)//B3LYP approach together with adequate gas-phase working reactions. There is a very good agreement between computational and experimental results.

  16. Crystal structures of unsymmetrically mixed β-pyrrole substituted nickel(II)-meso-tetraphenylporphyrins

    BHYRAPPA PUTTAIAH; VELKANNAN VEERAPANDIAN; SARANGI UJWAL KUMAR

    2016-07-01

    Crystal structures of solvated unsymmetrically substituted meso-tetraphenylporphyrins, 2,3,12,13, 17-pentachloro-5,7,8,10,15,18,20-hepta-phenylporphyrin, H₂TPP(Ph)₃(Cl)₅, 1 and its nickel(II), NiTPP(Ph)₃(Cl)₅, 2 were determined by single crystal XRD analysis. In addition, a new unsymmetricallysubstituted porphyrin, 2,3,12,13,17-pentacyano-5,7,8,10,15,18,20-heptaphenyl-porphinato nickel(II) complex, NiTPP(Ph)₃(CN)₅, 3 complex was synthesized and its solvated structure was examined by crystallography. These porphyrins exhibited dramatic nonplanar conformation of the macrocycle as evidenced from the averagedisplacement of the β-pyrrole carbon (±ΔCβ ) from the mean plane of the porphyrin ring and the trend in nonplanarity varies in the order: 2 (1.189(5) Å) > 1 (1.036(6) Å) > 3 (0.895(6) Å). The normal-coordinate structural decomposition analysis of these structures revealed mainly saddle distortion of the macrocycle combined with small degree of ruffled or domed distortions. The Hirshfeld surface analysis of structures 1-3 revealed solvate dependent intermolecular contacts with varying degree of H. . .H (43–49%), C. . .H (17–19%), H. . .Cl (25–30%) and N. . .H (~19%) contact contributions.

  17. Palladium complexes of pyrrole-2-aldehyde thiosemicarbazone: Synthesis, structure and spectral properties

    Piyali Paul; Samaresh Bhattacharya

    2014-09-01

    Reaction of pyrrole-2-aldehyde thiosemicarbazone (abbreviated as H2L, where H2 stands for the two potentially dissociable protons) with [Pd(PPh3)2Cl2] in ethanol in the presence of NEt3 afforded two complexes, [Pd(PPh3)(HLNS)Cl] and [Pd(PPh3)(LNNS)], where the thiosemicarbazone ligand is coordinated to the metal centre respectively as monoanionic N,S-donor (depicted by HLNS) and dianionic N,N,S-donor (depicted by LNNS). Similar reaction with Na2[PdCl4] afforded a bis-complex, [Pd(HLNS)2]. Crystal structures of all the three complexes have been determined.With reference to the structure of the uncoordinated thiosemicarbazone (H2L), the N,S-coordinationmode observed in [Pd(PPh3)(HLNS)Cl] and [Pd(HLNS)2] is associated with a geometrical change around the imine bond.While the N,N,S-mode of binding observed in [Pd(PPh3)(LNNS)] takes place without any such geometrical change. All three complexes display intense absorptions in the visible and ultraviolet regions, which have been analyzed by TDDFT method.

  18. New 1H-pyrrole-2,5-dione derivatives as efficient organic inhibitors of carbon steel corrosion in hydrochloric acid medium: Electrochemical, XPS and DFT studies

    Highlights: • 1H-pyrrole derivatives act as good corrosion inhibitors for carbon steel in 1 M HCl. • Adsorption of the inhibitors on carbon steel surface obeys Langmuir’s isotherm. • XPS showed that the inhibitors are chemisorbed on the metal surface. • Quantum chemical parameters were correlated with experimental results. - Abstract: New 1H-pyrrole-2,5-dione derivatives, namely 1-phenyl-1H-pyrrole-2,5-dione (PPD) and 1-(4-methylphenyl)-1H-pyrrole-2,5-dione (MPPD) were synthesised and their inhibitive action against the corrosion of carbon steel in 1 M HCl solution were investigated at 308 K by weight loss, potentiodynamic polarization curves, and electrochemical impedance spectroscopy (EIS) methods. The results showed that the investigated 1H-pyrrole-2,5-dione derivatives are good corrosion inhibitors for carbon steel in 1 M HCl medium, their inhibition efficiency increased with inhibitor concentration, and MPPD is slightly more effective than PPD. Potentiostatic polarization study showed that PPD and MPPD are mixed-type inhibitors in 1 M HCl. Impedance experimental data revealed a frequency distribution of the capacitance, simulated as constant phase element. The results obtained from electrochemical and weight loss studies were in reasonable agreement. The adsorption of MPPD and PPD on steel surface obeyed Langmuir’s adsorption isotherm. Thermodynamic data and XPS analysis clearly indicated that the adsorption mechanism of 1H-pyrrole-2,5-dione derivatives on carbon steel surface in 1 M HCl solution is mainly controlled by a chemisorption process. Quantum chemical calculations using the Density Functional Theory (DFT) were performed on 1H-pyrrole-2,5-dione derivatives to determine the relationship between molecular structures and their inhibition efficiencies

  19. Nerve cells culture from lumbar spinal cord on surfaces modified by plasma pyrrole polymerization.

    Zuñiga-Aguilar, E; Olayo, R; Ramírez-Fernández, O; Morales, J; Godínez, R

    2014-01-01

    Currently, there are several techniques for modified cell culture surfaces under research to improve cell growth and adhesion. Recently, different methods have been used for surface coating, using biomolecules that enhance cell attachment and growth of nerve cells from spinal cord, such as the use of Poly-DL-Ornithine/Laminin. Plasma-polymerized pyrrole (PPy)-treated surfaces have showed improvement on surfaces biocompatibility with the cells in culture since they do not interfere with any of the biological cell functions. In the present work, we present a novel mouse nerve cell culture technique, using PPy-treated cell culture surfaces. A comparative study of cell survival using Poly-DL-Ornithine/Laminin-treated surfaces was performed. Our results of cell survival when compared with data already reported by other investigators, show that cells cultured on the PPy-modified surface increased survival up to 21 days when compared with Poly-DL-Ornithine/Laminin-coated culture, where 8 days cell survival was obtained. There were electrical and morphological differences in the nerve cells grown in the different surfaces. By comparing the peak ion currents of Poly-DL-Ornithine/Laminin-seeded cells for 8 days with cells grown for 21 days on PPy, an increase of 516% in the Na(+) current and 127% in K(+) currents in cells seeded on PPy were observed. Immunofluorescence techniques showed the presence of cell synapses and culture viability after 21 days. Our results then showed that PPy-modified surfaces are an alternative culture method that increases nerve cells survival from lumbar spinal cord cell culture by preserving its electrical and morphological features. PMID:24650203

  20. Morphological and physicochemical properties of dip-coated poly {(2,5-diyl pyrrole) [4-nitrobenzylidène]} (PPNB) thin films: towards photovoltaic applications

    Mouchaal, Younes; Gherrass, Hamou; Bendoukha Reguig, Abdelkarim; Hachemaoui, Aïcha; Yahiaoui, Ahmed; Makha, Mohamed; Khelil, Abdelbacet; Bernede, Jean-Christian

    2015-02-01

    A new material: conjugated poly {(2,5-diyl pyrrole) [4-nitrobenzylidène]}, that we called (PPNB), has been synthesized and characterized. The cyclic voltammetry has been used in order to estimate first oxidation (Ep) and reduction (En) potentials of our polymer. These values have been assigned, respectively, to the position of the highest occupied molecular orbital (HOMO) and the lowest unoccupied molecular orbital (LUMO) and determination of the energy band gap which have been estimated to be 6.16, 3.89 and 2.27 eV respectively. Energy levels values of the HOMO and LUMO of the PPNB polymeric donor material were evaluated and the results are compatible with an electron transfer to C60 within an eventual junction, such values show that PPNB could be probed for applications in organic solar cells as donor material. PPNB Thin films have been deposited by dip-coating technique from Dichloromethane solvent with different polymer concentrations, and a dipping speed of 3.0 cm/min. For morphological characterization of the films scanning electron microscopy (SEM) was carried out. The samples, when observed by SEM, reveals that the films deposited are less dense, uniform. Cross-sectional SEM micrographs PPNB films show that thickness of the layers is homogeneous and has value of 35-40 nm. Optical characteristics of the polymer thin films were studied using UV-vis spectroscopy; absorption of wide range of wavelengths from 350 to 700 nm was observed. The optical band gap energy ranges between 1.9 eV and 1.94 eV. Based on these analyzes we realized heterojunction organic solar cells with the structure: ITO/Au/PPNB/C60/BCP/Al, the cells had a photovoltaique effect after J-V measuring, however the efficiency of photo generation under AM1.5 illumination was weak (about 0.02%) and needs to be improved.

  1. Synthesis and electrochemical properties of novel, donor–acceptor pyrrole derivatives with 1,8-naphthalimide units and their polymers

    A new class of bipolar monomers with pyrrole or thiophene–pyrrole–thiophene as electron donor and 1,8-naphthalimide as electron acceptor unit is reported. Donor–acceptor conjugated polymers were generated electrochemically. The synthesis of monomers, optical, electrochemical and spectroelectrochemical properties supported by theoretical calculations are presented. 1,8-naphthalimide units were attached directly to pyrrole in compounds 1a and 2a or by different bridges in the case of 1b and 2b. Intra-molecular donor–acceptor interactions of the monomers and its polymers were investigated using cyclic voltammetry, in-situ UV–Vis-NIR, electron spin resonance (ESR) spectroelectrochemistry and fluorescence spectroscopy. Studied compounds present large discrepancy (up to 1.31 eV for 2a) between energy gap values determined through electrochemical and optical measurements. The Time-dependent density functional theory (TDDFT) calculations help to explain this discrepancy. This is caused by weak HOMO to LUMO transition, 2000 times weaker than HOMO−2 to LUMO or HOMO to LUMO+1 transition. Altering the structure of monomers yields different stability and properties of obtained polymers. The p- and n-doping processes are separated. Anions are localized mainly on 1,8-naphthalimide units. Cations are localized mainly on pyrrole or thiophene–pyrrole–thiophene moiety and their polymer chains. Attachment of the additional thiophene units decreases the oxidation potential of the monomer and reduces the influence of the steric hindrance between 1,8-naphthalimide moiety and polymer/oligomers chain. This new class of model compounds is promising for use as a material with enhanced charge separation for wide range of optoelectronic, electrochromic and photovoltaic applications

  2. A Hydrogen Peroxide Sensor Prepared by Electropolymerization of Pyrrole Based on Screen-Printed Carbon Paste Electrodes

    Hui Xu

    2007-03-01

    Full Text Available A disposable amperometric biosensor for commercial use to detect hydrogenperoxide has been developed. The sensor is based on screen-printed carbon paste electrodesmodified by electropolymerization of pyrrole with horseradish peroxidase (HRP entrapped.The facture techniques of fabricating the enzyme electrodes are suitable for mass productionand quality control. The biosensor shows a linear amperometric response to H2O2 from 0.1to 2.0 mM, with a sensitivity of 33.24 μA mM-1 cm-2. Different operational parameters ofelectropolymerization are evaluated and optimized.

  3. Hepatoselectivity of statins: design and synthesis of 4-sulfamoyl pyrroles as HMG-CoA reductase inhibitors.

    Park, William K C; Kennedy, Robert M; Larsen, Scott D; Miller, Steve; Roth, Bruce D; Song, Yuntao; Steinbaugh, Bruce A; Sun, Kevin; Tait, Bradley D; Kowala, Mark C; Trivedi, Bharat K; Auerbach, Bruce; Askew, Valerie; Dillon, Lisa; Hanselman, Jeffrey C; Lin, Zhiwu; Lu, Gina H; Robertson, Andrew; Sekerke, Catherine

    2008-02-01

    4-Sulfamoyl pyrroles were designed as novel hepatoselective HMG-CoA reductase inhibitors (statins) to reduce myalgia, a statin-induced adverse effect. The compounds were prepared via a [3+2] cycloaddition of a Münchnone with a sulfonamide-substituted alkyne. We identified compounds with greater selectivity for hepatocytes compared to L6-myocytes than rosuvastatin and atorvastatin. There was an inverse correlation of myocyte potencies and ClogP values. A number of analogs were effective at reducing cholesterol in acute and chronic in vivo models but they lacked sufficient chronic in vivo activity to warrant further development. PMID:18155906

  4. Ru-Catalysed C–H Arylation of Indoles and Pyrroles with Boronic Acids: Scope and Mechanistic Studies

    Sollert, Carina; Devaraj, Karthik; Orthaber, Andreas; Gates, Paul J; Pilarski, Lukasz T

    2015-01-01

    The Ru-catalysed C2–H arylation of indoles and pyrroles by using boronic acids under oxidative conditions is reported. This reaction can be applied to tryptophan derivatives and tolerates a wide range of functional groups on both coupling partners, including bromides and iodides, which can be further derivatised selectively. New indole-based ruthenacyclic complexes are described and investigated as possible intermediates in the reaction. Mechanistic studies suggest the on-cycle intermediates do not possess a para-cymene ligand and that the on-cycle metalation occurs through an electrophilic attack by the Ru centre. PMID:25689052

  5. Synthesis and Crystal Structure of N-(1'-H-Pyrrol-2'-ylcarbonyl)-5-amino-1,10-phenanthroline

    WANG Yue-Hong; LIN Hai; LIN Hua-Kuan

    2008-01-01

    The title compound,N-(1'-H-pyrrol-2'-ylcarbonyl)-5-amino-1,10-phenanthroline,was synthesized by the reaction of a-pyrrolyl carbonyl chloride and 5-amino-1,10-phenanthroline in pyridine.Determined by X-ray structure analysis,it crystallizes in triclinic system,space group P(1)with the following crystallographic data:C20H21N5O3,Mr=379.42,a=7.8559(4),b=9.1681(6),c =14.6818(9)(A),α=73.254(10),β=88.938(15),γ=68.080(10)°,V=934.66(10)(A)3,Z=2,F(000)=400.Dc=1.348 g/cm3 and μ=0.094 mm-1.The final R=0.0680 and wR=0.1419 for 2142observed reflections with I>2σ(I),and R=0.1084 and wR=0.1643 for all reflections.Two aromatic ring planes(pyrrole and phenanthroline rings)are connected by the amide plane.Two title complex molecules are connected through hydrogen bonds and weak π-π stacking interactions to generate a 3-D supramolecule.

  6. Rhodium and iridium complexes of N-(2'-hydroxyphenyl)pyrrole-2-aldimine: Synthesis, structure, and spectral and electrochemical properties

    Semanti Basu; Indrani Pal; Ray J Butcher; Georgina Rosair; Samaresh Bhattacharya

    2005-03-01

    Reaction of N-(2'-hydroxyphenyl)pyrrole-2-aldimine (H2L) with [M(PPh3)3Cl] (M = Rh, Ir) affords complexes of type [M(PPh3)2(L)Cl]. Structures of both complexes have been determined by X-ray crystallography. In both complexes, the N-(2'-hydroxyphenyl)pyrrole-2-aldimine ligand is coordinated to the metal centre, via dissociation of the acidic protons, as a dianionic tridentate N,N,O-donor. The M(L)Cl fragment constitutes an equatorial plane with the metal at the centre and the two PPh3 ligands occupying axial positions. The complexes are diamagnetic (low-spin 6, = 0) and show intense MLCT transitions in the visible region. Cyclic voltammetry of the [M(PPh3)2(L)Cl] complexes shows reversible M(III)-M(IV) oxidation near 0.5 V vs SCE and quasi-reversible ligand-centred oxidative response near 1.0 V vs SCE.

  7. Radiosynthesis and in vivo evaluation of [{sup 11}C]-labelled pyrrole-2-carboxamide derivates as novel radioligands for PET imaging of monoamine oxidase A

    De Bruyne, Sylvie [Laboratory for Radiopharmacy, Ghent University, 9000 Ghent (Belgium); La Regina, Giuseppe [Istituto Pasteur, Fondazione Cenci Bolognetti, Dipartimento di Chimica e Tecnologie del Farmaco, Sapienza Universita di Roma, I-00185 Rome (Italy); Staelens, Steven [IBITECH-Medisip, Ghent University-IBBT, 9000 Ghent (Belgium); Wyffels, Leonie [Laboratory for Radiopharmacy, Ghent University, 9000 Ghent (Belgium); Deleye, Steven [IBITECH-Medisip, Ghent University-IBBT, 9000 Ghent (Belgium); Silvestri, Romano [Istituto Pasteur, Fondazione Cenci Bolognetti, Dipartimento di Chimica e Tecnologie del Farmaco, Sapienza Universita di Roma, I-00185 Rome (Italy); De Vos, Filip [Laboratory for Radiopharmacy, Ghent University, 9000 Ghent (Belgium)], E-mail: filipx.devos@ugent.be

    2010-05-15

    Introduction: Since MAO-A is an enzyme involved in the metabolism of neurotransmitters, fluctuations in MAO-A functionality are associated with psychiatric and neurological disorders as well as with tobacco addiction and behaviour. This study reports the radiolabelling of two [{sup 11}C]-labelled pyrrole-2-carboxamide derivates, RS 2315 and RS 2360, along with the characterization of their in vivo properties. Methods: The radiolabelling of [{sup 11}C]-RS 2315 and [{sup 11}C]-RS 2360 was accomplished by alkylation of their amide precursors with [{sup 11}C]CH{sub 3}I. Biodistribution, blocking and metabolite studies of both tracers were performed in NMRI mice. Finally, a PET study in Sprague-Dawley rats was performed for [{sup 11}C]-RS 2360. Results: Both tracers were obtained in a radiochemical yield of approximately 30% with radiochemical purity of >98%. Biodistribution studies showed high brain uptake followed by rapid brain clearance for both radiotracers. In the brain, [{sup 11}C]-RS 2360 was more stable than [{sup 11}C]-RS 2315. Blocking studies in mice could not demonstrate specificity of [{sup 11}C]-RS 2315 towards MAO-A or MAO-B. The blocking and imaging study with [{sup 11}C]-RS 2360 on the other hand indicated specific binding in MAO-A at the earliest time points. Conclusions: [{sup 11}C]-RS 2315 displayed a high nonspecific binding and is therefore not suitable for visualization of MAO-A in vivo. [{sup 11}C]-RS 2360 on the other hand has potential for mapping MAO-A since specific binding is demonstrated.

  8. Radiosynthesis and in vivo evaluation of [11C]-labelled pyrrole-2-carboxamide derivates as novel radioligands for PET imaging of monoamine oxidase A

    Introduction: Since MAO-A is an enzyme involved in the metabolism of neurotransmitters, fluctuations in MAO-A functionality are associated with psychiatric and neurological disorders as well as with tobacco addiction and behaviour. This study reports the radiolabelling of two [11C]-labelled pyrrole-2-carboxamide derivates, RS 2315 and RS 2360, along with the characterization of their in vivo properties. Methods: The radiolabelling of [11C]-RS 2315 and [11C]-RS 2360 was accomplished by alkylation of their amide precursors with [11C]CH3I. Biodistribution, blocking and metabolite studies of both tracers were performed in NMRI mice. Finally, a PET study in Sprague-Dawley rats was performed for [11C]-RS 2360. Results: Both tracers were obtained in a radiochemical yield of approximately 30% with radiochemical purity of >98%. Biodistribution studies showed high brain uptake followed by rapid brain clearance for both radiotracers. In the brain, [11C]-RS 2360 was more stable than [11C]-RS 2315. Blocking studies in mice could not demonstrate specificity of [11C]-RS 2315 towards MAO-A or MAO-B. The blocking and imaging study with [11C]-RS 2360 on the other hand indicated specific binding in MAO-A at the earliest time points. Conclusions: [11C]-RS 2315 displayed a high nonspecific binding and is therefore not suitable for visualization of MAO-A in vivo. [11C]-RS 2360 on the other hand has potential for mapping MAO-A since specific binding is demonstrated.

  9. The Synthesis of Novel 3-Substituted Poly(pyrroles) Bearing Crown-ether Moieties and a Study of their Electrochemical Properties

    Guernion, Nicolas J.L.; Blencowe, A.; Hayes, Wayne;

    2006-01-01

    A series of fourteen novel pyrrole monomers substituted at the 3-position with aliphatic and aromatic crown-ether moieties have been synthesised in good yield and characterised extensively. Several of those compounds were electropolymerised successfully in acetonitrile, using both potentiostatic ...

  10. Ion-Regulated Allosteric Binding of Fullerenes (C-60 and C-70) by Tetrathiafulvalene-Calix[4]pyrroles

    Davis, C. M.; Lim, J. M.; Larsen, K. R.;

    2014-01-01

    The effect of ionic species on the binding of fullerenes (C-60 and C-70) by tetrathiafulvalene-calix[4]pyrrole (TTF-C4P) receptors and the nature of the resulting supramolecular complexes (TTF-C4P + fullerene + halide anion + tetraalkylammonium cation) was studied in the solid state through single...... the C4P in a ball-and-socket binding mode. The interactions between the TTF-C4P receptors and the fullerene guests are highly influenced by both the nature of halide anions and their counter tetraalkylammonium cations. Three halides (F-, Cl-, and Br-) were studied. All three potentiate the binding of...... the two test fullerenes by inducing a conformational change from the 1,3-alternate to the cone conformer of the TTF-C4Ps, thus acting as positive heterotropic allosteric effectors. For a particular halide anion, the choice of tetraalkylammonium salts serves to modulate the strength of the TTF-C4P...

  11. Porous polypyrrole/polymethylmethacrylate composite film prepared by vapor deposition polymerization of pyrrole and its application for ammonia detection

    A simple method has been developed to fabricate porous polypyrrole/polymethyl methacrylate composite films. The synthesis procedures include the vapor deposition polymerization of pyrrole on the composite films of polymethyl methacrylate and ferric hydroxide bis(1,4-bis(2-ethylhexyl) sulfosuccinate), successively, washing the obtained composite films with methanol. Scanning electron microscopic and microscopic Raman spectral studies indicated that the pores had an average size of about 5 μm and they were uniformly dispersed in the whole films. The electrical conductivities of the composite films were measured to be in the range of 10-3 to 10-2 S cm-1. The porous composite films showed electroactivity, and the sensors based on them exhibited high sensitivity and fast response to ammonia gas

  12. Design and modelling of enzyme/poly-pyrrole modified electrodes for bio-catalyzed electro-synthesis processes

    This research thesis reports a study which aims at developing, analyzing and integrating an electrode-enzyme interface within an electro-enzymatic reactor to develop electrochemical biosensors. The adopted method comprises a confinement of the enzyme at the electrode surface by means of an electro-formed poly-pyrrole film. The author reports an experimental and theoretical study of the coupling between electrochemical reaction, enzymatic reaction and matter transfer in the polymer in order to better understand the operation of so-modified electrodes. Different parameters have an influence on the reaction rate. A numerical model (validated by experiments) allows the identification of the reaction limiting stages. A new elaboration protocol allows the polymer permeability to be increased. The interface is first applied to the reduction of the NAD coenzyme, and the process is also applied to the production of gluconic acid

  13. Hemispherand-Strapped Calix[4]pyrrole: An Ion-pair Receptor for the Recognition and Extraction of Lithium Nitrite.

    He, Qing; Zhang, Zhan; Brewster, James T; Lynch, Vincent M; Kim, Sung Kuk; Sessler, Jonathan L

    2016-08-10

    The hemispherand-strapped calix[4]pyrrole (1) acts as an ion pair receptor that exhibits selectivity for lithium salts. In organic media (CD2Cl2 and CD3OD, v/v, 9:1), receptor 1 binds LiCl with high preference relative to NaCl, KCl, and RbCl. DFT calculations provided support for the observed selectivity. Single crystal structures of five different lithium ion-pair complexes of 1 were obtained. In the case of LiCl, a single bridging water molecule between the lithium cation and chloride anion was observed, while tight contact ion pairs were observed in the case of the LiBr, LiI, LiNO3, and LiNO2 salts. Receptor 1 proved effective as an extractant for LiNO2 under both model solid-liquid and liquid-liquid extraction conditions. PMID:27442768

  14. Preparation and characterization of poly-pyrrole thin films functionalized by ion exchanger groups. Application to preparation of alpha sources

    After having outlined that dosing methods still present problems related to chemical separations techniques used before radioactivity measurements, and to spectrometric methods, this research thesis proposes the study of a new method of fabrication of a radioactive source. This method comprises the fabrication of a chemically reactive thin film by electro-polymerization, and the incorporation of actinides in the deposit by ion exchange. In this case, the deposit thickness could be controlled and the material transfer chemical mechanisms could be predicted and controlled

  15. Post Hartree–Fock and DFT Studies on Pyrrole···Nitrogen and Pyrrole···Carbon Monoxide Molecules

    P. Kolandaivel

    2002-07-01

    Full Text Available Abstract: The hydrogen bonded and van der Waals isomers of pyrrole···nitrogen and pyrrole···carbon monoxide have been studied using ab initio and density functional theory methods. Complex geometries and total energies of the isomers have been determined at HF, MP2, B3LYP and B3PW91 levels of theory employing 6-31G* basis set. For pyrrole···nitrogen complex, only two isomers have stable structure and the more stable one is found to be the hydrogen bonded isomer. Among the five isomers of pyrrole···carbon monoxide complex, the hydrogen bonded isomer is found to be the most stable form. The interaction energy for all these isomers have been calculated after eliminating the basis set superposition errors by using the full counterpoise correction method. Chemical hardness, chemical potential have been calculated and are used to study the stability of the molecules.

  16. Deproto-metallation of N-arylated pyrroles and indoles using a mixed lithium–zinc base and regioselectivity-computed CH acidity relationship

    Mohamed Yacine Ameur Messaoud

    2015-08-01

    Full Text Available The synthesis of N-arylated pyrroles and indoles is documented, as well as their functionalization by deprotonative metallation using the base in situ prepared from LiTMP and ZnCl2·TMEDA (1/3 equiv. With N-phenylpyrrole and -indole, the reactions were carried out in hexane containing TMEDA which regioselectively afforded the 2-iodo derivatives after subsequent iodolysis. With pyrroles and indoles bearing N-substituents such as 2-thienyl, 3-pyridyl, 4-methoxyphenyl and 4-bromophenyl, the reactions all took place on the substituent, at the position either adjacent to the heteroatom (S, N or ortho to the heteroatom-containing substituent (OMe, Br. The CH acidities of the substrates were determined in THF solution using the DFT B3LYP method in order to rationalize the experimental results.

  17. Silica sulfuric acid: a reusable solid catalyst for one pot synthesis of densely substituted pyrrole-fused isocoumarins under solvent-free conditions

    Sudipta Pathak

    2013-11-01

    Full Text Available A convenient and efficient methodology for the synthesis of densely substituted pyrrole-fused isocoumarins, which employs solid-supported silica sulfuric acid (SSA as catalyst, has been developed. When the mixture of ninhydrin adducts of acetylacetone/ethyl acetoacetate and primary amines was heated on the solid surface of SSA under solvent-free conditions, the pyrrole-fused isocoumarins were formed in good yields. This synthetic method has several advantages such as the employment of solvent-free reaction conditions without the use of any toxic reagents and metal catalysts, the ease of product isolation, the use of a recyclable catalyst, the low cost, the easy availability of the starting materials, and the excellent yields of products.

  18. 3-(Dicyanomethylidene)indan-1-one-Functionalized Calix[4]arene-Calix[4]pyrrole Hybrid: An Ion-Pair Sensor for Cesium Salts.

    Yeon, Yerim; Leem, Soojung; Wagen, Corin; Lynch, Vincent M; Kim, Sung Kuk; Sessler, Jonathan L

    2016-09-01

    A chromogenic calix[4]arene-calix[4]pyrrole hybrid ion pair receptor bearing an indane substituent at a β-pyrrolic position has been prepared. On the basis of solution-phase UV-vis spectroscopic analysis and (1)H NMR spectroscopic studies carried out in 10% methanol in chloroform, receptor 1 is able to bind only cesium ion pairs (e.g., CsF, CsCl, and CsNO3) but not the constituent cesium cation (as its perchlorate salt) or the F(-), Cl(-), or NO3(-) anions (as the tetrabutylammonium salts). It thus displays rudimentary AND logic gate behavior. Receptor 1 shows a colorimetric response to cesium ion pairs under conditions of solid-liquid (nitrobenzene) and liquid-liquid (D2O-nitrobenzene-d5) extraction. PMID:27533478

  19. Synthesis and phototoxicity of isomeric 7,9-diglutathione pyrrole adducts: Formation of reactive oxygen species and induction of lipid peroxidation

    Liang Ma

    2015-09-01

    Full Text Available Pyrrolizidine alkaloids (PAs are hepatotoxic, genotoxic, and carcinogenic in experimental animals. Because of their widespread distribution in the world, PA-containing plants are probably the most common poisonous plants affecting livestock, wildlife, and humans. Upon metabolism, PAs generate reactive dehydro-PAs and other pyrrolic metabolites that lead to toxicity. Dehydro-PAs are known to react with glutathione (GSH to form 7-GSH-(+/−-6,7-dihydro-7-hydroxy-1-hydroxymethyl-5H-pyrrolizine (7-GS-DHP in vivo and in vitro and 7,9-diGS-DHP in vitro. To date, the phototoxicity of GS-DHP adducts has not been well studied. In this study, we synthesized 7-GS-DHP, a tentatively assigned 9-GS-DHP, and two enantiomeric 7,9-diGS-DHP adducts by reaction of dehydromonocrotaline with GSH. The two 7,9-diGS-DHPs were separated by high performance liquid chromatography (HPLC and their structures were characterized by 1H nuclear magnetic resonance (NMR and 1H–1H correlation spectroscopy (COSY NMR spectral analysis. Photoirradiation of 7-GS-DHP, 9-GS-DHP, and the two 7,9-diGS-DHPs as well as dehydromonocrotaline, dehydroheliotrine, and the 7-R enantiomer of DHP (DHR, by UVA light at 0 J/cm2, 14 J/cm2, and 35 J/cm2 in the presence of a lipid, methyl linoleate, all resulted in lipid peroxidation in a light dose-responsive manner. The levels of lipid peroxidation induced by the two isomeric 7,9-diGS-DHPs were significantly higher than that by 7-GS-DHP and 9-GS-DHP. When 7,9-diGS-DHP was irradiated in the presence of sodium azide (NaN3, the level of lipid peroxidation decreased; lipid peroxidation was enhanced when methanol was replaced by deuterated methanol. These results suggest that singlet oxygen is a product induced by the irradiation of 7,9-diGS-DHP. When irradiated in the presence of superoxide dismutase (SOD, the level of lipid peroxidation decreased, indicating that lipid peroxidation is also mediated by superoxide. These results indicate that lipid

  20. Stereoselective self-sorting in the self-assembly of a Phe-Phe extended guanidiniocarbonyl pyrrole carboxylate zwitterion: formation of two diastereomeric dimers with significantly different stabilities.

    Rodler, Fabian; Sicking, Wilhelm; Schmuck, Carsten

    2011-07-28

    The 'dipeptide extended' guanidiniocarbonyl pyrrole carboxylate zwitterion GCP-Phe-Phe 1 forms stable dimers in DMSO. However, dimerization is highly stereoselective. Only homochiral dimers are formed and the (L,L)·(L,L) dimer (K(dim) > 10(5) M(-1)) is significantly more stable by a factor of 10(3) than the diastereomeric (D,L)·(D,L) dimer (K(dim) = 120 M(-1)). PMID:21670799

  1. Synthesis of new pyrrole, pyrazole, pyrimidine and pyrrolopyrimidine derivatives carrying a sulfonamide moiety of expected antitumor activity with studying the synergistic effect of γ-irradiation

    In a search for new cytotoxic agents with improved antitumor activity, some new pyrrole, pyrazole pyrimidine and pyrrolo[2,3-d] pyrimidine derivatives bearing sulfonamide moiety were synthesized. All the newly synthesized compound were subjected to in-vitro cytotoxic screening, also the synergism of the synthesized compounds with radiation was studies. These new compounds were docked in the active site of the carbonic anhydrase enzyme.

  2. 2,2′,5,5′-Tetramethyl-1,1′-(hexane-1,6-diyldi-1H-pyrrole

    Ana C. Santos

    2009-07-01

    Full Text Available The molecule of the title compound, C18H28N2, composed of two 2,5-dimethylpyrrole groups linked by a hexane chain, lies across a crystallographic inversion centre. The mean plane of the pyrrole ring is almost perpendicular to the mean plane of the central chain, making a dihedral angle of 89.09 (8°. The crystal structure is stabilized by intermolecular C—H...π interactions.

  3. Photocatalytic Degradation of Eosin Yellow Using Poly(pyrrole-co-aniline)-Coated TiO2/Nanocellulose Composite under Solar Light Irradiation

    Anirudhan, T. S.; Rejeena, S. R.

    2015-01-01

    The present study describes the feasibility of a novel adsorbent cum photocatalyst, poly(pyrrole-co-aniline)-coated TiO2/nanocellulose composite (P(Py-co-An)-TiO2/NCC), to remove eosin yellow (EY) from aqueous solutions. The removal of EY was investigated by batch adsorption followed by photocatalysis. The effect of various adsorption parameters like adsorbent dose, pH, contact time, initial concentration, and ionic strength has been optimized for treating effluents from the dye industry. Ads...

  4. Antitumor Activity of a 5-Hydroxy-1H-Pyrrol-2-(5H-One-Based Synthetic Small Molecule In Vitro and In Vivo.

    Yunyun Geng

    Full Text Available Alternative chemo-reagents are in great demand because chemotherapy resistance is one of the major challenges in current cancer treatment. 5-hydoxy-1H-pyrrol-2-(5H-one is an important N-heterocyclic scaffold that is present in natural products and medicinal chemistry. However, its antitumor activity has not been systematically explored. In this study, we screened a panel of 5-hydoxy-1H-pyrrol-2-(5H-one derivatives and identified compound 1d as possessing strong anti-proliferative activity in multiple cancer cell lines. Cell cycle analysis revealed that 1d can induce S-phase cell cycle arrest and that HCT116 was sensitive to 1d-induced apoptosis. Further analysis indicated that 1d preferentially induced DNA damage and p53 activation in HCT116 cells and that 1d-induced apoptosis is partly dependent on p53. Furthermore, we showed that 1d significantly suppressed tumor growth in xenograft tumor models in vivo. Taken together, our results suggest that 5-hydoxy-1H-pyrrol-2-(5H-one derivatives bear potential antitumor activity and that 1d is an effective agent for cancer treatment.

  5. Orange to black electrochromic behaviour in poly(2-(2-thienyl)-1H-pyrrole) thin films

    We have studied an electrochromic precursor, 2-(2-thienyl)-1H-pyrrole (1), using two improved procedures of the Trofimov reaction. Optimised stereochemical calculations at the B3LYP/6-311G* level showed almost equal s-cis and s-trans conformational populations in 1 with marked out-of-plane deviations of ca. 30o. Model calculations suggest that the predominant rotational conformation in undoped poly(1) would be s-trans with the essential out-of-plane deviations around the all three interheterocyclic bonds of ca. 25-30o. Monomer 1 exhibited two irreversible oxidation processes at +0.86 and +1.3 V corresponding to the oxidation of the pyrrole and thiophene rings, respectively. Orange to black electrochromic behaviour was found in ClO4- doped poly(1) thin films with colouring and bleaching times of 1.8 and 1.3 s, respectively. The colouration efficiency during the bleaching process was 233 cm2/C. The optical contrast at 450 nm was 19% and in the near-IR was 36%. The band-gap of poly(1) (1.6-1.7 eV) was found to be significantly lower than that of polypyrrole (2.85 eV) and polythiophene (2.3 eV) as a consequence of increased electron delocalisation in the system. Important differences in the morphology of doped and dedoped poly(1) films were observed by atomic-force microscopy (AFM). Doped poly(1) films showed a granular morphology with primary particles of 45-60 nm in size and an average surface roughness of 3.5 nm. On the other hand, dedoped poly(1) films showed interconnected aggregates of 65-90 nm in size as a consequence of particle fusion, with a surface roughness of 9.2 nm. In summary, poly(1) is a promising material for emerging flexible electrochromic devices such as displays and variable optical attenuators

  6. Preparation of thin {alpha}-particle sources using poly-pyrrole films functionalized by a chelating agent; Preparation de sources minces d'emetteurs alpha a l'aide de films de polypyrrole fonctionnalises par un ligand chelatant

    Mariet, C. [CEA Saclay, INSTN, Institut National des Sciences et Techniques Nucleaires, 91 - Gif-sur-Yvette (France); Universite Pierre et Marie Curie, 75 - Paris (France)

    2000-07-01

    This work takes place in the scope of analysis of the {alpha}-particle emitting elements U, Pu and Am present in compound environmental matrix like sols and sediments. The samples diversity and above all the {alpha}-ray characteristics require the analyst to implement a sequence of chemical steps in which the more restricting is the actinides concentration in a uniform and thin layer en allowing an accurately measure of alpha activity. On this account, we studied a new technique for radioactive sources preparation based on tow steps: preparation of a thin film as source support; incorporation of radioactive elements by a chelating extraction mechanism. The thin films were obtained through electro-polymerization of pyrrole monomer functionalized by an chelating ligand able to extract actinides from concentrated acidic solutions. Polymerization conditions of this monomer were perfected, then obtained films were characterized from a physico-chemical point of view. We point out their extracting properties were comparable to (retention capacity, distribution coefficient) to those of usual ion-exchange resins. The underscore of uranyl and americium nitrate complexes formed in the thin layer allowed to calculate the extraction constants in case acid extraction is negligible. Thanks to this results, the values of the coefficients distribution D{sub U} and D{sub Am} could be provided for all nitric solutions in which acid extraction is negligible. Optimal actinides retention conditions in the polymer were defined and used to settle a protocol for plutonium analysis in environmental samples. (author)

  7. Comparative neurotoxicity and pyrrole-forming potential of 2,5-hexanedione and perdeuterio-2,5-hexanedione in the rat

    DeCaprio, A.P.; Briggs, R.G.; Jackowski, S.J.; Kim, J.C.

    1988-01-01

    2,5-Hexanedione (2,5-HD), the neurotoxic metabolite of n-hexane, reacts with protein amines to form alkylpyrrole adducts. Pyrrolylation of neurofilament protein may be the initiating molecular event in 2,5-HD neuropathy. The present study compares the neurotoxic and pyrrole-forming potentials of 2,5-HD with those of perdeuterio-2,5-HD ((D10)-2,5-HD) in the rat. Due to a requirement for C-H bond breaking in the reaction mechanism, the latter derivative was expected to exhibit a primary isotope effect, thus forming the pyrrole at a slower rate. In vitro studies confirmed that (D10)-2,5-HD pyrrolylated protein at only one-third of the initial rate seen with native 2,5-HD. Prolonged incubation resulted in similar pyrrole concentrations with both derivatives. Adult, male Wistar rats were administered daily (5 days/week) ip doses of either 3.5 mmol 2,5-HD or (D10)-2,5-HD/kg/day for 17 days or 2.5 mmol/kg/day for 38 days. At termination, animals administered 2,5-HD and (D10)-2,5-HD exhibited 27 and 8% body weight loss, respectively. Moderate to severe hindlimb paralysis was present in the 2,5-HD groups while only mild effects were seen in (D10)-2,5-HD-dosed rats. Neuropathological changes were prominent in spinal cord sections from 2,5-HD-treated animals, while no effects were present in rats given the deuterated derivative. Pyrrole adduct concentrations in serum and axonal cytoskeletal proteins from 2,5-HD-treated animals were two- to threefold higher than in rats given equimolar doses of (D10)-2,5-HD. Levels of covalent crosslinking of axonal cytoskeletal proteins (assessed by sodium dodecyl sulfate-polyacrylamide gel electrophoresis) appeared to correlate with pyrrole concentrations. Tissue concentrations of each diketone isomer were not significantly different, indicating similar uptake of native and deuterated 2,5-HD.

  8. Electropolymerization of pyrrole on oxidizable metal under high frequency ultrasound irradiation. Application of focused beam to a selective masking technique

    Et Taouil, A. [Institut UTINAM, UMR 6213 CNRS, Universite de Franche-Comte, 30 Avenue de l' observatoire, 25009 Besancon Cedex (France); Lallemand, F., E-mail: fabrice.lallemand@univ-fcomte.f [Institut UTINAM, UMR 6213 CNRS, Universite de Franche-Comte, 30 Avenue de l' observatoire, 25009 Besancon Cedex (France); Hallez, L.; Hihn, J-Y. [Institut UTINAM, UMR 6213 CNRS, Universite de Franche-Comte, 30 Avenue de l' observatoire, 25009 Besancon Cedex (France)

    2010-12-01

    A novel masking technique against polymer deposition based on High Intensity Focused Ultrasound (HIFU) irradiation was developed for the first time. With this in mind, a variety of background salts were tested. Sodium salicylate was found to be the most effective electrolytic medium for pyrrole sonoelectropolymerization on copper as it leads to a very efficient passivating oxide layer preventing copper dissolution while enabling polymer formation independently from sonication. In such a medium, high frequency ultrasound greatly refines surface structure, and a slight increase in doping level is observed. Finally, it was proved that focused ultrasound increases copper dissolution in sodium oxalate electrolyte while preventing polypyrrole deposition. A selected zone on the copper substrate was thus irradiated by the focused ultrasound beam to protect it from polymerization. In a second stage, a self-assembled monolayer was deposited on this polymer-free area to create a surface biphased substrate. This type of masking technique can be proposed as an interesting alternative to lithography as it is easier to carry out and allows chemical waste reduction.

  9. A pyrrole quinoline quinone glucose dehydrogenase biosensor based on screen-printed carbon paste electrodes modified by carbon nanotubes

    A carbon nanotube (CNT) modified biosensor based on oxygen-independent, pyrrole quinoline quinone glucose dehydrogenase (PQQ-GDH) for monitoring glucose was studied. The disposable amperometric biosensors based on screen-printed carbon paste electrodes are low cost and suitable for mass production. Potassium ferricyanide was immobilized on the surface of the electrodes as an electron mediator, which decreased the work potential. The biosensor showed a linear amperometric response to glucose from 1 to 35 mM, with a sensitivity of 31.0 µA mM−1 cm−2. Experimentally, the compositions of PQQ-GDH, potassium ferricyanide, CNTs and other components were evaluated and optimized. Only 2 µl of sample are needed for one test, and the response time of the sensor is 20 s. The characteristics of the biosensor were studied through cyclic voltammetry, and experimental results showed that the CNTs could facilitate the electron transfer between the enzyme and electrode surface significantly. Compared with the biosensor without carbon nanotube modification, the CNTs improved the sensitivity of the biosensor up to five times

  10. Sub-10 nm Platinum Nanocrystals with Size and Shape Control: Catalytic Study for Ethylene and Pyrrole Hydrogenation

    Tsung, Chia-Kuang; Kuhn, John N.; Huang, Wenyu; Aliaga, Cesar; Hung, Ling-I; Somorjai, Gabor A.; Yang, Peidong

    2009-03-02

    Platinum nanocubes and nanopolyhedra with tunable size from 5 to 9 nm were synthesized by controlling the reducing rate of metal precursor ions in a one-pot polyol synthesis. A two-stage process is proposed for the simultaneous control of size and shape. In the first stage, the oxidation state of the metal ion precursors determined the nucleation rate and consequently the number of nuclei. The reaction temperature controlled the shape in the second stage by regulation of the growth kinetics. These well-defined nanocrystals were loaded into MCF-17 mesoporous silica for examination of catalytic properties. Pt loadings and dispersions of the supported catalysts were determined by elemental analysis (ICP-MS) and H2 chemisorption isotherms, respectively. Ethylene hydrogenation rates over the Pt nanocrystals were independent of both size and shape and comparable to Pt single crystals. For pyrrole hydrogenation, the nanocubes enhanced ring-opening ability and thus showed a higher selectivity to n-butylamine as compared to nanopolyhedra.

  11. Effect of non-electroactive additives on the early stage pyrrole electropolymerization on indium tin oxide electrodes

    Castro-Beltran, A. [Facultad de Ingeniería Mecánica y Eléctrica, Universidad Autónoma de Nuevo León, Ave. Pedro de Alba s/n, Ciudad Universitaria, C.P. 66451 San Nicolás de los Garza, N.L. (Mexico); Centro de Innovación Investigación y Desarrollo en Ingeniería y Tecnología (CIIDIT), Universidad Autónoma de Nuevo León, PIIT-Monterrey C.P. 66600 Apodaca, N.L. (Mexico); Dominguez, C.; Bahena-Uribe, D. [Centro Investigación en Ingeniería y Ciencias Aplicadas (CIICAp), Universidad Autónoma del Estado de Morelos, Av. Universidad 1001, Col. Chamilpa, C.P. 62209 Cuernavaca, Mor. (Mexico); Sepulveda-Guzman, S., E-mail: selene.sepulvedagz@uanl.edu.mx [Facultad de Ingeniería Mecánica y Eléctrica, Universidad Autónoma de Nuevo León, Ave. Pedro de Alba s/n, Ciudad Universitaria, C.P. 66451 San Nicolás de los Garza, N.L. (Mexico); Centro de Innovación Investigación y Desarrollo en Ingeniería y Tecnología (CIIDIT), Universidad Autónoma de Nuevo León, PIIT-Monterrey C.P. 66600 Apodaca, N.L. (Mexico); Cruz-Silva, R. [Research Center for Exotic NanoCarbon, Shinshu University, 4-17-1 Wakasato, Nagano 380-8553 (Japan)

    2014-09-01

    The use of non-electroactive additives during electrodeposition of conducting polymers has long been used to modify the properties of deposited films. These additives can improve the adhesion, and not only change the morphology and deposition rate but also modify the chemical composition of the electrodeposited polymer. Several compounds have been used to modify deposition of polypyrrole; however, there is no systematic study of these compounds. In this work, we comparatively studied several water soluble chemical compounds, a cationic polymer, an anionic polymer, a cationic surfactant, and an anionic surfactant during potentiostatic electrodeposition of polypyrrole. In order to study the effect of these compounds on the interface, where the electrochemical polymerization takes place, we used electrochemical impedance spectroscopy. The morphology during the initial stage of growth was studied by atomic force microscopy, whereas the resulting polypyrrole films were observed by scanning electron microscopy. - Highlights: • Early-stage polymerization polypyrrole particles on indium tin oxide (ITO). • Anionic additives promote pyrrole oxidation and polypyrrole film growth on ITO. • Cationic polyelectrolyte promotes adhesion between ITO and polypyrrole film. • Non-electroactive additives strongly influence polypyrrole nucleation on ITO.

  12. One electron vs. two electron electrochemical and chemical oxidation of electron-donor substituted diketo-pyrrolo-pyrroles

    Electrochemical and chemical (using FeCl3) oxidation reactions of a series of eight N,N′-dialkylated soluble diketo-pyrrolo-pyrrole dyes (DPPs) substituted by electron donating and/or electron withdrawing groups were investigated electrochemically and by UV–vis spectrometry and the results were rationalized by DFT calculations. Influence of substituents on HOMO and LUMO energies as well as on the electron transfer mechanism was followed. Destabilization of HOMO by two piperidino-substituents in 3,6-diphenyl-DPP 5 enabled to observe a potential inversion in electrochemical oxidation of this derivative, when a two-electron oxidation occurs leading directly to a dication, whereas other DPPs are oxidized first in a one-electron transfer to a radical cation. In chemical oxidation with FeCl3 the radical cation is produced by two mechanisms: either directly (standard reaction) or in the case of 5 by a comproportionation reaction of neutral molecule and its dication. Using mutual comparison of oxidation potentials and HOMO/LUMO energies a quite realistic limit of FeCl3 oxidation ability in acetonitrile was found

  13. Research on interfacial polymerization of pyrrole assist with Span80 system

    Yang, Q. H.; Tu, Z. Y.; Zhao, N. Y.

    2016-07-01

    With assistance of surfactants, self-assembled Polypyrrole (PPy) film was prepared via oil / water interfacial polymerization. The chemical structure and morphologies of the obtained samples have been characterized by Fourier transform infrared (FT-IR) and Scanning Electron Microscope (SEM), respectively. The electrochemical performance recorded on an electrochemical workstation, mainly includes cyclic voltammetry (CV) tests. The prepared PPy film has its own extremely vesicular structures from results and indicates by using different concentration surfactant Span80. The PPy film prepared 25 °C with 3.32 g/L Span80 (surpass its critical micelle concentration) as a surfactant possess a supernal specific capacitance of 368.18 F/g at a scan rate 50 mV/s in 1 M NaNO3 aqueous solution at.

  14. Metalloporphyrins with all the pyrrole nitrogens replaced with phosphorus atoms, MP(P)4 (M = Sc, Ti, Fe, Ni, Cu, Zn)

    Highlights: • First systematic DFT study of the MP(P)4 compounds with increasing number of d-electrons. • Complete substitution of pyrrole nitrogens by P-atoms does not change the ground spin state. • Complete substitution of pyrrole nitrogens by P-atoms results in a bowl-like shape. • Significant stabilization of the MP(P)4 LUMOs compared to the MP counterparts. • MP(P)4 HOMO/LUMO gaps are smaller than the MP HOMO/LUMO gaps. - Abstract: We performed first systematic DFT study of the structures and electronic features (frontier orbitals energies, HOMO/LUMO and optical gaps, IPs and EAs) of the MP(P)4 compounds, with increasing number of d-electrons: 3d14s2 (Sc) → 3d24s2 (Ti) → 3d64s2 (Fe) → 3d84s2 (Ni) → 3d104s1 (Cu) → 3d104s2 (Zn). We performed systematic comparison with the tetrapyrrole MP counterparts. Complete substitution of the pyrrole nitrogens by P-atoms does not change the calculated ground spin state of the compound. All the MP(P)4 species adopt a bowl-like shape, compared to generally planar or slightly distorted shapes of their MP counterparts. Significant positive charge accumulates on P-atoms in MP(P)4. Positive charges on the metals in MP(P)4 are noticeably lower than in the MP counterparts. The calculated MP(P)4 HOMO/LUMO gaps and optical gaps are noticeably smaller than the corresponding gaps in their MP counterparts, which is explained by stabilization of the MP(P)4 LUMOs

  15. Metalloporphyrins with all the pyrrole nitrogens replaced with phosphorus atoms, MP(P){sub 4} (M = Sc, Ti, Fe, Ni, Cu, Zn)

    Kuznetsov, Aleksey E., E-mail: aleksey73kuznets@gmail.com

    2015-02-02

    Highlights: • First systematic DFT study of the MP(P){sub 4} compounds with increasing number of d-electrons. • Complete substitution of pyrrole nitrogens by P-atoms does not change the ground spin state. • Complete substitution of pyrrole nitrogens by P-atoms results in a bowl-like shape. • Significant stabilization of the MP(P){sub 4} LUMOs compared to the MP counterparts. • MP(P){sub 4} HOMO/LUMO gaps are smaller than the MP HOMO/LUMO gaps. - Abstract: We performed first systematic DFT study of the structures and electronic features (frontier orbitals energies, HOMO/LUMO and optical gaps, IPs and EAs) of the MP(P){sub 4} compounds, with increasing number of d-electrons: 3d{sup 1}4s{sup 2} (Sc) → 3d{sup 2}4s{sup 2} (Ti) → 3d{sup 6}4s{sup 2} (Fe) → 3d{sup 8}4s{sup 2} (Ni) → 3d{sup 10}4s{sup 1} (Cu) → 3d{sup 10}4s{sup 2} (Zn). We performed systematic comparison with the tetrapyrrole MP counterparts. Complete substitution of the pyrrole nitrogens by P-atoms does not change the calculated ground spin state of the compound. All the MP(P){sub 4} species adopt a bowl-like shape, compared to generally planar or slightly distorted shapes of their MP counterparts. Significant positive charge accumulates on P-atoms in MP(P){sub 4}. Positive charges on the metals in MP(P){sub 4} are noticeably lower than in the MP counterparts. The calculated MP(P){sub 4} HOMO/LUMO gaps and optical gaps are noticeably smaller than the corresponding gaps in their MP counterparts, which is explained by stabilization of the MP(P){sub 4} LUMOs.

  16. 3He NMR studies on helium-pyrrole, helium-indole, and helium-carbazole systems: a new tool for following chemistry of heterocyclic compounds.

    Radula-Janik, Klaudia; Kupka, Teobald

    2015-02-01

    The (3)He nuclear magnetic shieldings were calculated for free helium atom and He-pyrrole, He-indole, and He-carbazole complexes. Several levels of theory, including Hartree-Fock (HF), Second-order Møller-Plesset Perturbation Theory (MP2), and Density Functional Theory (DFT) (VSXC, M062X, APFD, BHandHLYP, and mPW1PW91), combined with polarization-consistent pcS-2 and aug-pcS-2 basis sets were employed. Gauge-including atomic orbital (GIAO) calculated (3)He nuclear magnetic shieldings reproduced accurately previously reported theoretical values for helium gas. (3)He nuclear magnetic shieldings and energy changes as result of single helium atom approaching to the five-membered ring of pyrrole, indole, and carbazole were tested. It was observed that (3)He NMR parameters of single helium atom, calculated at various levels of theory (HF, MP2, and DFT) are sensitive to the presence of heteroatomic rings. The helium atom was insensitive to the studied molecules at distances above 5 Å. Our results, obtained with BHandHLYP method, predicted fairly accurately the He-pyrrole plane separation of 3.15 Å (close to 3.24 Å, calculated by MP2) and yielded a sizable (3)He NMR chemical shift (about -1.5 ppm). The changes of calculated nucleus-independent chemical shifts (NICS) with the distance above the rings showed a very similar pattern to helium-3 NMR chemical shift. The ring currents above the five-membered rings were seen by helium magnetic probe to about 5 Å above the ring planes verified by the calculated NICS index. PMID:25228253

  17. Structure and spectroscopic properties of N,S-coordinating 2-methylsulfanyl-N-[(1H-pyrrol-2-ylmethylidene]aniline methanol monosolvate

    D. Douglas Richards

    2015-10-01

    Full Text Available The reaction of pyrrole-2-carboxaldehyde and 2-(methylsulfanylaniline in refluxing methanol gave an olive-green residue in which yellow crystals of the title compound, C12H12N2S·CH3OH, were grown from slow evaporation of methanol at 263 K. In the crystal, hydrogen-bonding interactions link the aniline molecule and a nearby methanol solvent molecule. These units are linked by a pair of weak C—H...Omethanol interactions, forming inversion dimers consisting of two main molecules and two solvent molecules.

  18. Gliclazide impurity F: N-[(perhydro­cyclo­penta­[c]pyrrol-2-yl)amino­carbon­yl]-o-toluene­sulfonamide

    Di Wu; Xueyuan Wang; Dongying Pang; Wei Su; Yan Sun

    2012-01-01

    The title compound, C15H21N3O3S, is known to be an impurity of gliclazide [systematic name: N-(hexahydro-1H-cyclopenta[c]pyrrol-2-ylcarbamoyl)-4-methylbenzenesulfonamide], a sulfonylurea antidiabetic drug. Gliclazide has a p-tolyl group substituting the sulfonamide functionality, while the title molecule contains an o-tolyl group. Both five-membered fused rings adopt envelope conformations. In the crystal, N—H...O hydrogen bonds are formed between HN(C=O)NH groups, building centrosy...

  19. Synthesis of 5,6-dihydropyrrolo[2,1-a]isoquinolines featuring an intramolecular radical-oxidative cyclization of polysubstituted pyrroles, and evaluation of their cytotoxic activity.

    Reyes-Gutiérrez, Paul E; Camacho, José R; Ramírez-Apan, Maria Teresa; Osornio, Yazmin M; Martínez, Roberto

    2010-10-01

    A three-step protocol for the synthesis of 1,2,3,8,9-pentasubstituted-5,6-dihydropyrrolo[2,1-a]isoquinolines is described, using van Leusen's polysubstituted pyrrole construction followed by intramolecular radical-oxidative cyclization of the isoquinoline system. The cytotoxic activities of the dihydropyrroloisoquinolines were tested on six tumor cell lines. Preliminary structure-activity studies revealed the importance of the identity of the aromatic substituent at the C-2 position, particularly a phenyl, m-(amino) phenyl or m-(cyclohexylmethylpiperazinamide) phenyl substituent, for cytotoxic activity. PMID:20672155

  20. 1-Benzoyl-3-[3-cyano-8-methyl-4-(1-methyl-1H-pyrrol-2-yl-5,6,7,8-tetrahydroquinolin-2-yl]thiourea

    Abdullah M. Asiri

    2011-09-01

    Full Text Available In the N-substituted benzoylthiourea, C24H23N5OS, the benzoylthiourea unit is non-planar (r.m.s. deviation = 0.126 Å. The aliphatic part of the tetrahydroquinoline fused-ring system is disordered over two positions in a 0.592 (5:0.408 (5 ratio. The pyridine and pyrrole rings are twisted by 55.2 (1° in order to avoid crowding of their respective substituents. Pairs of molecules are linked by N—H...N hydrogen bonds, forming centrosymmetric dimers. Furthermore, an intramolecular N—H...O hydrogen bond stabilizes the molecular conformation.

  1. Enhanced open-circuit voltage in polymer solar cells by dithieno[3,2-b:2 ',3 '-d]pyrrole N-acylation

    Vanormelingen, Wouter; KESTERS, Jurgen; Verstappen, Pieter; DRIJKONINGEN, Jeroen; KUDRJASOVA, Julija; Koudjina, Simplice; Liegéois, Vincent; Champagne, Benoît; Manca, Jean; Lutsen, Laurence; Vanderzande, Dirk; Maes, Wouter

    2014-01-01

    A series of low bandgap copolymers composed of N-acyl-substituted dithieno[3,2-b:2′,3′-d]pyrroles (DTPs) as the electron rich donor constituents (with various alkyl side chain patterns) combined with different electron deficient acceptor building blocks are developed for polymer solar cell applications. Due to the introduction of the N-acyl substituents, the HOMO energy levels of the push–pull copolymers decrease as compared to the N-alkyl-DTP analogues, resulting in an increased open-circuit...

  2. Comparison of the resonance-enhanced multiphoton ionization spectra of pyrrole and 2,5-dimethylpyrrole: Building toward an understanding of the electronic structure and photochemistry of porphyrins

    Beames, Joseph M.; Nix, Michael G. D.; Hudson, Andrew J.

    2009-11-01

    The photophysical properties of porphyrins have relevance for their use as light-activated drugs in cancer treatment and sensitizers in solid-state solar cells. However, the appearance of their UV-visible spectra is usually explained inadequately by qualitative molecular-orbital theories. We intend to gain a better insight into the intense absorption bands, and excited-state dynamics, that make porphyrins appropriate for both of these applications by gradually building toward an understanding of the macrocyclic structure, starting with studies of smaller pyrrolic subunits. We have recorded the (1+1) and (2+1) resonance-enhanced multiphoton ionization (REMPI) spectra of pyrrole and 2,5-dimethylpyrrole between 25 600 cm-1 (390 nm) and 48 500 cm-1 (206 nm). We did not observe a (1+1) REMPI signal through the optically bright B12 (ππ ∗) and A11 (ππ ∗) states in pyrrole due to ultrafast deactivation via conical intersections with the dissociative A12 (πσ ∗) and B11 (πσ ∗) states. However, we did observe (2+1) REMPI through Rydberg states with a dominant feature at 27 432 cm-1 (two-photon energy, 54 864 cm-1) assigned to a 3d←π transition. In contrast, 2,5-dimethylpyrrole has a broad and structured (1+1) REMPI spectrum between 36 000 and 42 500 cm-1 as a result of vibronic transitions to the B12 (ππ ∗) state, and it does not show the 3d←π Rydberg transition via (2+1) REMPI. We have complemented the experimental studies by a theoretical treatment of the excited states of both molecules using time-dependent density functional theory (TD-DFT) and accounted for the contrasting features in the spectra. TD-DFT modeled the photochemical activity of both the optically dark π1σ∗ states (dissociative) and optically bright π1π∗ states well, predicting the barrierless deactivation of the B12 (ππ ∗) state of pyrrole and the bound minimum of the B12 (ππ ∗) state in 2,5-dimethylpyrrole. However, the quantitative agreement between vibronic

  3. Structural evaluation of tandem hairpin pyrrole-imidazole polyamides recognizing human telomeres.

    Hirata, Akiyoshi; Nokihara, Kiyoshi; Kawamoto, Yusuke; Bando, Toshikazu; Sasaki, Asuka; Ide, Satoru; Maeshima, Kazuhiro; Kasama, Takeshi; Sugiyama, Hiroshi

    2014-08-13

    A polyamide containing N-methylpyrrole (Py) and N-methylimidazole (Im), designated PIPA, binds with high affinity and specificity to specific nucleotide sequences in the minor groove of double-helical DNA. Based on a recent report of the synthesis of PIPA for telomere visualization, the present paper focused on the size of the connecting part (hinge region) of two PIPA segments of the tandem hairpin PIPA, Dab(Im-Im-Py)-Py-Py-Py-Im-[Hinge]-Dab(Im-Im-Py)-Py-Py-Py-Im-βAla-NH(CH2)3N(CH3)-(CH2)3NH-[Dye]. The present paper also describes the characterization of binding by measuring the thermal melting temperature and surface plasmon resonance and by specific staining of telomeres (TTAGGG)n in human cells. Microheterogeneity was also investigated by high-resolution mass spectrometry. We found that the optimal compound as the hinge segment for telomere staining was [-NH(C2H4O)2(C2H4)CO-] with tetramethylrhodamine as the fluorescent dye. PMID:25036716

  4. A DFT Study of Pyrrole-Isoxazole Derivatives as Chemosensors for Fluoride Anion

    Shanshan Tang

    2012-09-01

    Full Text Available The interactions between chemosensors, 3-amino-5-(4,5,6,7-tetrahydro-1H-indol-2-ylisoxazole-4-carboxamide (AIC derivatives, and different anions (F Cl, Br, AcO, and H2PO4 have been theoretically investigated using DFT approaches. It turned out that the unique selectivity of AIC derivatives for F is ascribed to their ability of deprotonating the host sensors. Frontier molecular orbital (FMO analyses have shown that the vertical electronic transitions of absorption and emission for the sensing signals are characterized as intramolecular charge transfer (ICT. The study of substituent effects suggests that all the substituted derivatives are expected to be promising candidates for fluoride chemosensors both in UV-vis and fluorescence spectra except for derivative with benzo[d]thieno[3,2-b]thiophene fragment that can serve as ratiometric fluorescent fluoride chemosensor only.

  5. Ferrocene-Functionalized 4-(2,5-Di(thiophen-2-yl)-1H-pyrrol-1-yl)aniline: A Novel Design in Conducting Polymer-Based Electrochemical Biosensors

    Rukiye Ayranci; Dilek Odaci Demirkol; Metin Ak; Suna Timur

    2015-01-01

    Herein, we report a novel ferrocenyldithiophosphonate functional conducting polymer and its use as an immobilization matrix in amperometric biosensor applications. Initially, 4-(2,5-di(thiophen-2-yl)-1H-pyrrol-1-yl)amidoferrocenyldithiophosphonate was synthesized and copolymerized with 4-(2,5-di(thiophen-2-yl)-1H-pyrrol-1-yl)benzenamine at graphite electrodes. The amino groups on the polymer were utilized for covalent attachment of the enzyme glucose oxidase. Besides, ferrocene on the backbon...

  6. Conjugated and fluorescent polymer based on dansyl-substituted pyrrole prepared by electrochemical polymerization in acetonitrile containing boron trifluoride diethyl etherate

    Graphical abstract: - Highlights: • A fluorescent pyrrole derivative bearing a dansyl substituent (PyPDG) was synthesized. • PyPDG was electropolymerized onto ITO in (C4H9)4NBF4/CH3CN/BFEE mixed electrolyte. • The resulting polymer (PPyPDG) films displayed electrochromic behavior. • PPyPDG is a good green light emitter material. - Abstract: A fluorescent pyrrole derivative bearing a dansyl substituent was prepared by a simple synthetic route and electropolymerized onto Indium Tin Oxide (ITO) electrodes. The presence of the dansyl group in the monomer precursor prevents the electropolymerization in usual systems, such as (C4H9)4NBF4 in acetonitrile (CH3CN). For this reason, it was added 20% boron trifluoride diethyl etherate (BFEE) to this system, to achieve electropolymerization. The resulting poly[3-(N-pyrrolyl)propyl dansylglycinate] (PPyPDG) films displayed electrochromic behavior. Their color varied from greenish-yellow, in the neutral state, to greyish-green, in the oxidized state; moreover PPyPDG is a good green light emitter material. Therefore, PPyPDG films might be potentially applicable in displays and optoelectronic devices

  7. Strikingly different luminescent properties arising from single crystals grown from solution or from the vapor phase in a diketo-pyrrolo-pyrrole analog

    Imoda, Tomohiko; Mizuguchi, Jin

    2007-10-01

    The title compound di-cyano-pyrrolo-pyrrole (DCPP) is an analog of diketo-pyrrolo-pyrrole (DPP) known as a red pigment on the market. Brilliant orange photoluminescence has been observed in crystals of DCPP recrystallized from solution (crystal I); whereas the luminescence was quite weak in single crystals grown from the vapor phase (crystal II). To elucidate the difference in luminescent properties, a series of structural analysis together with thermal analysis has been carried out on crystals I and II at -180 °C, RT, 150 °C, and 200 °C. However, no difference in structure is recognized between crystals I and II within the precision of the x-ray analysis. Nevertheless, a slight difference in sublimation temperature of about 5° is observed between crystals I and II. Since the sublimation temperature depends on the cohesion in the solid state and the cohesion, in turn, governs the extent of lattice vibration (i.e., nonradiative process), a slight difference in sublimation temperature appears to determine the fraction between the radiative and nonradiative processes in crystals I and II.

  8. High content of pyridinic- and pyrrolic-nitrogen-modified carbon nanotubes derived from blood biomass for the electrocatalysis of oxygen reduction reaction in alkaline medium

    Graphical abstract: Display Omitted -- Highlights: •An ORR electrocatalyst was fabricated from blood biomass and carbon nanotube. •The N-CNT catalyst exhibits good ORR activity, methanol resistance and stability. •The pyrolysis process produces high contents of pyridinic and pyrrolic N species. •The pyridinic-N group may play more important role in the active sites for ORR. -- Abstract: Here we present a facile synthetic route to design nitrogen-doped nanostructured carbon-based electrocatalyst for oxygen reduction reaction (ORR) by the copyrolysis of blood biomass from pig and carbon nanotubes (CNTs) at high temperatures. The nitrogen-doped CNTs obtained at 800 °C not only results in excellent ORR activity with four-electron transfer selectivity in alkaline medium, but also exhibits superior methanol-tolerant property and long-term stability. It is confirmed that high-temperature pyrolysis processes can facilitate to produce higher contents of pyridinic- and pyrrolic-N binding groups in electrocatalysts, contributing to the enhancement of ORR performance in terms of onset potential, half-wave potential, and limited current density. We also propose that the planar-N configuration may be the active site that is responsible for the improved ORR electrocatalytic performance. The straight-forward and cheap synthesis of the active and stable electrocatalyst makes it a promising candidate for electrochemical power sources such as fuel cells or metal-air batteries

  9. Catalytic mechanisms of direct pyrrole synthesis via dehydrogenative coupling mediated by PNP-Ir or PNN-Ru pincer complexes: Crucial role of proton-transfer shuttles in the PNP-Ir system

    Qu, Shuanglin

    2014-04-02

    Kempe et al. and Milstein et al. have recently advanced the dehydrogenative coupling methodology to synthesize pyrroles from secondary alcohols (e.g., 3) and β-amino alcohols (e.g., 4), using PNP-Ir (1) and PNN-Ru (2) pincer complexes, respectively. We herein present a DFT study to characterize the catalytic mechanism of these reactions. After precatalyst activation to give active 1A/2A, the transformation proceeds via four stages: 1A/2A-catalyzed alcohol (3) dehydrogenation to give ketone (11), base-facilitated C-N coupling of 11 and 4 to form an imine-alcohol intermediate (18), base-promoted cyclization of 18, and catalyst regeneration via H2 release from 1R/2R. For alcohol dehydrogenations, the bifunctional double hydrogen-transfer pathway is more favorable than that via β-hydride elimination. Generally, proton-transfer (H-transfer) shuttles facilitate various H-transfer processes in both systems. Notwithstanding, H-transfer shuttles play a much more crucial role in the PNP-Ir system than in the PNN-Ru system. Without H-transfer shuttles, the key barriers up to 45.9 kcal/mol in PNP-Ir system are too high to be accessible, while the corresponding barriers (<32.0 kcal/mol) in PNN-Ru system are not unreachable. Another significant difference between the two systems is that the addition of alcohol to 1A giving an alkoxo complex is endergonic by 8.1 kcal/mol, whereas the addition to 2A is exergonic by 8.9 kcal/mol. The thermodynamic difference could be the main reason for PNP-Ir system requiring lower catalyst loading than the PNN-Ru system. We discuss how the differences are resulted in terms of electronic and geometric structures of the catalysts and how to use the features in catalyst development. © 2014 American Chemical Society.

  10. Alternating copolymers of cyclopenta[2,1-b;3,4-b']dithiophene and Thieno[3,4-c]pyrrole-4,6-dione for high-performance polymer solar cells

    Li, Zhao; Du, Xiaomei; Scoles, Ludmila; Robertson, Gilles; Toll, Floyd; Ding, Jianfu [Institute for Chemical Process and Environmental Technology (ICPET), National Research Council of Canada (NRC), Ottawa, ON (Canada); Tsang, Sai-Wing; Zhang, Yanguang; Tao, Ye; Lu, Jianping [Institute for Microstructural Sciences (IMS), National Research Council of Canada (NRC), Ottawa, ON (Canada)

    2011-09-09

    A series of alternating copolymers of cyclopenta[2,1-b;3,4-b']dithiophene (CPDT) and thieno[3,4-c]pyrrole-4,6-dione (TPD) have been prepared and characterized for polymer solar cell (PSC) applications. Different alkyl side chains, including butyl (Bu), hexyl (He), octyl (Oc), and 2-ethylhexyl (EH), are introduced to the TPD unit in order to adjust the packing of the polymer chain in the solid state, while the hexyl side chain on the CPDT unit remains unchanged to simplify discussion. The polymers in this series have a simple main chain structure and can be synthesized easily, have a narrow band gap and a broad light absorption. The different alkyl chains on the TPD unit not only significantly influence the solubility and chain packing, but also fine tune the energy levels of the polymers. The polymers with Oc or EH group have lower HOMO (highest occupied molecular orbital) and LUMO (lowest unoccupied molecular orbital) energy levels, resulting higher open circuit voltages (V{sub oc}) of the PSC devices. Power conversion efficiencies (PCEs) up to 5.5% and 6.4% are obtained from the devices of the Oc substituted polymer (PCPDTTPD-Oc) with PC{sub 61}BM and PC{sub 71}BM, respectively. This side chain effect on the PSC performance is related to the formation of a fine bulk heterojunction structure of polymer and PCBM domains, as observed with atomic force microscopy. (Copyright copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  11. Synthesis, characterization and conductivity studies of polypyrrole–fly ash composites

    M V Murugendrappa; Syed Khasim; M V N Ambika Prasad

    2005-10-01

    in situ polymerization of pyrrole was carried out in the presence of fly ash (FA) to synthesize polypyrrole–fly ash composites (PPy/FA) by chemical oxidation method. The PPy/FA composites have been synthesized with various compositions (10, 20, 30, 40 and 50 wt%) of fly ash in pyrrole. The surface morphology of these composites was studied with scanning electron micrograph (SEM). The polypyrrole–fly ash composites were also characterized by employing X-ray diffractometry (XRD) and infrared spectroscopy (IR). The a.c. conductivity behaviour has been investigated in the frequency range 102–106 Hz. The d.c. conductivity was studied in the temperature range from 40–200°C. The dimensions of fly ash in the matrix have a greater influence on the observed conductivity values. The results obtained for these composites are of greater scientific and technological interest.

  12. Schiff base functionalized Organopropylsilatranes: Synthesis and structural characterization

    Gurjaspreet Singh; Promila; Amandeep Saroa; Jandeep Singh; Raj Pal Sharm; V Ferretti

    2016-02-01

    Synthesis of Schiff bases linked to organopropylsilatranes were performed by condensation reaction of post-functionalized silatranes such as aminopropylsilatrane (4), aminopropyl-3,7,10-trimethylsilatrane (5) and N-substituted aminopropylsilatrane (10) with two different aldehydes viz. pyrrole-2-carboxaldehyde and 2-hydroxy-1-napthaldehyde. The resulting Schiff base substituted silatranes were well characterized by elemental analysis, spectroscopic studies [IR, (1H, 13C) NMR, and MS]. The structures of two silatranes were confirmed by single crystal X-ray diffraction analysis.

  13. Emission and absorption of light in poly pyrrole synthesized by plasma; Emision y absorcion de luz en polipirrol sintetizado por plasma

    Enriquez, M.A.; Colin, E.; Olayo, M.G.; Cruz, G.J.; Ordonez, E. [ININ, A.P. 18-1027, 11801 Mexico D.F. (Mexico); Benavides, R. [Departamento de Procesos de Transformacion, CIQA, Blvd. Enrique Reyna 140, Saltillo, Coahuila (Mexico); Morales, J.; Olayo, R. [UAM-I, Apdo. Postal 55-534, Iztapalapa, D.F. (Mexico)]. e-mail: gcc@nuclear.inin.mx

    2007-07-01

    The poly pyrrole structure (PPy) consists of heterocyclic rings with conjugation that it depends on the intensity of the electric field applied during the synthesis, and its luminescence is related with the {pi}-{pi}{sup *} transitions of that conjugation. To irradiate with light of different wavelengths, the results indicate that the polymer absorbs in the interval from 290 to 700 nm and it emits between 450 and 470 nm. The basal conductivity of the polymers, without electromagnetic excitation, it was measured in 10{sup -15} S/cm, however, to interact with visible light it is increased approximately 10 times and when excite with UV light it is increased up to 3 magnitude orders. (Author)

  14. Cation Recognition: Novel Potentiometric PVC-Membrane Sensor based on Meso-octamethylcalix[4]pyrrole for the Determination of Trace Amounts of Titanium (III) Ions

    The present work deals with developing a novel high selective membrane electrode based on meso-octamethylcalix[4]pyrrole for accurate determination of trace amount of titanium (III) ions in real sample solutions. The amounts of ionophore (4 mg), PVC (33 mg), dioctyl phthalate (DOP) as plasticizer (62.8 mg) and sodium tetrakis [3,5-bis (trifluoromethyl) phenyl] borate (NaTFPB) as an ionic additive (0.2 mg) were optimized in the preparation of the membrane. The electrode exhibited a linear response with a near Nernstian slope of 29.49±0.16 (mV per decade of activity) over the pH range from 1 to 3 with a satisfactory concentration range of 1.0 x 10-6 to 1.0 x x10-2 M. The developed sensor exhibited good reproducibility over a period of about 3 months with a fast response time of 15 seconds. (author)

  15. Effects of Molecular Structure on Intramolecular Charge Carrier Transport in Dithieno [3,2-b: 2,3-d] Pyrrole-Based Conjugated Copolymers

    Yoshihito Honsho

    2012-01-01

    Full Text Available Intramolecular mobility of positive charge carriers in conjugated polymer films based on dithieno [2,3-b: 2,3-d] pyrrole (DTP is studied by time-resolved microwave conductivity (TRMC. A series of DTP homopolymer and copolymers combined with phenyl, 2,2-biphenyl, thiophene, 2,2-bithiophene, and 9,9-dioctylfluorene were synthesized by Suzuki-Miyaura and Yamamoto coupling reactions. Polymers containing DTP unit are reported to show high value of hole mobility measured by FET method, and this type of polymers is expected to have stable HOMO orbitals which are important for hole transportation. Among these copolymers, DTP coupled with 9,9-dioctylfluorene copolymer showed the highest charge carrier mobility as high as 1.7 cm2/Vs, demonstrating an excellent electrical property on rigid copolymer backbones.

  16. Gamma irradiation effect on polymers derived of pyrrole synthesized by plasma; Efecto de irradiacion gamma en polimeros derivados de pirrol sintetizados por plasma

    Lopez G, O. G.

    2013-07-01

    This work studies the effect of gamma irradiation at doses of 50, 100, 200, 400 and 800 kGy on polymers obtained from pyrrole synthesized by plasma. The evolution of the structure was studied by Fourier transform infrared spectroscopy (Ftir) and X-ray photoelectron spectroscopy (XPS). The Ftir spectra show that poly pyrroles have N-H, C-H, C=O, triple and consecutive double bonds in their structure. The irradiated polymers show the same chemical groups in their structure without significant changes. Nevertheless, a more detailed analysis by XPS allows the identification of superficial chemical states, such as: C=CH-C, C=CC-C, C-NH-C, C-NC-C, etc., and shows that most of these states are present in all polymers but with different participation. One possible mechanism indicates that as the irradiation dose increases, dehydrogenation processes are performed increasing fragmentation, crosslinking and formation of multiple bonds. The fragmentation and thermal degradation were studied by thermogravimetric analysis, indicating that the loss of moisture and light compounds formed during gamma irradiation occurs in the firsts 100 grades C. The main degradation of all polymers occurs from 150 to 700 grades C, suggesting that the thermal stability is independent of the irradiation dose in the interval studied. Morphology was studied using scanning electron microscopy techniques. Before irradiation, the polymer presented a uniform and practically smooth surface, however, after gamma irradiation, the applied energy increased roughness and macro fragmentation. The roughness and functional groups on the surface reduced the contact angle with water as the irradiation dose increased. However, the polymers are hydrophilic, because for all doses that contact angle is smaller than 90 grades C. Electrical conductivity was calculated respect to temperature in the interval from 25 to 100 grades C. Conductivity increases with temperature and is slightly greater in the irradiated polymers

  17. Anticancer potential of pyrrole (1, 2, a) pyrazine 1, 4, dione, hexahydro 3-(2-methyl propyl) (PPDHMP) extracted from a new marine bacterium, Staphylococcus sp. strain MB30.

    Lalitha, P; Veena, V; Vidhyapriya, P; Lakshmi, Pragna; Krishna, R; Sakthivel, N

    2016-05-01

    Marine bacterium, strain MB30 isolated from the deep sea sediment of Bay of Bengal, India, exhibited antimicrobial activity against human pathogenic bacteria. Based on the 16S rRNA sequence homology and subsequent phylogenetic tree analysis, the strain MB30 was identified as Staphylococcus sp. The bioactive metabolite produced by the strain MB30 was purified through silica gel column chromatography and preparative HPLC. Purified metabolite was further characterized by FT-IR, LC-MS and NMR analyses. On the basis of spectroscopic data, the metabolite was identified as pyrrole (1, 2, a) pyrazine 1, 4, dione, hexahydro 3-(2-methyl propyl) (PPDHMP). The PPDHMP exhibited in vitro anticancer potential against lung (A549) and cervical (HeLa) cancer cells in a dose-dependent manner with the IC50 concentration of 19.94 ± 1.23 and 16.73 ± 1.78 μg ml(-1) respectively. The acridine orange (AO)/ethidium bromide (EB) and 4,6-diamidino-2-phenylindole dihydrochloride (DAPI) staining of the IC50 concentration of PPDHMP-treated cancer cells exhibited an array of morphological changes such as nuclear condensation, cell shrinkage and formation of apoptotic bodies. The PPDHMP-treated cancer cells induced the progressive accumulation of fragmented DNA in a time-dependent manner. Based on the flow cytometric analysis, it has become evident that the compound was also effective in arresting the cell cycle at G1 phase. Further, the Western blotting analysis confirmed the down-regulation of cyclin-D1, cyclin dependent kinase (CDK-2), anti-apoptotic Bcl-2 family proteins (Bcl-2 and Bcl-xL), activation of caspase-9 and 3 with the cleavage of PARP. The PPDHMP-treated cancer cells also showed the inhibition of migration and invasive capacity of cancer cells. In the present investigation, for the first time, we have reported the extraction, purification and characterization of an anticancer metabolite, PPDHMP from a new marine bacterium, Staphylococcus sp. strain MB30. PMID:26852140

  18. A convenient method for 14C-labeling of N-(2-oxo-5-phenyl-2,3-dihydro-1H-benzo[e] [1,4]diazepin-3-yl)-1H-pyrrole-2-carboxamide-[carboxy-14C] as CCK-A antagonist

    N-(2-oxo-5-phenyl-2,3-dihydro-1H-benzo[e] [1,4]diazepin-3-yl)-1H-pyrrole-2-carboxamide-[carboxy-14C] was prepared as part of a five-step sequence from pyrrol-2-carbonitrile-[cyano-14C] as a key synthetic intermediate which has been synthesized from 2-bromopyrrole and zinc [14C]-cyanide in the presence of tetrakis (triphenylphosphine)palladium. (author)

  19. Characterization of acid tars

    Acid tars from the processing of petroleum and petrochemicals using sulfuric acid were characterized by gas chromatography/mass spectrometry (GC/MS), inductively coupled plasma/optical emission spectrometry (ICP/OES), differential scanning calorimetry (DSC), Fourier transform infrared (FTIR) spectrometry, and scanning electron microscopy/energy dispersive X-ray (SEM/EDX) micro-analysis. Leaching of contaminants from the acid tars in 48 h batch tests with distilled water at a liquid-to-solid ratio 10:1 was also studied. GC/MS results show that the samples contained aliphatic hydrocarbons, cyclic hydrocarbons, up to 12 of the 16 USEPA priority polycyclic aromatic hydrocarbons (PAHs), and numerous other organic groups, including organic acids (sulfonic acids, carboxylic acids and aromatic acids), phenyl, nitrile, amide, furans, thiophenes, pyrroles, and phthalates, many of which are toxic. Metals analysis shows that Pb was present in significant concentration. DSC results show different transition peaks in the studied samples, demonstrating their complexity and variability. FTIR analysis further confirmed the presence of the organic groups detected by GC/MS. The SEM/EDX micro-analysis results provided insight on the surface characteristics of the samples and show that contaminants distribution was heterogeneous. The results provide useful data on the composition, complexity, and variability of acid tars; information which hitherto have been scarce in public domain.

  20. Biocatalytic ammonolysis of (5S)-4,5-dihydro-1H-pyrrole-1,5-dicarboxylic acid, 1-(1,1-dimethylethyl)-5-ethyl ester: preparation of an intermediate to the dipeptidyl peptidase IV inhibitor Saxagliptin.

    Gill, Iqbal; Patel, Ramesh

    2006-02-01

    An efficient biocatalytic method has been developed for the conversion of (5S)-4,5-dihydro-1H-pyrrole-1,5-dicarboxylic acid, 1-(1,1-dimethylethyl)-5-ethyl ester (1) into the corresponding amide (5S)-5-aminocarbonyl-4,5-dihydro-1H-pyrrole-1-carboxylic acid, 1-(1,1-dimethylethyl)ester (2), which is a critical intermediate in the synthesis of the dipeptidyl peptidase IV (DPP4) inhibitor Saxagliptin (3). Candida antartica lipase B mediates ammonolysis of the ester with ammonium carbamate as ammonia donor to yield up to 71% of the amide. The inclusion of Ascarite and calcium chloride as adsorbents for carbon dioxide and ethanol byproducts, respectively, increases the yield to 98%, thereby offering an efficient and practical alternative to chemical routes which yield 57-64%. PMID:16257208

  1. Electronic, Spectral, and Electrochemical Properties of (TPPBr(x)())Zn Where TPPBr(x)() Is the Dianion of beta-Brominated-Pyrrole Tetraphenylporphyrin and x Varies from 0 to 8.

    D'Souza, Francis; Zandler, Melvin E.; Tagliatesta, Pietro; Ou, Zhongping; Shao, Jianguo; Van Caemelbecke, Eric; Kadish, Karl M.

    1998-09-01

    The electronic, spectral, and electrochemical characterization of (meso-tetraphenylporphyrinato)zinc(II) complexes bearing between 0 and 8 bromo substituents at the beta-pyrrole positions is reported. The investigated compounds are represented as (TPPBr(x)())Zn where TPPBr(x)() is the dianion of brominated 5,10,15,20-tetraphenylporphyrin and x varies between 0 and 8. Each porphyrin undergoes four well-defined one-electron transfer reactions to yield porphyrin pi-cation radicals and dications upon oxidation and porphyrin pi-anion radicals and dianions upon reduction. Half-wave potentials for the first reduction of (TPPBr(x)())Zn can be described by a single linear free energy relationship, and plots of E(1/2) versus the number of Br groups on the complex show a linear correlation with a positive slope of 63 mV per Br group. This is not the case for the other three electron transfer processes of the compounds where plots of E(1/2) versus the number of Br groups show distinctly different linear correlations for derivatives with 0-4 Br groups and those with 4-8 Br groups. The effect of increasing number of Br groups on the spectral and electrochemical properties of the neutral complexes was examined over the whole series of compounds, and these experimental results are compared to results of theoretical calculations by semiempirical molecular orbital AM1 methods using configurational interactions (CI) over the four Gouterman frontier pi-orbitals. The dihedral angle containing the four porphyrin macrocycle ring nitrogens is proposed as a measure of porphyrin ring nonplanarity, and this value increases with increasing number of Br substituents on (TPPBr(x)())Zn. Results of the AM1-CI = 4 calculations indicate that the spectrally determined HOMO-LUMO gap, i.e., the energy corresponding to the low-energy absorption band, varies in a nonlinear fashion with increasing number of Br substituents on the macrocycle and this is due to both the electronic effect of the

  2. 4-Hydroxy-7-oxo-5-heptenoic Acid (HOHA) Lactone is a Biologically Active Precursor for the Generation of 2-(ω-Carboxyethyl)pyrrole (CEP) Derivatives of Proteins and Ethanolamine Phospholipids

    Hua WANG; Linetsky, Mikhail; Guo, Junhong; Choi, Jaewoo; Hong, Li; Chamberlain, Amanda S.; Howell, Scott J.; Howes, Andrew M.; Robert G Salomon

    2015-01-01

    2-(ω-Carboxyethyl)pyrrole (CEP) derivatives of proteins were previously shown to have significant pathological and physiological relevance to age-related macular degeneration, cancer and wound healing. Previously, we showed that CEPs are generated in the reaction of ε-amino groups of protein lysyl residues with 1-palmityl-2-(4-hydroxy-7-oxo-5-heptenoyl)-sn-glycero-3-phosphatidylcholine (HOHA-PC), a lipid oxidation product uniquely generated by oxidative truncation of doco...

  3. A highly efficient group-assisted purification method for the synthesis of poly-functionalized pyrimidin-5-yl-pyrroles via one-pot four-component domino reaction.

    Dommaraju, Yuvaraj; Prajapati, Dipak

    2015-02-01

    A highly efficient, catalyst-free group-assisted purification chemical protocol for the construction of pyrimidine containing poly-functionalized pyrroles from a four-component domino reaction of acyclic-1,3-dicarbonyls or electron deficient alkynes, aromatic amines, barbituric acid and arylglyoxal hydrates under mild reaction conditions has been developed. The prominent features of the present protocol are environmentally benign, mild reaction conditions, atom economy, no column chromatography separation, easy isolation of products and excellent yields. PMID:25173493

  4. Thieno[3,2-b]- and thieno[2,3-b]pyrrole bioisosteric analogues of the hallucinogen and serotonin agonist N,N-dimethyltryptamine.

    Blair, J B; Marona-Lewicka, D; Kanthasamy, A; Lucaites, V L; Nelson, D L; Nichols, D E

    1999-03-25

    The synthesis and biological activity of 6-[2-(N, N-dimethylamino)ethyl]-4H-thieno[3,2-b]pyrrole (3a) and 4-[2-(N, N-dimethylamino)ethyl]-6H-thieno[2,3-b]pyrrole (3b), thienopyrroles as potential bioisosteres of N,N-dimethyltryptamine (1a), are reported. Hallucinogen-like activity was evaluated in the two-lever drug discrimination paradigm using LSD- and DOI-trained rats. Neither 3a nor 3b substituted for LSD or DOI up to doses of 50 micromol/kg. By comparison, 1a fully substituted in LSD-trained rats. However, 3a and 3b fully substituted for the 5-HT1A agonist LY293284 ((-)-(4R)-6-acetyl-4-(di-n-propylamino)-1,3,4, 5-tetrahydrobenz[c,d]indole). Both 3a and 3b induced a brief "serotonin syndrome" and salivation, an indication of 5-HT1A receptor activation. At the cloned human 5-HT2A receptor 3b had about twice the affinity of 3a. At the cloned human 5-HT2B and 5-HT2C receptors, however, 3a had about twice the affinity of 3b. Therefore, thiophene lacks equivalence as a replacement for the phenyl ring in the indole nucleus of tryptamines that bind to 5-HT2 receptor subtypes and possess LSD-like behavioral effects. Whereas both of the thienopyrroles had lower affinity than the corresponding 1a at 5-HT2 receptors, 3a and 3b had significantly greater affinity than 1a at the 5-HT1A receptor. Thus, thienopyrrole does appear to serve as a potent bioisostere for the indole nucleus in compounds that bind to the serotonin 5-HT1A receptor. These differences in biological activity suggest that serotonin receptor isoforms are very sensitive to subtle changes in the electronic character of the aromatic systems of indole compounds. PMID:10090793

  5. Pyrrole and 2,5-heptanedione in the urine of rats and 2,5-heptanedione in the urine of man: analytical determination of excretion upon exposure to n-heptane; Pyrrole und 2,5-Heptandion im Urin der Ratte und 2,5-Heptandion im Urin des Menschen: Analytische Bestimmung der Ausscheidung nach Exposition gegn n-Heptan

    Stoermer, A.G.C.

    1997-09-01

    A method for quantifying levels of the neurotoxic metabolite 2,5-heptanedione in rats and man after experimental exposure to n-heptane was developed. It consisted in determining the quantity of 2,5-heptanedione excreted in urine and the relevant excretion kinetics. Moreover, the excretion of pyrrole in the urine of rats was measured. In the urine of non-exposed rats and man, a basic excretion of 2,5-heptanedione was measured, with the rates of excretion being 0.11 and 4.5 nmol per hour, respectively. This basic excretion of 2,5-heptanedione is assumed to have an endogenous cause. The quantitive investigation of the dose dependence of the excretion of 2,5-heptanedione and pyrrole in the urine of rats and of 2,5-heptanedione in the urine of man is a prerequisite for assessing the risk posed by n-heptane with a view to peripheral neuropathies. (orig./MG) [Deutsch] Ziel dieser Arbeit war die Entwicklung einer Methode zur Quantifizierung der Belastung von Ratte und Mensch mit dem neurotoxischen Metaboliten 2,5-Heptandion nach experimentellen Expositionen gegen n-Heptan. Dazu sollte jeweils die ausgeschiedene Menge und die zugehoerige Ausscheidungskinetik von 2,5-Heptandion im Urin bestimmt werden. Darueber hinaus sollte die Ausscheidung von Pyrrolen im Urin von Ratten gemessen werden. Im Urin von nicht exponierten Ratten und Menschen wurde eine Grundausscheidung von 2,5-Heptandion gefunden, wobei die Ausscheidungsraten jeweils 0,11 bzw. 4,5 nmol/h betrugen. Fuer die Grundausscheidung von 2,5-Heptandion wird ein endogener Ursprung angenommen. Die quantitativen Untersuchungen zur Dosisabhaengigkeit der Ausscheidung im Urin von 2,5-Heptandion und Pyrrolen bei der Ratte und von 2,5-Heptandion beim Menschen sind eine Grundvoraussetzung fuer eine Abschaetzung des Risikos von n-Heptan fuer periphere Neuropathien. (orig./MG)

  6. Scientific Opinion on Flavouring Group Evaluation 77, Revision 1 (FGE.77Rev1: Consideration of Pyridine, Pyrrole and Quinoline Derivatives evaluated by JECFA (63rd meeting structurally related to Pyridine, Pyrrole, Indole and Quinoline Derivatives evaluated by EFSA in FGE.24Rev2 (2013

    EFSA Panel on Food Contact Materials, Enzymes, Flavourings and Processing Aids (CEF

    2014-02-01

    Full Text Available The Panel on Food Contact Materials, Enzymes, Flavourings and Processing Aids of the European Food Safety Authority was requested to consider evaluations of flavouring substances assessed since 2000 by the Joint FAO/WHO Expert Committee on Food Additives (the JECFA, and to decide whether further evaluation is necessary, as laid down in Commission Regulation (EC No 1565/2000. The present consideration concerns a group of 22 pyridine, pyrrole and quinoline derivatives evaluated by the JECFA (63rd meeting. The revision of this consideration is made since additional toxicity data have become available for isoquinoline [FL-no: 14.001], pyrrole [FL-no: 14.041] and 2-acetylpyrrole [FL-no: 14.047]. The toxicity data on 2-acetylpyrrole should also cover 2-propionylpyrrole [FL-no: 14.068]. Further, additional genotoxicity data on 6-methylquinoline [FL-no: 14.042] have become available. The Panel concluded that for 6-methylquinoline [FL-no: 14.042], the new genotoxicity data did not clear the concern with respect to genotoxicity in vitro and accordingly the substance is not evaluated through the Procedure. For 18 substances [FL-no: 14.001, 14.004, 14.007, 14.030, 14.038, 14.039, 14.041, 14.047, 14.058, 14.059, 14.060, 14.061, 14.065, 14.066, 14.068, 14.071, 14.072 and 14.164] considered in this FGE, the Panel agrees with the JECFA conclusion, “No safety concern at estimated levels of intake as flavouring substances” based on the MSDI approach. For three substances [FL-no: 13.134, 14.045 and 14.046], additional toxicological data are still required. Besides the safety assessment of these flavouring substances, the specifications for the materials of commerce have also been evaluated, and the information is considered adequate for all the substances.

  7. Fe nanoparticle tailored poly(N-methyl pyrrole) nanowire matrix: a CHEMFET study from the perspective of discrimination among electron donating analytes

    Back-gated chemically sensitive field effect transistor (CHEMFET) platforms have been developed with electrochemically synthesized poly(N-methyl pyrrole) nanowires by a templateless route. The nanowire matrix has been tailored with Fe nanoparticles to probe their effect in enhancing the sensing capabilities of the nanowire platform, and further to see if the inculcation of Fe nanoparticles is helpful to enhance the screening capability of the sensor among electron donating analytes. A noticeable difference in the sensing behaviour of the CHEMFET sensor was observed when it was exposed to three different analytes—ammonia, phosphine and carbon monoxide. FET transfer characteristics were instrumental in the corroboration of the experimental validations. The observations have been rationalized considering the simultaneous modulation of the work functions of Fe and polymeric material. The real time behaviour of the sensor shows that the sensor platform is readily capable of sensing the validated analytes at a ppb level of concentration with good response and recovery behaviour. The best response could be observed for ammonia with an Fe nanoparticle tailored polymeric matrix, with a sensitivity of ∼31.58% and excellent linearity (R2 = 0.985) in a concentration window of 0.05 ppm to 1 ppm. (paper)

  8. [Determination of ten pesticides of pyrazoles and pyrroles in tea by accelerated solvent extraction coupled with gas chromatography-tandem mass spectrometry].

    Xu, Dunming; Lu, Shengyu; Chen, Dajie; Lan, Jinchang; Zhang, Zhigang; Yang, Fang; Zhou, Yu

    2013-03-01

    An effective method was developed and applied to determine the residues of ten pesticides of pyrazoles and pyrroles in tea by accelerated solvent extraction coupled with gas chromatography-tandem mass spectrometry (ASE-GC-MS/MS). The samples were extracted with ethyl acetate-hexane (1:1, v/v) for 5 min at 1.03 x 10(7) Pa and 100 degree C for one cycle. Then, they were purified by Envi-Carb/PSA column, and eluted by ethyl acetate-hexane (1:1, v/v). The analytes were determined by GC-MS/MS and quantified by external standard method. The limits of quantification were 0.003 mg/kg for fenpyroximate, 0.001 mg/kg for fipronil-sulfide, 0.002 mg/kg for fipronil, 0.005 mg/kg for fipronil-sulfone, 0.002 mg/kg for chlorfenapyr, 0.006 mg/kg for flusilazole, 0.001 mg/kg for difenzoquat, 0.001 mg/kg for pyraflufen-ethyl, 0.000 3 mg/kg for tebufenpyrad and 0.005 mg/kg for tolfenpyrad. The results show that the proposed method is sensitive and accurate for the determination of the ten pesticide residues. PMID:23785993

  9. Photocatalytic Degradation of Eosin Yellow Using Poly(pyrrole-co-aniline-Coated TiO2/Nanocellulose Composite under Solar Light Irradiation

    T. S. Anirudhan

    2015-01-01

    Full Text Available The present study describes the feasibility of a novel adsorbent cum photocatalyst, poly(pyrrole-co-aniline-coated TiO2/nanocellulose composite (P(Py-co-An-TiO2/NCC, to remove eosin yellow (EY from aqueous solutions. The removal of EY was investigated by batch adsorption followed by photocatalysis. The effect of various adsorption parameters like adsorbent dose, pH, contact time, initial concentration, and ionic strength has been optimized for treating effluents from the dye industry. Adsorption of EY reached maximum at pH 4.5 and complete removal of dye was achieved using 3.5 g/L of P(Py-co-An-TiO2/NCC. Adsorption equilibrium data were fitted with Langmuir and Fritz-Schlunder isotherm models and the kinetics of adsorption follows a second-order mechanism. The adsorption capacity of P(Py-co-An-TiO2/NCC was found to be 3.39 × 10−5 mol/g and reached equilibrium within 90 min. The photocatalytic degradation of adsorbed dye under sunlight was possible and about 92.3% of dye was degraded within 90 min. The reusability of P(Py-co-An-TiO2/NCC was also investigated. The results indicate that P(Py-co-An-TiO2/NCC is the best material for the wiping out of EY from aqueous solutions.

  10. Pyrrole-Terminated Ionic Liquid Surfactant: One Molecule with Multiple Functions for Controlled Synthesis of Diverse Multispecies Co-Doped Porous Hollow Carbon Spheres.

    Li, Jian; Zhu, Wei; Ji, Jingwei; Wang, Peng; Lan, Yue; Gao, Ning; Yin, Xianpeng; Wang, Hui; Li, Guangtao

    2016-05-01

    Rationally and efficiently controlling chemical composition, microstructure, and morphology of carbon nanomaterials plays a crucial role in significantly enhancing their functional properties and expending their applications. In this work, a novel strategy for simultaneously controlling these structural parameters was developed on the base of a multifunctional precursor approach, in which the precursor not only serves as carbon source and structure-directing agent, but also contains two heteroatom doping sites. As exemplified by using pyrrole-terminated ionic liquid surfactant as such precursor, in conjunction with sol-gel chemistry this strategy allows for efficiently producing well-defined hollow carbon spheres with controlled microstructure and chemical compositions. Remarkably, the dual-doping sites in confined silica channels provide an exciting opportunity and flexibility to access various doped carbons through simply anion exchange or altering the used oxidative polymerization agent, especially the multispecies codoped materials by combination of the two doping modes. All the results indicate that the described strategy may open up a new avenue for efficiently synthesizing functional carbon materials with highly controllable capability. PMID:27093191

  11. ToF-SIMS Characterization of Silk Fibroin and Polypyrrole Composite Actuators

    Bradshaw, Nathan P.; Severt, Sean Y.; Wang, Zhaoying; Fengel, Carly V.; Larson, Jesse D.; Zhu, Zihua; Murphy, Amanda; Leger, Janelle M.

    2015-08-31

    Biocompatible materials capable of controlled actuation under biologically relevant conditions are in high demand for use in a number of biomedical applications. Recently, we demonstrated that a composite material composed of silk biopolymer and the conducting polymer poly(pyrrole) can bend under an applied voltage using a simple bilayer device. Here we present further characterization of these bilayer actuators using time of flight secondary ion mass spectrometry, and provide clarification on the mechanism of actuation and factors affecting device performance and stability. We will discuss the results of this study in the context of strategies for optimization of device performance.

  12. Monocrotaline pyrrole-induced megalocytosis of lung and breast epithelial cells: Disruption of plasma membrane and Golgi dynamics and an enhanced unfolded protein response

    The pyrrolizidine alkaloid monocrotaline (MCT) initiates pulmonary hypertension by inducing a 'megalocytosis' phenotype in target pulmonary arterial endothelial, smooth muscle and Type II alveolar epithelial cells. In cultured endothelial cells, a single exposure to the pyrrolic derivative of monocrotaline (MCTP) results in large cells with enlarged endoplasmic reticulum (ER) and Golgi and increased vacuoles. However, these cells fail to enter mitosis. Largely based upon data from endothelial cells, we proposed earlier that a disruption of the trafficking and mitosis-sensor functions of the Golgi (the 'Golgi blockade' hypothesis) may represent the subcellular mechanism leading to MCTP-induced megalocytosis. In the present study, we investigated the applicability of the Golgi blockade hypothesis to epithelial cells. MCTP induced marked megalocytosis in cultures of lung A549 and breast MCF-7 cells. This was associated with a change in the distribution of the cis-Golgi scaffolding protein GM130 from a discrete juxtanuclear localization to a circumnuclear distribution consistent with an anterograde block of GM130 trafficking to/through the Golgi. There was also a loss of plasma membrane caveolin-1 and E-cadherin, cortical actin together with a circumnuclear accumulation of clathrin heavy chain (CHC) and α-tubulin. Flotation analyses revealed losses/alterations in the association of caveolin-1, E-cadherin and CHC with raft microdomains. Moreover, megalocytosis was accompanied by an enhanced unfolded protein response (UPR) as evidenced by nuclear translocation of Ire1α and glucose regulated protein 58 (GRP58/ER-60/ERp57) and a circumnuclear accumulation of PERK kinase and protein disulfide isomerase (PDI). These data further support the hypothesis that an MCTP-induced Golgi blockade and enhanced UPR may represent the subcellular mechanism leading to enlargement of ER and Golgi and subsequent megalocytosis

  13. Marked Consequences of Systematic Oligothiophene Catenation in Thieno[3,4-c]pyrrole-4,6-dione and Bithiopheneimide Photovoltaic Copolymers

    Zhou, Nanjia; Guo, Xugang; Ponce Ortiz, Rocio; Harschneck, Tobias; Manley, Eric F.; Lou, Sylvia J.; Hartnett, Patrick E.; Yu, Xinge; Horwitz, Noah E.; Mayorga Burrezo, Paula; Aldrich, Thomas J.; Lopez Navarrete, Juan T.; Wasielewski, Michael R.; Chen, Lin X.; Chang, Robert P. H.; Facchetti, Antonio; Marks, Tobin J.

    2015-10-07

    As effective building blocks for high-mobility transistor polymers, oligothiophenes are receiving attention for polymer solar cells (PSCs) because the resulting polymers can effectively suppress charge recombination. Here we investigate two series of in-chain donor-acceptor copolymers, PTPDnT and PBTInT, based on thieno[3,4-c]pyrrole-4,6-dione (TPD) or bithiopheneimide (BTI) as electron acceptor units, respectively, and oligothiophenes (nTs) as donor counits, for high-performance PSCs. Intramolecular S···O interaction leads to more planar TPD polymer backbones, however backbone torsion yields greater open-circuit voltages for BTI polymers. Thiophene addition progressively raises polymer HOMOs but marginally affects their band gaps. FT-Raman spectra indicate that PTPDnT and PBTInT conjugation lengths scale with nT catenation up to n = 3 and then saturate for longer oligomer. Furthermore, the effects of oligothiophene alkylation position are explored, revealing that the alkylation pattern greatly affects film morphology and PSC performance. The 3T with “outward” alkylation in PTPD3T and PBTI3T affords optimal π-conjugation, close stacking, long-range order, and high hole mobilities (0.1 cm2/(V s)). These characteristics contribute to the exceptional ~80% fill factors for PTPD3T-based PSCs with PCE = 7.7%. The results demonstrate that 3T is the optimal donor unit among nTs (n = 1-4) for photovoltaic polymers. Grazing incidence wide-angle X-ray scattering, transmission electron microscopy, and time-resolved microwave conductivity measurements reveal that the terthiophene-based PTPD3T blend maintains high crystallinity with appreciable local mobility and long charge carrier lifetime. These results provide fundamental materials structure-device performance correlations and suggest guidelines for designing oligothiophene-based polymers with optimal thiophene catenation and appropriate alkylation pattern to maximize PSC performance.

  14. Property-based design and synthesis of new chloroquine hybrids via simple incorporation of 2-imino-thiazolidine-4-one or 1h-pyrrol-2, 5-dione fragments on the 4-amino-7-chloroquinoline side chain

    Rojas, Fernando A.; Kouznetsov, Vladimir V., E-mail: kouznet@uis.edu.co [Laboratorio de Quimica Organica y Biomolecular, Escuela de Quimica, Universidad Industrial de Santander, Bucaramanga (Colombia)

    2011-09-15

    In the present work, the syntheses of new 4-amino-7-chloroquinoline N-derivatives were performed by selective modification of the side chain amino group of N-(7-chloroquinoline-4-yl) alkyldiamines, basis framework of chloroquine (CQ) drug through the incorporation of heterocyclic 2-imino-thiazolidine-4-one and {sup 1}H-pyrrol-2,5-dione systems. These potential activity modulators were selected thanks to their characteristic properties, and evaluated by virtual screening employing the OSIRIS and Molinspirations platforms. Designed and synthesized quinolinic derivatives could increase the antimalarial activity of CQ analogues without affecting the lipophilicity as described in literature, suggesting them as candidates for further biological assessments. (author)

  15. Ordering effects in benzo[1,2-b:4,5-b']difuran-thieno[3,4-c]pyrrole-4,6- dione polymers with >7% solar cell efficiency

    Warnan, Julien

    2014-05-15

    Benzo[1,2-b:4,5-b\\']difuran-thieno[3,4-c]pyrrole-4,6-dione (PBDFTPD) polymers prepared by microwave-assisted synthesis can achieve power conversion efficiencies (PCEs) >7% in bulk-heterojunction solar cells with phenyl-C61/71-butyric acid methyl ester (PCBM). In "as-cast" PBDFTPD-based devices solution-processed without a small-molecule additive, high PCEs can be obtained in spite of the weak propensity of the polymers to self-assemble and form π-aggregates in thin films. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Crystal structure of diethyl 2,2′-[((1E,1′E-{[(1R,4R-cyclohexane-1,4-diyl]bis(azanylylidene}bis(methanylylidenebis(1H-pyrrole-2,1-diyl]diacetate

    Jasim Alshawi

    2015-03-01

    Full Text Available The whole molecule of the title compound, C24H32N4O4, is generated by inversion symmetry. The cyclohexane ring adopts a chair conformation and the conformation about the C=N bonds is E. The pyrrole rings have an anti confirmation with respect to the cyclohexane moiety and the ethyl acetate groups have extended conformations. In the crystal, molecules are linked by pairs of C—H...O hydrogen bonds forming chains, enclosing R22(10 ring motifs with inversion symmetry, propagating parallel to the (101 plane.

  17. Crystal structure of ethyl 2-(2-{1-[N-(4-bromophenyl)-2-oxo-2-phenylacetamido]-2-tert-butylamino-2-oxoethyl}-1H-pyrrol-1-yl)acetate

    Tetsuji Moriguchi; Venkataprasad Jalli; Suvratha Krishnamurthy; Akihiko Tsuge; Kenji Yoza

    2015-01-01

    In the title compound, C28H30BrN3O5, there is an intramolecular N—H...O hydrogen bond and an intramolecular C—H...O hydrogen bond, both forming S(9) ring motifs. The planes of the 4-bromophenyl ring and the phenyl ring are inclined to that of the pyrrole ring by 48.05 (12) and 77.45 (14)°, respectively, and to one another by 56.25 (12)°. In the crystal, molecules are linked via C—H...O hydrogen bonds and C—H...π interactions, forming slabs parallel to (10-1).

  18. Clean and Efficient One-Pot Synthesis of New 2-Oxo-2,3-Dihydro-1H-Pyrrole-3-Carboxylic Acid and 2-Oxo-1,2-Dihydro-Pyridine-3-Carboxylic Acid Derivatives through Ball Milling under Catalyst-Free and Solvent-Free Conditions

    Mohamed Ould M'hamed

    2015-01-01

    A high-yielding one-pot ball milling method for the synthesis of new 2-oxo-2,3-dihydro-1H-pyrrole-3-carboxylic acid and 2-oxo-1,2-dihydropyridine- 3-carboxylic acid was developed under solvent-free and catalystfree conditions. The proposed method is simple and has environmental and economic advantages.

  19. EFSA CEF Panel (EFSA Panel on Food Contact Materials, Enzymes, Flavourings and Processing Aids), 2014. Scientific Opinion on Flavouring Group Evaluation 77, Revision 1 (FGE.77Rev1): Consideration of Pyridine, Pyrrole and Quinoline Derivatives evaluated by JECFA (63rd meeting)

    Beltoft, Vibe Meister; Binderup, Mona-Lise; Frandsen, Henrik Lauritz;

    for isoquinoline [FL-no: 14.001], pyrrole [FL-no: 14.041] and 2-acetylpyrrole [FL-no: 14.047]. The toxicity data on 2-acetylpyrrole should also cover 2-propionylpyrrole [FL-no: 14.068]. Further, additional genotoxicity data on 6-methylquinoline [FL-no: 14.042] have become available. The Panel...

  20. Characterization of the spontaneous “aging” of the heme oxygenase from the pathological bacterium Neisseria meningitidis via cleavage of the C-terminus in contact with the substrate; Implications for functional studies and the crystal structure†

    Liu, Yangzhong; Ma, Li-Hua; Zhang, Xuhong; Yoshida, Tadashi; Satterlee, James D.; La Mar, Gerd N.

    2006-01-01

    Solution 1H NMR spectroscopy and mass spectrometry are utilized to characterize the irreversible “aging” of native heme oxygenase from N. meningitidis, NmHO. 2D NMR characterization of the cyanide-inhibited substrate complex shows that the C-terminal interaction between Arg208His209 and the exposed pyrrole of the protohemin substrate in the “native” NmHO complex is lost in the “aging”. Mass spectrometry and N-terminal sequencing of WT and “aged” NmHO reveal that the “aging” process involves c...

  1. (3′R-3′-Benzyl-2′,3′-dihydro-1H-spiro[indole-3,1′-naphtho[2,3-c]pyrrole]-2,4′,9′-trione

    Garima Sharma

    2012-09-01

    Full Text Available In the title compound, C26H18N2O3, the maximum deviations from planarity for the tetrahydro-1H-naphtho[2,3-c]pyrrole and indoline rings systems are 0.091 (1 and 0.012 (2 Å, respectively. These ring systems make a dihedral angle of 89.95 (6° with each other and they make dihedral angles of 73.42 (8 and 71.28 (9°, respectively, with the benzene ring. In the crystal, inversion dimers linked by pairs of N—H...O hydrogen bonds generate R22(8 loops and C—H...O interactions connect the dimers into corrugated sheets lying parallel to the bc plane.

  2. A Novel Photocleaver with Long Wavelength Absorption-Highly Efficient Antitumor Agent:4-(2-Diethylamino-ethylamino)-8-oxo-8H-acenaphtho-[1,2-b]pyrrole-9-carbonitrile

    ZHANG Zhi-chao; L(U¨) Zhe; QIAN Xu-hong; LIU Feng-yu; SHENG Hui

    2005-01-01

    The photocleavage abilities of a novel family of compounds, 8-oxo-8 H -acenaphtho[1,2-b] pyrrole-9-carbonitrile and its derivatives(compounds 1-5) were evaluated with M13 mp18 single strand circular DNA. Only compound 1 with a diethylamine group could bind to DNA via electrostatic attraction and intercalation. At a concentration of 50 μmol/L, it could generate singlet oxygen to cleave circular DNA into linear DNA under the irradiation of long wavelength light(λ>400 nm). The antitumor ability of compound 1 was also evaluated in vitro, and its IC50 on HeLa cells was as low as 6.8 μmol/L.

  3. Static headspace analysis using polyurethane phases--application to roasted coffee volatiles characterization.

    Rodrigues, C; Portugal, F C M; Nogueira, J M F

    2012-01-30

    Static headspace sorptive extraction using polyurethane foams (HSSE(PU)) followed by gas chromatography coupled to mass spectrometry is proposed for volatile analysis. The application of this novel analytical approach to characterize the volatiles profile from roasted coffee samples, selected as model system, revealed remarkable advantages under convenient experimental conditions. The comparison of HSSE(PU) with other well-established procedures, such as headspace sorptive extraction using polydimethylsiloxane (HSSE(PDMS)) and headspace solid phase microextraction using carboxen/polydimethylsiloxane fibers (HS-SPME(CAR/PDMS)), showed that the former presented much higher capacity, sensitivity and even selectivity, where larger abundance and number of roasted coffee volatile compounds (e.g. furans, pyrazines, ketones, acids and pyrroles) could be achieved, under similar experimental conditions. The data presented herein proved, for the first time, that PU foams present great performance for static headspace sorption-based procedures, showing to be an alternative polymeric phase for volatile analysis. PMID:22284526

  4. Synthesis and characterization of a novel meso-porphyrin and its metallo derivatives

    Paulo Cesar Bega

    2014-02-01

    Full Text Available There has been a growing interest in the properties of substituted meso-tetraarylporphyrins and metallo porphyrins as catalysts for oxidation of hydrocarbons, oxygen detection, among others. This work describes the synthesis of a new porphyrin, 5,10,15,20-tetrakis(4-butoxy-3-methoxyphenylporphyrin, and its metallo complexes. Herein it was used a readily available reactant, vanillin, as starting material which was submitted to alkylation with n-bromobutane affording the synthetic precursor. The desired porphyrin was obtained by reacting the O-alkylated aldehyde with pyrrole in the presence of propionic acid (Alder-Longo method. The purified porphyrin was then subjected to the metallation process using iron (II and manganese (II salts. The synthesized compounds were characterized by IR, UV-Vis, NMR and EPR spectroscopy.

  5. Schiff bases of N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and its silatranes: Synthesis and characterization

    Gurjaspreet Singh; Amandeep Saroa; Sadhika Khullar; Sanjay K Mandal

    2015-04-01

    This paper aims at the introduction of azomethine group by the condensation reaction of N-(2-aminoethyl)-3-aminopropyltrimethoxysilane with different compounds containing carbonyl group such as 2’-hydroxyacetophenone, salicylaldehyde, pyrrole-2-carboxaldehyde, acetylacetone and ethyl acetoacetate. Further, transesterification reaction of these Schiff base modified silanes with triethanolamine as a tripodal ligand leads to the synthesis of corresponding silatranes 1–5 bearing Schiff base functionalized long chain in the axial position. All the synthesized compounds are characterized by spectroscopic methods, elemental analysis and mass spectrometry. The authentication of Schiff base modified silatranes is scrutinized by single X-ray crystal structure of silatrane 1. The thermal stability of the five silatranes is studied by thermo-gravimetric analysis (TGA).

  6. A Theoretical Study of the Relationships between Electronic Structure and CB1 and CB2 Cannabinoid Receptor Binding Affinity in a Group of 1-Aryl-5-(1-H-pyrrol-1-yl-1-H-pyrazole-3-carboxamides

    Francisco Salgado-Valdés

    2014-01-01

    Full Text Available We report the results of a search for model-based relationships between hCB1 and hCB2 receptor binding affinity and molecular structure for a group of 1-aryl-5-(1-H-pyrrol-1-yl-1-H-pyrazole-3-carboxamides. The wave functions and local atomic reactivity indices were obtained at the B3LYP/6-31G(d,p levels of theory with full geometry optimization. Interaction pharmacophores were generated for both receptors. The main conclusions of this work are as follows. (1 We obtained statistically significant equations relating the variation of hCB1 and hCB2 receptor binding affinities with the variation of definite sets of local atomic reactivity indices. (2 The interaction of the molecules with the hCB1 and hCB2 receptors seems to be highly complex and mainly orbital controlled. (3 The interaction mechanisms seem to be different for each type of receptor. This study, contrarily to the statistically backed ones, is able to provide a microscopic insight of the mechanisms involved in the binding process.

  7. Electron-deficient N-alkyloyl derivatives of thieno[3,4-c]pyrrole-4,6-dione yield efficient polymer solar cells with open-circuit voltages > 1 v

    Warnan, Julien

    2014-05-13

    Poly(benzo[1,2-b:4,5-b′]dithiophene-thieno[3,4-c]pyrrole-4,6-dione) (PBDTTPD) polymer donors yield some of the highest open-circuit voltages (V OC, ca. 0.9 V) and fill factors (FF, ca. 70%) in conventional bulk-heterojunction (BHJ) solar cells with PCBM acceptors. Recent work has shown that the incorporation of ring substituents into the side chains of the BDT motifs in PBDTTPD can induce subtle variations in material properties, resulting in an increase of the BHJ device VOC to ∼1 V. In this contribution, we report on the synthesis of N-alkyloyl-substituted TPD motifs (TPD(CO)) and show that the electron-deficient motifs can further lower both the polymer LUMO and HOMO levels, yielding device VOC > 1 V (up to ca. 1.1 V) in BHJ solar cells with PCBM. Despite the high VOC achieved (i.e., low polymer HOMO), BHJ devices cast from TPD(CO)-based polymer donors can reach power conversion efficiencies (PCEs) of up to 6.7%, making these promising systems for use in the high-band-gap cell of tandem solar cells. © 2014 American Chemical Society.

  8. Linear side chains in benzo[1,2-b:4,5-b′]dithiophene-thieno[3,4-c] pyrrole-4,6-dione polymers direct self-assembly and solar cell performance

    Cabanetos, Clement

    2013-03-27

    While varying the size and branching of solubilizing side chains in π-conjugated polymers impacts their self-assembling properties in thin-film devices, these structural changes remain difficult to anticipate. This report emphasizes the determining role that linear side-chain substituents play in poly(benzo[1,2-b:4,5-b′]dithiophene-thieno[3,4-c]pyrrole-4,6-dione) (PBDTTPD) polymers for bulk heterojunction (BHJ) solar cell applications. We show that replacing branched side chains by linear ones in the BDT motifs induces a critical change in polymer self-assembly and backbone orientation in thin films that correlates with a dramatic drop in solar cell efficiency. In contrast, we show that for polymers with branched alkyl-substituted BDT motifs, controlling the number of aliphatic carbons in the linear N-alkyl-substituted TPD motifs is a major contributor to improved material performance. With this approach, PBDTTPD polymers were found to reach power conversion efficiencies of 8.5% and open-circuit voltages of 0.97 V in BHJ devices with PC71BM, making PBDTTPD one of the best polymer donors for use in the high-band-gap cell of tandem solar cells. © 2013 American Chemical Society.

  9. Ethyl-2-amino-pyrrole-3-carboxylates are novel potent anticancer agents that affect tubulin polymerization, induce G2/M cell-cycle arrest, and effectively inhibit soft tissue cancer cell growth in vitro.

    Boichuk, Sergei; Galembikova, Aigul; Zykova, Svetlana; Ramazanov, Bulat; Khusnutdinov, Ramil; Dunaev, Pavel; Khaibullina, Svetlana; Lombardi, Vincent

    2016-08-01

    Microtubules are known to be one of the most attractive and validated targets in cancer therapy. However, the clinical use of drugs that affect the dynamic state of microtubules has been hindered by chemoresistance and toxicity issues. Accordingly, the development of novel agents that target microtubules is needed. Here, we report the identification of novel compounds with pirrole and carboxylate structures: ethyl-2-amino-pyrrole-3-carboxylates (EAPCs) that provide potent cytotoxic activities against multiple soft tissue cancer cell lines in vitro. Using the MTS cell proliferation assay, we assessed the activity of EAPCs on various cancer cell lines including leiomyosarcoma SK-LMS-1, rhabdomyosarcoma RD, gastrointestinal stromal tumor GIST-T1, A-673 Ewing's sarcoma, and U-2 OS osteosarcoma. We found that in the majority of cases, two EAPC compounds (EAPC-20 and EAPC-24) considerably inhibited cancer cell proliferation in vitro. The growth-inhibitory effects of EAPC-20 and EAPC-24 were time and dose dependent. The molecular mechanisms of action of these compounds were because of the inhibition of tubulin polymerization and induction of a robust G2/M cell-cycle arrest, leading to considerable accumulation of tumor cells in the M-phase. Finally, EAPCs induced tumor cell death by apoptotic pathways. The above-mentioned effects were also observed in most soft tissue tumor cell lines and the gastrointestinal stromal tumor cell line investigated. Taken together, our data identify potent antitumor activity of EAPCs in vitro, thus providing a novel scaffold with which to develop potent chemotherapeutic agents for cancer therapy. PMID:27129079

  10. The formation of [M-H]+ ions in N-alkyl-substituted thieno[3,4-c]-pyrrole-4,6-dione derivatives during atmospheric pressure photoionization mass spectrometry

    Sioud, Salim

    2014-10-09

    RESULTS [M-H]+ ions were observed under APPI conditions. The type of dopant and the length of the alkyl chain affected the formation of these ions. MS/MS fragmentation of [M-H]+ and [M + H]+ ions exhibited completely different patterns. Theoretical calculations revealed that the loss of hydrogen molecules from the [M + H]+ ions is the most favourable condition under which to form [M-H]+ ions.CONCLUSIONS [M-H]+ ions were detected in all the TPD derivatives studied here under the special experimental conditions during APPI, using a halogenated benzene dopant, and TPD containing substituted N-alkyl side chains with a minimum of four carbon atoms. Density functional theory calculations showed that for [M-H]+ ions to be formed under these conditions, the loss of hydrogen molecules from the [M + H]+ ions is proposed to be necessary.RATIONALE The formation of ions during atmospheric pressure photoionization (APPI) mass spectrometry in the positive mode usually provides radical cations and/or protonated species. Intriguingly, during the analysis of some N-alkyl-substituted thieno[3,4-c]pyrrole-4,6-dione (TPD) derivatives synthesized in our laboratory, unusual [M-H]+ ion peaks were observed. In this work we investigate the formation of [M-H]+ ions observed under APPI conditions.METHODS Multiple experimental parameters, including the type of ionization source, the composition of the solvent, the type of dopant, the infusion flow rate, and the length of the alkyl side chain were investigated to determine their effects on the formation of [M-H]+ ions. In addition, a comparison study of the gas-phase tandem mass spectrometric (MS/MS) fragmentation of [M + H]+ vs [M-H]+ ions and computational approaches were used.

  11. Synthesis, characterization and electrochemical behavior of polypyrrole/carbon nanotube composites using organometallic-functionalized carbon nanotubes

    Thorn-like, organometallic-functionalized carbon nanotubes were successfully developed via a novel microwave hydrothermal route. The organometallic complex with methyl orange and iron (III) chloride served as reactive seed template, resulting in the oriented polymerization of pyrrole on the modified carbon nanotubes without the assistance of other oxidants. Morphological and structural characterizations of the carbon nanotube/methyl orange-iron (III) chloride and polypyrrole/carbon nanotube composites were examined using transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), infrared spectroscopy and X-ray diffraction (XRD). The electrochemical property of the polypyrrole/carbon nanotube composite was elucidated by cyclic voltammetry and galvanostatic charge-discharge. A specific capacitance of 304 F g-1 was obtained within the potential range of -0.5-0.5 V in 1 M KCl solution.

  12. Detailed characterization of a Comparative Reactivity Method (CRM) instrument for ambient OH reactivity measurements: experiments vs. modeling

    Michoud, Vincent; Locoge, Nadine; Dusanter, Sébastien

    2015-04-01

    The Hydroxyl radical (OH) is the main daytime oxidant in the troposphere, leading to the oxidation of Volatile Organic Compounds (VOCs) and the formation of harmful pollutants such as ozone (O3) and Secondary Organic Aerosols (SOA). While OH plays a key role in tropospheric chemistry, recent studies have highlighted that there are still uncertainties associated with the OH budget, i.e the identification of sources and sinks and the quantification of production and loss rates of this radical. It has been demonstrated that ambient measurements of the total OH loss rate (also called total OH reactivity) can be used to identify and reduce these uncertainties. In this context, the Comparative Reactivity Method (CRM), developed by Sinha et al. (ACP, 2008), is a promising technique to measure total OH reactivity in ambient air and has already been used during several field campaigns. This technique relies on monitoring competitive reactions of OH with ambient trace gases and a reference compound (pyrrole) in a sampling reactor to derive ambient OH reactivity. However, this technique requires a complex data processing chain that has yet to be carefully investigated in the laboratory. In this study, we present a detailed characterization of a CRM instrument developed at Mines Douai, France. Experiments have been performed to investigate the dependence of the CRM response on humidity, ambient NOx levels, and the pyrrole-to-OH ratio inside the sampling reactor. Box modelling of the chemistry occurring in the reactor has also been performed to assess our theoretical understanding of the CRM measurement. This work shows that the CRM response is sensitive to both humidity and NOx, which can be accounted for during data processing using parameterizations depending on the pyrrole-to-OH ratio. The agreement observed between laboratory studies and model results suggests a good understanding of the chemistry occurring in the sampling reactor and gives confidence in the CRM

  13. Sensitive and selective electrochemical determination of quinoxaline-2-carboxylic acid based on bilayer of novel poly(pyrrole) functional composite using one-step electro-polymerization and molecularly imprinted poly(o-phenylenediamine)

    Yang, Yukun; Fang, Guozhen; Wang, Xiaomin; Pan, Mingfei; Qian, Hailong; Liu, Huilin; Wang, Shuo, E-mail: s.wang@tust.edu.cn

    2014-01-02

    Graphical abstract: -- Highlights: •PPY-GO-BiCoPc composite was formed using a simple electrochemical method for the first time. •A novel PoPD-MIP sensor based on PPY-GO-BiCoPc composite had been fabricated. •The PPY-GO-BiCoPc functional composite was introduced to improve performance of the sensor. •Highly sensitive, selective and stable sensor had been achieved. •The established MIP sensor could be promising in food safety analysis. -- Abstract: A facile and efficient molecularly imprinted polymer (MIP) recognition element of electrochemical sensor was fabricated by directly electro-polymerizing monomer o-phenylenediamine (oPD) in the presence of template quinoxaline-2-carboxylic acid (QCA), based on one-step controllable electrochemical modification of poly(pyrrole)-graphene oxide-binuclear phthalocyanine cobalt (II) sulphonate (PPY-GO-BiCoPc) functional composite on glassy carbon electrode (GCE). The MIP film coated on PPY-GO-BiCoPc functional composite decorated GCE (MIP/PPY-GO-BiCoPc/GCE) was presented for the first time. The synergistic effect and electro-catalytic activity toward QCA redox of PPY-GO-BiCoPc functional composite were discussed using various contrast tests. Also, the effect of experimental variables on the current response such as, electro-polymerization cycles, template/monomer ratio, elution condition for template removal, pH of the supporting electrolyte and accumulation time, were investigated in detail. Under the optimized conditions, the proposed MIP sensor possessed a fast rebinding dynamics and an excellent recognition capacity to QCA, while the anodic current response of square wave voltammetry (SWV) was well-proportional to the concentration of QCA in the range of 1.0 × 10{sup −8}–1.0 × 10{sup −4} and 1.0 × 10{sup −4}–5.0 × 10{sup −4} mol L{sup −1} with a low detection limit of 2.1 nmol L{sup −1}. The established sensor was applied successfully to determine QCA in commercial pork and chicken muscle

  14. 4-Hydroxy-7-oxo-5-heptenoic Acid (HOHA) Lactone is a Biologically Active Precursor for the Generation of 2-(ω-Carboxyethyl)pyrrole (CEP) Derivatives of Proteins and Ethanolamine Phospholipids.

    Wang, Hua; Linetsky, Mikhail; Guo, Junhong; Choi, Jaewoo; Hong, Li; Chamberlain, Amanda S; Howell, Scott J; Howes, Andrew M; Salomon, Robert G

    2015-05-18

    2-(ω-Carboxyethyl)pyrrole (CEP) derivatives of proteins were previously shown to have significant pathological and physiological relevance to age-related macular degeneration, cancer and wound healing. Previously, we showed that CEPs are generated in the reaction of ε-amino groups of protein lysyl residues with 1-palmityl-2-(4-hydroxy-7-oxo-5-heptenoyl)-sn-glycero-3-phosphatidylcholine (HOHA-PC), a lipid oxidation product uniquely generated by oxidative truncation of docosahexanenate-containing phosphatidylcholine. More recently, we found that HOHA-PC rapidly releases HOHA-lactone and 2-lyso-PC (t1/2 = 30 min at 37 °C) by nonenzymatic transesterification/deacylation. Now we report that HOHA-lactone reacts with Ac-Gly-Lys-OMe or human serum albumin to form CEP derivatives in vitro. Incubation of human red blood cell ghosts with HOHA-lactone generates CEP derivatives of membrane proteins and ethanolamine phospholipids. Quantitative analysis of the products generated in the reaction HOHA-PC with Ac-Gly-Lys-OMe showed that HOHA-PC mainly forms CEP-dipeptide that is not esterified to 2-lysophosphatidycholine. Thus, the HOHA-lactone pathway predominates over the direct reaction of HOHA-PC to produce the CEP-PC-dipeptide derivative. Myleoperoxidase/H2O2/NO2(-) promoted in vitro oxidation of either 1-palmityl-2-docosahexaneoyl-sn-glycero-3-phosphatidylcholine (DHA-PC) or docosahexaenoic acid (DHA) generates HOHA-lactone in yields of 0.45% and 0.78%, respectively. Lipid oxidation in human red blood cell ghosts also releases HOHA-lactone. Oxidative injury of ARPE-19 human retinal pigmented epithelial cells by exposure to H2O2 generated CEP derivatives. Treatment of ARPE-19 cells with HOHA-lactone generated CEP-modified proteins. Low (submicromolar), but not high, concentrations of HOHA-lactone promote increased vascular endothelial growth factor (VEGF) secretion by ARPE-19 cells. Therefore, HOHA-lactone not only serves as an intermediate for the generation of CEPs but

  15. Synthesis and preliminary characterization of radioiodinated benzofuran-3-yl-(indol-3-yl)maleimide derivatives as potential SPECT imaging probes for the detection of glycogen synthase kinase-3β (GSK-3β) in the brain.

    Ono, Masahiro; Kitada, Ayane; Watanabe, Hiroyuki; Miyazaki, Anna; Kimura, Hiroyuki; Saji, Hideo

    2016-06-30

    We report on the synthesis and preliminary characterization of two radioiodinated benzofuran-3-yl-(indol-3-yl)maleimides, 3-(benzofuran-3-yl)-4-(5-[(125) I]iodo-1-methyl-1H-indol-3-yl)-1H-pyrrole-2,5-dione ([(125) I]5), and 3-(5-[(125) I]iodo-1-methyl-1H-indol-3-yl)-4-(6-methoxybenzofuran-3-yl)-1H-pyrrole-2,5-dione ([(125) I]6), as the first potential SPECT imaging probes targeting glycogen synthase kinase-3β (GSK-3β). In this study, we used (125) I as a surrogate of (123) I because of its ease of use. The radioiodinated ligands were prepared from the corresponding tributyltin precursors through an iododestannylation reaction using hydrogen peroxide as an oxidant with a radiochemical yield of 10-30%. In vitro binding experiments suggested that both compounds show high affinity for GSK-3β at a level similar to a known GSK-3β inhibitor. Biodistribution studies with normal mice revealed that the radioiodinated compounds display sufficient uptake into (1.8%ID/g at 10 min postinjection) and clearance from the brain (1.0%ID/g at 60 min postinjection). These preliminary results suggest that the further optimization of radioiodinated benzofuran-3-yl-(indol-3-yl)maleimide derivatives may facilitate the development of clinically useful SPECT imaging probes for the in vivo detection of GSK-3β. PMID:27126914

  16. Synthesis, spectroscopic characterizations, crystal structures and DFT studies of nalidixic acid carbonyl hydrazones derivatives

    Bergamini, F. R. G.; Ribeiro, M. A.; Lancellotti, M.; Machado, D.; Miranda, P. C. M. L.; Cuin, A.; Formiga, A. L. B.; Corbi, P. P.

    2016-09-01

    This article describes the synthesis and characterization of the 1-ethyl-7-methyl-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carbohydrazide (hzd) and six carbonyl hydrazones derivatives of the nalidixic with 1H-pyrrol-2-ylmethylidene (hpyrr), 1H-imidazol-2-ylmethylidene (h2imi), pyridin-2-ylmethylidene (h2py), pyridin-3-ylmethylidene (h3py), pyridin-4-ylmethylidene(h4py) and (2-hydroxyphenyl)methylidene (hsali). The carbonyl hydrazones were characterized by elemental and ESI-QTOF-MS analyses, IR and detailed NMR spectroscopic measurements. The 2D NMR experiments allowed the unambiguous assignment of the hydrogen, carbon and nitrogen atoms, which have not been reported for nalidixic acid carbonyl hydrazone derivatives so far. Crystal structures of hzd and the new carbonyl hydrazones h2imi, hpyrr and h3py were determined by X-ray diffraction studies. Although the synthesis of hzd was reported decades ago, the hzd crystal structure have not been reported yet. Geometric optimizations of all the characterized structures were performed with the aid of DFT studies. Despite the fact that the hydrazones with 2-pyridine carboxylic acid (h2py) and salicyl aldehyde (hsali) were already reported by literature, a detailed spectroscopic study followed by DFT studies are also reported for such compounds in this manuscript. Antimicrobial studies of the compounds are also presented.

  17. Detailed characterizations of a Comparative Reactivity Method (CRM) instrument: experiments vs. modelling

    Michoud, V.; Hansen, R. F.; Locoge, N.; Stevens, P. S.; Dusanter, S.

    2015-04-01

    The Hydroxyl radical (OH) is an important oxidant in the daytime troposphere that controls the lifetime of most trace gases, whose oxidation leads to the formation of harmful secondary pollutants such as ozone (O3) and Secondary Organic Aerosols (SOA). In spite of the importance of OH, uncertainties remain concerning its atmospheric budget and integrated measurements of the total sink of OH can help reducing these uncertainties. In this context, several methods have been developed to measure the first-order loss rate of ambient OH, called total OH reactivity. Among these techniques, the Comparative Reactivity Method (CRM) is promising and has already been widely used in the field and in atmospheric simulation chambers. This technique relies on monitoring competitive OH reactions between a reference molecule (pyrrole) and compounds present in ambient air inside a sampling reactor. However, artefacts and interferences exist for this method and a thorough characterization of the CRM technique is needed. In this study, we present a detailed characterization of a CRM instrument, assessing the corrections that need to be applied on ambient measurements. The main corrections are, in the order of their integration in the data processing: (1) a correction for a change in relative humidity between zero air and ambient air, (2) a correction for the formation of spurious OH when artificially produced HO2 react with NO in the sampling reactor, and (3) a correction for a deviation from pseudo first-order kinetics. The dependences of these artefacts to various measurable parameters, such as the pyrrole-to-OH ratio or the bimolecular reaction rate constants of ambient trace gases with OH are also studied. From these dependences, parameterizations are proposed to correct the OH reactivity measurements from the abovementioned artefacts. A comparison of experimental and simulation results is then discussed. The simulations were performed using a 0-D box model including either (1) a

  18. Pyrrole-Based Conductive Polymers For Capacitors

    Nagasubramanian, Ganesan; Di Stefano, Salvador

    1994-01-01

    Polypyrrole films containing various dopant anions exhibit superior capacitance characteristics. Used with nonaqueous electrolytes. Candidate for use in advanced electrochemical double-layer capacitors capable of storing electrical energy at high densities. Capacitors made of these films used in automobiles and pulsed power supplies.

  19. Transducer characterization

    For inservice inspection transducer characterization can be an important item if one wants to compare ultrasonic examination data obtained at different times (fingerprint). It is possible that the transducers used during previous examinations are lost or will become defect. In such a case it is most useful if one can check the characteristics of the replacement transducers. Some time ago an elegant characterization method was developed by the EURATOM Joint Research Centre of Ispra based on liquid crystals. This method is now under development at Neratoom and the results so far indicate that a robust characterization rig can be built at a reasonable price

  20. Crystal structure of ethyl 2-(2-{1-[N-(4-bromo­phen­yl)-2-oxo-2-phenyl­acetamido]-2-tert-butyl­amino-2-oxo­ethyl}-1H-pyrrol-1-yl)acetate

    Moriguchi, Tetsuji; Jalli, Venkataprasad; Krishnamurthy, Suvratha; Tsuge, Akihiko; Yoza, Kenji

    2015-01-01

    In the title compound, C28H30BrN3O5, there is an intra­molecular N—H⋯O hydrogen bond and an intra­molecular C—H⋯O hydrogen bond, both forming S(9) ring motifs. The planes of the 4-bromo­phenyl ring and the phenyl ring are inclined to that of the pyrrole ring by 48.05 (12) and 77.45 (14)°, respectively, and to one another by 56.25 (12)°. In the crystal, mol­ecules are linked via C—H⋯O hydrogen bonds and C—H⋯π inter­actions, forming slabs parallel to (10-1).

  1. Metal based new triazoles: Their synthesis, characterization and antibacterial/antifungal activities

    Sumrra, Sajjad H.; Chohan, Zahid H.

    2012-12-01

    A series of new triazoles and their oxovanadium(IV) complexes have been synthesized, characterized and evaluated for antibacterial/antifungal properties. The new Schiff bases ligands (L1)-(L5) were prepared by the condensation reaction of 3,5-diamino-1,2,4-triazole with 2-hydroxy-1-naphthaldehyde, pyrrole-2-carboxaldehyde, pyridine-2-carboxaldehyde, 2-acetyl pyridine and 2-methoxy benzaldehyde. The structures of the ligands have been established on the basis of their physical, spectral (IR, 1H and 13C NMR and mass spectrometry) and elemental analytical data. The prepared ligands were used to synthesize their oxovanadium(IV) complexes (1)-(5) which were also characterized by their physical, spectral and analytical data and proposed to have a square pyramidal geometry. The ligands and their complexes were screened for in vitro antibacterial activity against six bacterial species such as, Escherichia coli, Shigella flexneri, Pseudomonas aeruginosa, Salmonella typhi, Staphylococcus aureus, and Bacillus subtilis and for in vitro antifungal activity against six fungal strains, Trichophyton longifusus, Candida albicans, Aspergillus flavus, Microsporum canis, Fusarium solani, and Candida glabrata. Cytotoxic nature of the compounds was also reported using brine shrimp bioassay method against Artemia salina.

  2. In-vitro investigations of the speed of pyrrole formation of 2,5-hexanedione and 2,5-heptanedione with N{alpha}-acetyl-L-lysine as a precondition for a comparative assessment of the neurotoxic potentials of the two {gamma}-diketones; In-vitro-Untersuchungen zur Pyrrolbildungsgeschwindigkeit von 2,5-Hexandion und 2,5-Heptandion mit N{alpha}-Acetyl-L-lysin als Voraussetzung fuer eine vergleichende Abschaetzung der neurotoxischen Potentiale beider {gamma}-Diketone

    Richter, M.F.

    1997-09-01

    N-hexane and n-heptane are important solvents. Chronic exposure to n-hexane causes polyneuropathies, which are attributed to the metabolite 2,5-hexanedione, a {gamma} diketone. As a basis for a comparative assessment of the neurotoxic potentials of 2,5-hexanedione and 2,5-heptanedione, an in-vitro test was developed and used to investigate the speed of pyrrole formation of the two {gamma} diketones in reacting with the {epsilon} amino group of N{alpha}-acetyl L-lysine. The speed of the formation of pyrrole was always directly proportional to the respective reactant concentration. It consequently is subject to a second-order kinetics. As a further result, the pyrrole formation speed of 2,5-heptanedione was found to be only half that of 2,5-hexanedione. The results lead to the conclusion that 2,5-heptanedione poses a smaller risk of developing peripheral neuropathy than 2,5-hexanedione. (orig./MG) [Deutsch] n-Hexan und n-Heptan sind wichtige Loesungsmittel. Chronische Exposition gegenueber n-Hexan ruft Polyneuropathien hervor, die auf den Metaboliten 2,5-Hexandion, ein {gamma}-Diketon, zurueckgefuehrt werden. Als Grundlage fuer eine vergleichende Abschaetzung der neurotoxischen Potentiale von 2,5-Hexandion und 2,5-Heptandion wurde in der vorliegenden Arbeit ein In-vitro-Test entwickelt, mit dem die Pyrrolbildungsgeschwindigkeiten der beiden {gamma}-Diketone mit der {epsilon}-Aminogruppe von N{alpha}-Acetyl-L-Iysin untersucht wurden. Die Pyrrolbildungsgeschwindigkeit war stets direkt proportional zur jeweiligen Reaktantenkonzentration. Somit unterliegt sie einer Kinetik 2. Ordnung. Weiterhin wurde gezeigt, dass die Pyrrolbildungsgeschwindigkeit fuer 2,5-Heptandion nur etwa halb so gross ist wie fuer 2,5-Hexandion. Aus den Ergebnissen wird gefolgert, dass das von 2,5-Heptandion ausgehende Risiko an peripheren Neuropathien zu erkranken geringer ist, als das von 2,5-Hexandion ausgehende. (orig./MG)

  3. Preparation and characterization of electrical conductive PVA based materials for peripheral nerve tube-guides.

    Gonçalves, C; Ribeiro, J; Pereira, T; Luís, A L; Mauricio, A C; Santos, J D; Lopes, M A

    2016-08-01

    Peripheral nerve regeneration is a serious clinical problem. Presently, there are several nerve tube-guides available in the market, however with some limitations. The goal of this work was the development of a biomaterial with high electrical conductivity to produce tube-guides for nerve regeneration after neurotmesis injuries whenrver an end-to-end suture without tension is not possible. A matrix of poly(vinyl alcohol) (PVA) was used loaded with the following electrical conductive materials: COOH-functionalized multiwall carbon nanotubes (MWCNTs), poly(pyrrole) (PPy), magnesium chloride (MgCl2 ), and silver nitrate (AgNO3 ). The tube-guide production was carried out by a freezing/thawing process (physical crosslinking) with a final annealing treatment. After producing the tube-guide for nerve regeneration, the physicochemical characterization was performed. The most interesting results were achieved by loading PVA with 0.05% of PPy or COOH- functionalized CNTs. These tubes combined the electrical conductivity of carbon nanotubes (CNTs) and PPy with the biocompatibility of PVA matrix, with potential clinical application for nerve regeneration. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 104A: 1981-1987, 2016. PMID:27027727

  4. Synthesis characterization and structural investigations on lanthanon(III) chelates of tridentate Schiff bases

    The dissociation constants of O-(N-pyrrole-2-methyl imino) propanoic acid [H2PP] and O-(N-furan-2-chloroimino)ethane thiol [HFT], stability constants and thermodynamic parameters of their chelates with La(II), Ce(III), Nd(III), Sm(III), Gd(III), Tb(III), Dy(III), Ho(III) and Er(III) have been determined by Calvin-Bjerrum pH-titration techniques as modified by Irving and Rossotti in 30% (v/v) alcohol-water medium (μ=0.01 M, 0.05 M and 0.1 M NaClO4) at 25, 35 and 45degC. Solid Ln(III) chelates were characterized by molecular mass, elemental analysis, magnetic moment, conductance, 1H NMR, electronic and IR spectra. HFT-Ln(III)-chelates show 1:3 metal-ligand stoichiometry whereas H2PP-Ln(III)-chelates show 1:2 stoichiometry. Physico-chemical studies such as magnetic, IR, NMR etc. also support these geometries. HFT and H2PP are respectively monoprotic and biprotic tridentates. In view of the above facts a trigonal tricapped pyramidal and octahedral geometries can be assigned to the HFT-Ln(III) and H2PP-Ln(III) chelates respectively. (author). 15 refs., 4 tabs., 1 fig

  5. Cellulose aerogels functionalized with polypyrrole and silver nanoparticles: In-situ synthesis, characterization and antibacterial activity.

    Wan, Caichao; Li, Jian

    2016-08-01

    Green porous and lightweight cellulose aerogels have been considered as promising candidates to substitute some petrochemical host materials to support various nanomaterials. In this work, waste wheat straw was collected as feedstock to fabricate cellulose hydrogels, and a green inexpensive NaOH/polyethylene glycol solution was used as cellulose solvent. Prior to freeze-drying treatment, the cellulose hydrogels were integrated with polypyrrole and silver nanoparticles by easily-operated in-situ oxidative polymerization of pyrrole using silver ions as oxidizing agent. The tri-component hybrid aerogels were characterized by scanning electron microscope, transmission electron microscope, energy dispersive X-ray spectroscopy, selected area electron diffraction, X-ray photoelectron spectroscopy, and X-ray diffraction. Moreover, the antibacterial activity of the hybrid aerogels against Escherichia coli (Gram-negative), Staphylococcus aureus (Gram-positive) and Listeria monocytogenes (intracellular bacteria) was qualitatively and quantitatively investigated by parallel streak method and determination of minimal inhibitory concentration, respectively. This work provides an example of combining cellulose aerogels with nanomaterials, and helps to develop novel forms of cellulose-based functional materials. PMID:27112885

  6. Synthesis, characterization and a.c. conductivity of polypyrrole/Y2O3 composites

    T K Vishnuvardhan; V R Kulkarni; C Basavaraja; S C Raghavendra

    2006-02-01

    Conducting polymer composites of polypyrrole/yttrium oxide (PPy/Y2O3) were synthesized by in situ polymerization of pyrrole with Y2O3 using FeCl3 as an oxidant. The Y2O3 is varied in five different weight percentages of PPy in PPy/Y2O3 composites. The synthesized polymer composites are characterized by infrared and X-ray diffraction techniques. The surface morphology of the composite is studied by scanning electron microscopy. The glass transition temperature of the polymer and its composite is discussed by DSC. Electrical conductivity of the compressed pellets depends on the concentration of Y2O3 in PPy. The frequency dependent a.c. conductivity reveals that the Y2O3 concentration in PPy is responsible for the variation of conductivity of the composites. Frequency dependent dielectric constant at room temperature for different composites are due to interfacial space charge (Maxwell Wagner) polarization leading to the large value of dielectric constant. Frequency dependent dielectric loss, as well as variation of dielectric loss as a function of mass percentage of Y2O3 is also presented and discussed.

  7. The application of zero-current potentiometry in chemical synthesis and characterization of polypyrrole using electrochemical sensors

    Budimir, M.V. (Faculty of Agriculture, Univ. of Osijek (Yugoslavia)); Sak-Bosnar, M. (Pedagogical Faculty, Univ. of Osijek (Yugoslavia)); Kovac, S. (Faculty of Food Tech., Univ. of Osijek (Yugoslavia)); Duic, L. (Faculty of Tech., Inst. of Electrochemistry, Univ. of Zagreb (Yugoslavia))

    1991-01-01

    The chemical polymerization of pyrrole to highly conducting polypyrrole in aqueous and acetonitrile solutions using various oxidizing agents was studied. The course of synthesis was followed using zero-current potentiometry with a platinum reference electrode as redox sensor. The obtained results can be used for a better understanding of pyrrole polymerization kinetics. In addition, the halogenide-ion content as counter ion can be determined potentiometrically after chemical degradation of polypyrrole using a chloride-selective electrode as sensor. (orig.).

  8. Column solid phase extraction and flame atomic absorption spectrometric determination of manganese(II) and iron(III) ions in water, food and biological samples using 3-(1-methyl-1H-pyrrol-2-yl)-1H-pyrazole-5-carboxylic acid on synthesized graphene oxide.

    Pourjavid, Mohammad Reza; Sehat, Ali Akbari; Arabieh, Masoud; Yousefi, Seyed Reza; Hosseini, Majid Haji; Rezaee, Mohammad

    2014-02-01

    A modified, selective, highly sensitive and accurate procedure for the determination of trace amounts of manganese and iron ions is established in the presented work. 3-(1-Methyl-1H-pyrrol-2-yl)-1H-pyrazole-5-carboxylic acid (MPPC) and graphene oxide (GO) were used in a glass column as chelating reagent and as adsorbent respectively prior to their determination by flame atomic absorption spectrometry. The adsorption mechanism of titled metals complexes on GO was investigated by using computational chemistry approach based on PM6 semi-empirical potential energy surface (PES). The effect of some parameters including pH, flow rate and volume of sample and type, volume and concentration of eluent, as well as the adsorption capacity of matrix ions on the recovery of Mn(II) and Fe(III) was investigated. The limit of detection was 145 and 162 ng L(-1) for Mn(II) and Fe(III), respectively. Calibration was linear over the range of 0.31-355 μg L(-1) for Mn(II) and 0.34-380 μg L(-1) for Fe(III) ions. The method was successfully applied for the determination of understudied ions in water, food and biological samples. PMID:24411390

  9. NiCrFe2-O4 ferrite nanoparticles and their composites with polypyrrole: synthesis, characterization and magnetic properties

    E H El-Ghazzawy; S N Alamri

    2015-08-01

    Nanocrystalline nickel chromium ferrite (NiCrFe2-O4, = 0.1, 0.2) have been prepared by the chemical co-precipitation method. Half of the samples have been sintered at 620°C and the other at 1175°C. Then polypyrrole (PPy)–NiCrFe2-O4 composites have been synthesized by polymerization of pyrrole monomer in the presence of NiCrFe2-O4 nanoparticles. The structure, morphology and magnetic properties of the samples have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Fourier transform infrared (FT-IR) spectroscopy and vibrating sample magnetometer. Also, the initial magnetic permeability measurements as functions of temperature and frequency have been performed. The XRD and FT-IR studies have confirmed the well crystalline phase of ferrite nanoparticles, and the presence of amorphous PPy in the composite samples. The SEM and TEM images have obviously clarified the coating of ferrite nanoparticles by PPy in the composite samples. The hysteresis loop of the samples has proved that the samples are soft magnetic material because of their low coercivity.

  10. Synthesis and partial characterization of a new low gap polymer: poly-2(5)-propenylidenepyrrole

    Hevesi, L. (Dept. of Chemistry, Facultes Universitaires N.-D. de la Paix, Namur (Belgium)); Proess, G. (Dept. of Chemistry, Facultes Universitaires N.-D. de la Paix, Namur (Belgium)); Lazarescu-Grigore, A. (Dept. of Chemistry, Facultes Universitaires N.-D. de la Paix, Namur (Belgium))

    1993-07-01

    As a result of previous studies on the reactivity of 1-selenoallyl cationic species with pyrroles, a synthetic scheme, based on the dramatic solvent effects on the regiochemistry of these reactions, has been devised for the preparation of the polymeric material 6 composed of alternating propenyl and pyrrole units. It is argued that oxidation of 6 using Ph[sub 3]CSbCl[sub 6] or DDQ produces the title compound 8 where every other alternating pyrrole ring should have a quinoid structure. In agreement with theoretical predictions of bandgap lowering by these quinoid structure units, preliminary measurements on the undoped and iodine-doped 8 gave conductivity values of [sigma]=1.1x10[sup -6] and [sigma]=(2.4-5.4)x10[sup -6] [Omega][sup -1] cm[sup -1], respectively. (orig.)

  11. Column solid phase extraction and flame atomic absorption spectrometric determination of manganese(II) and iron(III) ions in water, food and biological samples using 3-(1-methyl-1H-pyrrol-2-yl)-1H-pyrazole-5-carboxylic acid on synthesized graphene oxide

    Pourjavid, Mohammad Reza, E-mail: pourjavid@gmail.com [NFCRS, Nuclear Science and Technology Research Institute, P.O. Box 11365-8486, Tehran (Iran, Islamic Republic of); Sehat, Ali Akbari [Department of Analytical Chemistry, Faculty of Chemistry, University College of Science, University of Tehran, P.O. Box 14155-6455, Tehran (Iran, Islamic Republic of); Arabieh, Masoud; Yousefi, Seyed Reza; Hosseini, Majid Haji; Rezaee, Mohammad [NFCRS, Nuclear Science and Technology Research Institute, P.O. Box 11365-8486, Tehran (Iran, Islamic Republic of)

    2014-02-01

    A modified, selective, highly sensitive and accurate procedure for the determination of trace amounts of manganese and iron ions is established in the presented work. 3-(1-Methyl-1H-pyrrol-2-yl)-1H-pyrazole-5-carboxylic acid (MPPC) and graphene oxide (GO) were used in a glass column as chelating reagent and as adsorbent respectively prior to their determination by flame atomic absorption spectrometry. The adsorption mechanism of titled metals complexes on GO was investigated by using computational chemistry approach based on PM6 semi-empirical potential energy surface (PES). The effect of some parameters including pH, flow rate and volume of sample and type, volume and concentration of eluent, as well as the adsorption capacity of matrix ions on the recovery of Mn(II) and Fe(III) was investigated. The limit of detection was 145 and 162 ng L{sup −1} for Mn(II) and Fe(III), respectively. Calibration was linear over the range of 0.31–355 μg L{sup −1} for Mn(II) and 0.34–380 μg L{sup −1} for Fe(III) ions. The method was successfully applied for the determination of understudied ions in water, food and biological samples. - Highlights: • We use synthesized graphene oxide as adsorbent for SPE of Mn(II) and Fe(III) ions. • Adsorption mechanism was investigated by PM6 semi-empirical potential energy surface. • Detection limits were 145 and 162 ng L{sup −1} for Mn and Fe, respectively. • The preconcentration factor was 325 and sample flow rate is 8 mL min{sup −1}. • It was successfully applied to the determination of Mn and Fe ions in real samples.

  12. Coordination of Fe(III), Co(II), Ni(II), Cu(II), Zn(II), Cd(II), Hg(II), Pd(II) and Pt(II) with 2,5-hexanedione bis(thiosemicarbazone), HBTS: crystal structure of cis-[Pd(HBTS)]Cl2 and 1-(2,5-dimethyl-1H-pyrrol-yl)-thiourea.

    Jeragh, Bakir; El-Asmy, Ahmed A

    2014-09-15

    Metal complexes of Fe3+, Co2+, Ni2+, Cu2+, Zn2+, Cd2+, Hg2+, Pd2+ or Pt2+ with 2,5-hexanedione bis(thiosemicarbazone), HBTS; have been prepared and spectroscopically investigated. The empirical formulae of the complexes were suggested based on the elemental analysis. Single crystal of Pd(II) has been solved to be cis-form of square-planar geometry by the X-ray crystallography. 1H and 13C NMR spectra have been recorded for HBTS, Zn(II), Cd(II), Hg(II), Pd(II) and Pt(II) complexes, in DMSO-d6, showing the mode of chelation. The ligand acts as a neutral or a binegative tetradentate (N2S2) or neutral bidentate on the basis of FT-IR. The magnetic moments and electronic spectra provide information about the geometry of the complexes which supported by calculating the ligand field parameters for the Co(II) and Fe(III) complexes. The Ni(II) complex has subnormal magnetic moment (0.71 BM) indicative of a mixed stereochemistry of square-planar and tetrahedral structure. [Cu(HBTS-2H)] measured 0.93 BM indicating high interaction between the copper centers. The ligand may be ordered at the top of the spectrochemical series which giving high ligand field splitting energy (10 Dq=17,900 cm(-1) for Co2+ complex). The mass spectra of some complexes proved their stable chemical formulae while the TGA depicts the degradation steps and the final residue. In evaporating the mother liquor during the preparation of HBTS, new compound is obtained naming 1-(2,5-dimethyl-1H-pyrrol-yl)thiourea and its crystal was solved. PMID:24813284

  13. Coordination of Fe(III), Co(II), Ni(II), Cu(II), Zn(II), Cd(II), Hg(II), Pd(II) and Pt(II) with 2,5-hexanedione bis(thiosemicarbazone), HBTS: Crystal structure of cis-[Pd(HBTS)]Cl2 and 1-(2,5-dimethyl-1H-pyrrol-yl)-thiourea

    Jeragh, Bakir; El-Asmy, Ahmed A.

    2014-09-01

    Metal complexes of Fe3+, Co2+, Ni2+, Cu2+, Zn2+, Cd2+, Hg2+, Pd2+ or Pt2+ with 2,5-hexanedione bis(thiosemicarbazone), HBTS; have been prepared and spectroscopically investigated. The empirical formulae of the complexes were suggested based on the elemental analysis. Single crystal of Pd(II) has been solved to be cis-form of square-planar geometry by the X-ray crystallography. 1H and 13C NMR spectra have been recorded for HBTS, Zn(II), Cd(II), Hg(II), Pd(II) and Pt(II) complexes, in DMSO-d6, showing the mode of chelation. The ligand acts as a neutral or a binegative tetradentate (N2S2) or neutral bidentate on the basis of FT-IR. The magnetic moments and electronic spectra provide information about the geometry of the complexes which supported by calculating the ligand field parameters for the Co(II) and Fe(III) complexes. The Ni(II) complex has subnormal magnetic moment (0.71 BM) indicative of a mixed stereochemistry of square-planar and tetrahedral structure. [Cu(HBTS-2H)] measured 0.93 BM indicating high interaction between the copper centers. The ligand may be ordered at the top of the spectrochemical series which giving high ligand field splitting energy (10Dq = 17,900 cm-1 for Co2+ complex). The mass spectra of some complexes proved their stable chemical formulae while the TGA depicts the degradation steps and the final residue. In evaporating the mother liquor during the preparation of HBTS, new compound is obtained naming 1-(2,5-dimethyl-1H-pyrrol-yl)thiourea and its crystal was solved.

  14. Synthesis by plasma and characterization of compounds derived from polyacetylene

    This work presents a study on, the synthesis by plasma and the characterization of an aliphatic conjugated polymer, polyacetylene-chlorinated (Pac), and two aromatic polymers, Poly pyrrole (P Py-Cl) and Poly thiophene (Pth-Cl) synthesized with chlorine and the electrical conductivity. The last two polymers were synthesized to compare the chlorine-polymer interaction in aliphatic and aromatic polymers synthesized by plasma and their repercussion on the electrical transport of charges in the material. The structure and morphology of the polymers were studied using scanning electron microscopy (Sem), energy dispersive spectroscopy (EDS), infrared spectroscopy (Ft-IR), conductivity analysis and X-Ray photon spectroscopy (XPS). The results showed that Pac is soluble in acetone and other organic solvents, which indicates a low proportion of crosslinking in the polymers. This point is important because the crosslinking reduces the electrical conductivity in the material. The Pac conductivity is in the range of 1 x 10-12 to 6 x 10-4 S/cm in the internal of 35- 90% of relative humidity. A possible mechanism for the transport of electrical charges in Pac is by means of the double and simple conjugated bonds in the polymers. Pth-Cl and P Py-Cl present electric conductivity in the interval of 9 x 10-5 to 1 x 10-2 S/cm and show a great dependence on the relative humidity. The chlorine addition in these polymers was through simultaneous polymerization with chloroform. This last compound can decompose if the energy of the plasma is relatively high, and the fragments can link to the polymer in a hybrid process of copolymerization. An important point of this work is that the polymer is soluble, a difference of the obtained via plasma as the poli aniline, P Py-CI and Pth-Cl both studied in this work. If took in account that the Pac is single the monomer and that P Py-Cl and Pth-CI is affected by the chlorine that modifies the conductivity of the material, then Pac presents an

  15. Detailed characterizations of the new Mines Douai comparative reactivity method instrument via laboratory experiments and modeling

    Michoud, V.; Hansen, R. F.; Locoge, N.; Stevens, P. S.; Dusanter, S.

    2015-08-01

    The hydroxyl (OH) radical is an important oxidant in the troposphere, which controls the lifetime of most air quality- and climate-related trace gases. However, there are still uncertainties concerning its atmospheric budget, and integrated measurements of OH sinks have been valuable to improve this aspect. Among the analytical tools used for measuring total OH reactivity in ambient air, the comparative reactivity method (CRM) is spreading rapidly in the atmospheric community. However, measurement artifacts have been highlighted for this technique, and additional work is needed to fully characterize them. In this study, we present the new Mines Douai CRM instrument, with an emphasis on the corrections that need to be applied to ambient measurements of total OH reactivity. Measurement artifacts identified in the literature have been investigated, including (1) a correction for a change in relative humidity between the measurement steps leading to different OH levels, (2) the formation of spurious OH in the sampling reactor when hydroperoxy radicals (HO2) react with nitrogen monoxide (NO), (3) not operating the CRM under pseudo-first-order kinetics, and (4) the dilution of ambient air inside the reactor. The dependences of these artifacts on various measurable parameters, such as the pyrrole-to-OH ratio and the bimolecular reaction rate constants of ambient trace gases with OH, have also been studied. Based on these observations, parameterizations are proposed to correct ambient OH reactivity measurements. On average, corrections of 5.2 ± 3.2, 9.2 ± 15.7, and 8.5 ± 5.8 s-1 were respectively observed for (1), (2) and (3) during a field campaign performed in Dunkirk, France (summer 2014). Numerical simulations have been performed using a box model to check whether experimental observations mentioned above are consistent with our understanding of the chemistry occurring in the CRM reactor. Two different chemical mechanisms have been shown to reproduce the magnitude

  16. Full characterization of polypyrrole thin films electrosynthesized in room temperature ionic liquids, water or acetonitrile

    Highlights: • Polypyrrole films were electrodeposited from three room temperature ionic liquids. • Polymer films were characterized using many surface analysis techniques. • The incorporation of anions and/or cations inside the polymer films was evidenced. • The influence of the ionic liquid on the polymer properties was deeply studied. - Abstract: Pyrrole was electrochemically oxidized in two conventional media (water and acetonitrile) and in three room temperature ionic liquids: 1-butyl-3-methylimidazolium hexafluorophosphate, 1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide, and 1-butyl-1-methylpyrrolidinium bis(trifluoromethanesulfonyl)imide. Infrared and Raman Spectroscopies confirmed the formation of polypyrrole by electropolymerization but were unable to demonstrate the presence of anions in the polymer films. The use of ionic liquids as growth media resulted in polymer films having a good electrochemical activity. The difference of activity from one polymer film to the other was mainly attributed to the difference of viscosity between the solvents used. The morphological features of the polypyrrole films were also fully studied. Profilometric measurements demonstrated that polymer films grown, at the same potential, in ionic liquids were thinner and had a smaller roughness than those grown in other solvents. Atomic Force Microscopy showed that polypyrrole films had nearly similar micrometric nodular structure whatever the growth medium even if some differences of porosity and homogeneity were observed using Scanning Electron Microscopy. The incorporation of counter-anions at the top surface of the films was finally evidenced by X-ray Photoelectron Spectroscopy. These anions were also incorporated inside the polymer film with a uniform distribution as shown by Glow Discharge Optical Emission Spectroscopy

  17. Old and new pharmacology: positive allosteric modulation of the alpha7 nicotinic acetylcholine receptor by the 5-hydroxytryptamine(2B/C) receptor antagonist SB-206553 (3,5-dihydro-5-methyl-N-3-pyridinylbenzo[1,2-b:4,5-b']di pyrrole-1(2H)-carboxamide).

    Dunlop, John; Lock, Tim; Jow, Brian; Sitzia, Fabrizio; Grauer, Steven; Jow, Flora; Kramer, Angela; Bowlby, Mark R; Randall, Andrew; Kowal, Dianne; Gilbert, Adam; Comery, Thomas A; Larocque, James; Soloveva, Veronica; Brown, Jon; Roncarati, Renza

    2009-03-01

    The alpha7 nicotinic acetylcholine receptor (nAChR) has been implicated in Alzheimer's disease and schizophrenia, leading to efforts targeted toward discovering agonists and positive allosteric modulators (PAMs) of this receptor. In a Ca2+ flux fluorometric imaging plate reader assay, SB-206553 (3,5-dihydro-5-methyl -N-3-pyridinylbenzo [1, 2-b:4,5 -b']-di pyrrole-1(2H)-carboxamide), a compound known as a 5-hydroxytryptamine(2B/2C) receptor antagonist, produced an 8-fold potentiation of the evoked calcium signal in the presence of an EC(20) concentration of nicotine and a corresponding EC(50) of 1.5 muM for potentiation of EC(20) nicotine responses in GH4C1 cells expressing the alpha7 receptor. SB-206553 was devoid of direct alpha7 receptor agonist activity and selective against other nicotinic receptors. Confirmation of the PAM activity of SB-206553 on the alpha7 nAChR was obtained in patch-clamp electrophysiological experiments in GH4C1 cells, where it failed to evoke any detectable currents when applied alone, yet dramatically potentiated the currents evoked by an EC(20) (17 microM) and EC(100) (124 microM) of acetylcholine (ACh). Native nicotinic receptors in CA1 stratum radiatum interneurons of rat hippocampal slices could also be activated by ACh (200 microM), an effect that was entirely blocked by the alpha7-selective antagonist methyllycaconitine (MLA). These ACh currents were potentiated by SB-206553, which increased the area of the current response significantly, resulting in a 40-fold enhancement at 100 microM. In behavioral experiments in rats, SB-206553 reversed an MK-801 (dizocilpine maleate)-induced deficit in the prepulse inhibition of acoustic startle response, an effect attenuated in the presence of MLA. This latter observation provides further evidence in support of the potential therapeutic utility of alpha7 nAChR PAMs in schizophrenia. PMID:19050173

  18. Preparation and characterization of electronically conducting polypyrrole-montmorillonite nanocomposite and its potential application as a cathode material for oxygen reduction

    Simple wet chemical processes were deployed to prepare low-cost conducting nanocomposites based on natural clays with 2:1 layered structures such as sodium montmorillonite (MMT). Ce(IV) modified MMT was used for the spontaneous polymerization of pyrrole within clay interlayers. The resulted clay-conducting polypyrrole nanocomposites containing the reduced form of the oxidising agent, have been extensively characterized by X-ray diffraction (XRD) technique for interlayer spacing variations and by Fourier transform infra red (FT-IR) spectroscopy to study the interactions between the clay and polymer functional groups. DC polarization technique with both blocking and non-blocking electrodes was used to distinguish between the ionic and electronic transport numbers and to recognize the type of mobile ionic species. AC impedance analysis further resolved the electrical conduction of these materials. Bulk conductivity analysis implied that the polypyrrole (PPY) formed within Ce(IV) modified MMT posses dominant electronic conductivity. The low-cost, light-weight and stable polymer-clay nanocomposite prepared by Ce(IV) intercalated MMT, [Ce(III)-PPY-MMT], seems to be a promising cathode material for oxygen reduction and hence may find applications in fuel cell industries.

  19. Practical materials characterization

    2014-01-01

    Presents cross-comparison between materials characterization techniquesIncludes clear specifications of strengths and limitations of each technique for specific materials characterization problemFocuses on applications and clear data interpretation without extensive mathematics

  20. Hybride magnetic nanostructure based on amino acids functionalized polypyrrole

    Conducting polypyrrole is especially promising for many commercial applications because of its unique optical, electric, thermal and mechanical properties. We report the synthesis and characterization of novel pyrrole functionalized monomers and core-shell hybrid nanostructures, consisting of a conjugated polymer layer (amino acids functionalized pyrrole copolymers) and a magnetic nanoparticle core. For functionalization of the pyrrole monomer we used several amino acids: tryptophan, leucine, phenylalanine, serine and tyrosine. These amino acids were linked via different types of hydrophobic linkers to the nitrogen atom of the pyrrole monomer. The magnetic core-shell hybrid nanostructures are characterized by various methods such as FTIR spectroscopy, transmission electron microscopy (TEM) and magnetic measurements

  1. Hybride magnetic nanostructure based on amino acids functionalized polypyrrole

    Nan, Alexandrina, E-mail: alexandrina.nan@itim-cj.ro; Bunge, Alexander; Turcu, Rodica [National Institute for Research and Development of Isotopic and Molecular Technologies, 67-103 Donat, 400293 Cluj-Napoca (Romania)

    2015-12-23

    Conducting polypyrrole is especially promising for many commercial applications because of its unique optical, electric, thermal and mechanical properties. We report the synthesis and characterization of novel pyrrole functionalized monomers and core-shell hybrid nanostructures, consisting of a conjugated polymer layer (amino acids functionalized pyrrole copolymers) and a magnetic nanoparticle core. For functionalization of the pyrrole monomer we used several amino acids: tryptophan, leucine, phenylalanine, serine and tyrosine. These amino acids were linked via different types of hydrophobic linkers to the nitrogen atom of the pyrrole monomer. The magnetic core-shell hybrid nanostructures are characterized by various methods such as FTIR spectroscopy, transmission electron microscopy (TEM) and magnetic measurements.

  2. Waste Characterization Methods

    Vigil-Holterman, Luciana R. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Naranjo, Felicia Danielle [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2016-02-02

    This report discusses ways to classify waste as outlined by LANL. Waste Generators must make a waste determination and characterize regulated waste by appropriate analytical testing or use of acceptable knowledge (AK). Use of AK for characterization requires several source documents. Waste characterization documentation must be accurate, sufficient, and current (i.e., updated); relevant and traceable to the waste stream’s generation, characterization, and management; and not merely a list of information sources.

  3. N-Nitro-1H-pyrrole-2-carboxamide

    Long Liu; Chunlin He; Zengxi Li; Chunshan Li; Xiangping Zhang; Suojiang Zhang

    2011-01-01

    In the title compound, C5H5N3O3, the nitro group is twisted with respect to the amide group, with C—N—N—O torsion angles of 29.0 (2) and −153.66 (14)°. In the crystal, molecules are linked through intermolecular N—H...O and C—H...O hydrogen bonds, forming supramolecular chains along the a axis. These chains stack in parallel and form distinct layer motifs in the (001) plane.

  4. N-Nitro-1H-pyrrole-2-carboxamide

    Long Liu

    2011-02-01

    Full Text Available In the title compound, C5H5N3O3, the nitro group is twisted with respect to the amide group, with C—N—N—O torsion angles of 29.0 (2 and −153.66 (14°. In the crystal, molecules are linked through intermolecular N—H...O and C—H...O hydrogen bonds, forming supramolecular chains along the a axis. These chains stack in parallel and form distinct layer motifs in the (001 plane.

  5. GLOVEBOX GLOVE CHARACTERIZATION SUMMARY

    Korinko, P.

    2012-05-14

    A task was undertaken to determine primarily the permeation behavior of various glove compounds from four manufacturers. As part of the basic characterization task, the opportunity to obtain additional mechanical and thermal properties presented itself. Consequently, a total of fifteen gloves were characterized for permeation, Thermogravimetric Analysis, Puncture Resistance, Tensile Properties and Dynamic Mechanical Analysis. Detailed reports were written for each characterization technique used. This report contains the summary of the results.

  6. Materials Characterization Facility

    Federal Laboratory Consortium — The Materials Characterization Facility enables detailed measurements of the properties of ceramics, polymers, glasses, and composites. It features instrumentation...

  7. Characterization of revenue equivalence

    Heydenreich, B.; Müller, R.; Uetz, M.J.; Vohra, R.

    2009-01-01

    The property of an allocation rule to be implementable in dominant strategies by a unique payment scheme is called revenue equivalence. We give a characterization of revenue equivalence based on a graph theoretic interpretation of the incentive compatibility constraints. The characterization holds f

  8. Characterizations of Exponentiated Distributions

    gholamhossein g hamedani

    2013-01-01

    Variuos characterizations of the class of exponentiated distributions are presented.  These characterizations are based on a simple relationship between two truncated moments and based on functions of the nth order statistic.  The results are applied to certain well-known members of this class.

  9. Isocyanide or nitrosyl complexation to hemes with varying tethered axial base ligand donors: synthesis and characterization.

    Sharma, Savita K; Kim, Hyun; Rogler, Patrick J; A Siegler, Maxime; Karlin, Kenneth D

    2016-09-01

    A series of ferrous-heme 2,6-dimethylphenyl isocyanide (DIMPI) and ferrous-heme mononitrosyl complexes have been synthesized and characterized. The heme portion of the complexes studied is varied with respect to the nature of the axial ligand, including complexes, where it is covalently tethered to the porphyrinate periphery. Reduced heme complexes, [(F8)Fe(II)], [(P(Py))Fe(II)], [(P(Im))Fe(II)], and [(P(ImH))Fe(II)], where F8 = tetrakis(2,6-difluorophenyl)-porphyrinate and P(Py), P(Im), and P(ImH) are partially fluorinated tetraaryl porphyrinates with covalently appended axial base pyridyl/imidazolyl or histamine moieties, were employed; P(ImH) is a new construct. Room temperature addition of DIMPI to these iron(II) complexes affords the bis-isocyanide species [(F8)Fe(II)-(DIMPI)2] in the case of [(F8)Fe(II)], while for the other hemes, mono-DIMPI compounds are obtained, [(P(Py))Fe(II)-(DIMPI)] [(2)-DIMPI], [(P(Im))Fe(II)-(DIMPI)] [(3)-DIMPI], and [(P(ImH))Fe(II)-(DIMPI)] [(4)-DIMPI]. The structures of complexes (3)-DIMPI and (4)-DIMPI have been determined by single crystal X-ray crystallography, where interesting H…F(porphryinate aryl group) interactions are observed. (19)F-NMR spectra determined for these complexes suggest that H…F(porphyrinate aryl groups) attractions also occur in solution, the H atom coming either from the DIMPI methyl groups or from a porphyinate axial base imidazole or porphyrinate pyrrole. Similarly, we have used nitrogen monoxide to generate ferrous-nitrosyl complexes, a five-coordinate species for F8, [(F8)Fe(II)-(NO)], or low-spin six-coordinate compounds [(P(Py))Fe(II)-(NO)], [(P(Im))Fe(II)-(NO)], and [(P(ImH))Fe(II)-(NO)]. The DIMPI and mononitrosyl complexes have also been characterized using UV-Vis, IR, (1)H-NMR, and EPR spectroscopies. PMID:27350154

  10. Novel conductive polypyrrole/zinc oxide/chitosan bionanocomposite: synthesis, characterization, antioxidant, and antibacterial activities

    Ebrahimiasl S

    2014-12-01

    Full Text Available Saeideh Ebrahimiasl,1,2 Azmi Zakaria,3 Anuar Kassim,4 Sri Norleha Basri4 1Department of Nanotechnology, Institute of Advanced Technology, Universiti Putra Malaysia, Serdang, Malaysia; 2Department of Chemistry, Ahar Branch, Islamic Azad University, Ahar, Iran; 3Department of Physics, Universiti Putra Malaysia, Serdang, Malaysia; 4Department of Chemistry, Universiti Putra Malaysia, Serdang, Malaysia Abstract: An antibacterial and conductive bionanocomposite (BNC film consisting of polypyrrole (Ppy, zinc oxide (ZnO nanoparticles (NPs, and chitosan (CS was electrochemically synthesized on indium tin oxide (ITO glass substrate by electrooxidation of 0.1 M pyrrole in aqueous solution containing appropriate amounts of ZnO NPs uniformly dispersed in CS. This method enables the room temperature electrosynthesis of BNC film consisting of ZnO NPs incorporated within the growing Ppy/CS composite. The morphology of Ppy/ZnO/CS BNC was characterized by scanning electron microscopy. ITO–Ppy/CS and ITO–Ppy/ZnO/CS bioelectrodes were characterized using the Fourier transform infrared technique, X-ray diffraction, and thermogravimetric analysis. The electrical conductivity of nanocomposites was investigated by a four-probe method. The prepared nanocomposites were analyzed for antioxidant activity using the 2,2-diphenyl-1-picrylhydrazyl assay. The results demonstrated that the antioxidant activity of nanocomposites increased remarkably by addition of ZnO NPs. The electrical conductivity of films showed a sudden decrease for lower weight ratios of ZnO NPs (5 wt%, while it was increased gradually for higher ratios (10, 15, and 20 wt%. The nanocomposites were analyzed for antibacterial activity against Gram-positive and Gram-negative bacteria. The results indicated that the synthesized BNC is effective against all of the studied bacteria, and its effectiveness is higher for Pseudomonas aeruginosa. The thermal stability and physical properties of BNC films were

  11. Panel 3 - characterization

    Erck, R.A.; Erdemir, A.; Janghsing Hsieh; Lee, R.H.; Xian Zheng Pan; Deming Shu [Argonne National Lab., IL (United States); Feldman, A. [National Inst. of Standards and Technology, Gaithersburg, MD (United States); Glass, J.T. [North Carolina State Univ., Raleigh (United States); Kleimer, R. [Coors Ceramics Co., Golden, CO (United States); Lawton, E.A. [JPL/Caltech, Pasadena, CA (United States); McHargue, C.J. [Univ. of Tennessee, Knoxville (United States)

    1993-01-01

    The task of this panel was to identify and prioritize needs in the area of characterization of diamond and diamond-like-carbon (DLC) films for use in the transportation industry. Until recent advances in production of inexpensive films of diamonds and DLC, it was not feasible that these materials could be mass produced. The Characterization Panel is restricting itself to identifying needs in areas that would be most useful to manufacturers and users in producing and utilizing diamond and DLC coatings in industry. These characterization needs include in-situ monitoring during growth, relation of structure to performance, and standards and definitions.

  12. Characterization of nanomaterials

    This paper provides an overview of the main techniques used for the characterization of nanomaterials. The knowledge of some basic characteristics, inherent morphology, microstructure, the distribution phase and chemical composition, it is essential to evaluate the functional properties of nanomaterials and make predictions about their behavior in operation. For the characterization of nanomaterials can be used in both imaging techniques both analytic techniques. Among the first found wide application optical microscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Among the latter some types of spectroscopy and X-ray diffraction (XRD). For each type of material to characterize the choice of the most appropriate technique it is based on the type of details that you want to obtain, and on their scale. In this paper are discussed in detail some examples and the main methods used for the characterization of nanomaterials.

  13. How to characterize disorder

    Egami, T.

    2016-05-01

    Researchers working on nuclear materials encounter disorder in the atomic structure all the time, usually caused by irradiation. The nature of disorder varies widely, from lattice defects to amorphous phase formation. Generally it is not easy to characterize the state of disorder with the accuracy necessary to elucidate the properties caused by structural disorder. However, owing to advances in the tools of characterization and rapid rise in computer power, significant progress has been made in characterizing structural disorder. We discuss how to describe and determine the structure and dynamics of disordered materials using scattering measurements and modeling. Lattice defects caused by irradiation usually has negative effects on properties, but glasses and highly disordered materials can be irradiation resistant, and could be useful as nuclear materials. Characterizing and controlling disorder is becoming an important endeavor in the field of nuclear materials.

  14. Characterization of revenue equivalence

    Heydenreich, Birgit; Müller, Rudolf; Uetz, Marc

    2007-01-01

    The property of an allocation rule to be implementable in dominant strategies by a unique payment scheme is called revenue equivalence. In this paper we give a characterization of revenue equivalence based on a graph theoretic interpretation of the incentive compatibility constraints. The characterization holds for any (possibly in¯nite) outcome space and many of the known results about revenue equivalence are immediate consequences.

  15. Characterization of Revenue Equivalence

    Heydenreich, B.; Müller, R.J.; Uetz, M.J.; R. Vohra

    2008-01-01

    The property of an allocation rule to be implementable in dominant strategies by a unique payment scheme is called \\emph{revenue equivalence}. In this paper we give a characterization of revenue equivalence based on a graph theoretic interpretation of the incentive compatibility constraints. The characterization holds for any (possibly infinite) outcome space and many of the known results are immediate consequences. Moreover, revenue equivalence can be identified in cases where existing theor...

  16. Site characterization handbook

    1988-06-01

    This Handbook discusses both management and technical elements that should be considered in developing a comprehensive site characterization program. Management elements typical of any project of a comparable magnitude and complexity are combined with a discussion of strategies specific to site characterization. Information specific to the technical elements involved in site characterization is based on guidance published by the Nuclear Regulatory Commission (NRC) with respect to licensing requirements for LLW disposal facilities. The objective of this Handbook is to provide a reference for both NRC Agreement States and non-Agreement States for use in developing a comprehensive site characterization program that meets the specific objectives of the State and/or site developer/licensee. Each site characterization program will vary depending on the objectives, licensing requirements, schedules/budgets, physical characteristics of the site, proposed facility design, and the specific concerns raised by government agencies and the public. Therefore, the Handbook is not a prescriptive guide to site characterization. 18 refs., 6 figs.

  17. Space Solar Cell Characterization Laboratory

    Federal Laboratory Consortium — FUNCTION: Measures, characterizes, and analyzes photovoltaic materials and devices. The primary focus is the measurement and characterization of solar cell response...

  18. Site characterization plan:

    The Yucca Mountain site in Nevada is one of three candidate sites for the first geologic repository for radioactive waste. On May 28, 1986, it was recommended for detailed study in a program of site characterization. This site characterization plan (SCP) has been prepared in acordance with the requirements of the Nuclear Waste Policy Act to summarize the information collected to date about the geologic conditions at the site;to describe the conceptual designs for the repository and the waste package and to present the plans for obtaining the geologic information necessary to demonstrate the suitability of the site for a repository, to design the repository and the waste package, to prepare an environmental impact statement, and to obtain from the US Nuclear Regulatory Commission (NRC) an authorization to construct the repository. This introduction begins with a brief section on the process for siting and eveloping a repository, followed by a discussion of the pertinent legislation and regulations. A description of site characterization is presented next;it describes the facilities to be constructed for the site characterization program and explains the principal activities to be conducted during the program. Finally, the purpose, content, organizing prinicples, and organization of this site characterization plan are outlined, and compliance with applicable regulations is discussed. 880 refs., 130 figs., 25 tabs

  19. Site characterization plan:

    The Yucca Mountain site in Nevada is one of three candidate sites for the first geologic repository for radioactive waste. On May 28, 1986, it was recommended for detailed study in a program of site characterization. This site characterization plan (SCP) has been prepared in accordance with the requirements of the Nuclear Waste Policy Act to summarize the information collected to date about the geologic conditions at the site;to describe the conceptual designs for the repository and the waste package;and to present the plans for obtaining the geologic information necessary to demonstrate the suitability of the site for repository, to design the repository and the waste package, to prepare an environmental impact statement, and to obtain from the US Nuclear Regulatory Commission (NRC) an authorization to construct the repository. This introduction begins with a brief section on the process for siting and developing a repository, followed by a discussion of the pertinent legislation and regulations. A description of site characterization is presented next;it describes the facilities to be constructed for the site characterization program and explains the principal activities to be conducted during the program. Finally, the purpose, content, organizing principles, and organization of this site characterization plan are outlined, and compliance with applicable regulations is discussed

  20. Monodisperse metal nanoparticle catalysts on silica mesoporous supports: synthesis, characterizations, and catalytic reactions

    Somorjai, G.A.

    2009-09-14

    The design of high performance catalyst achieving near 100% product selectivity at maximum activity is one of the most important goals in the modern catalytic science research. To this end, the preparation of model catalysts whose catalytic performances can be predicted in a systematic and rational manner is of significant importance, which thereby allows understanding of the molecular ingredients affecting the catalytic performances. We have designed novel 3-dimensional (3D) high surface area model catalysts by the integration of colloidal metal nanoparticles and mesoporous silica supports. Monodisperse colloidal metal NPs with controllable size and shape were synthesized using dendrimers, polymers, or surfactants as the surface stabilizers. The size of Pt, and Rh nanoparticles can be varied from sub 1 nm to 15 nm, while the shape of Pt can be controlled to cube, cuboctahedron, and octahedron. The 3D model catalysts were generated by the incorporation of metal nanoparticles into the pores of mesoporous silica supports via two methods: capillary inclusion (CI) and nanoparticle encapsulation (NE). The former method relies on the sonication-induced inclusion of metal nanoparticles into the pores of mesoporous silica, whereas the latter is performed by the encapsulation of metal nanoparticles during the hydrothermal synthesis of mesoporous silica. The 3D model catalysts were comprehensively characterized by a variety of physical and chemical methods. These catalysts were found to show structure sensitivity in hydrocarbon conversion reactions. The Pt NPs supported on mesoporous SBA-15 silica (Pt/SBA-15) displayed significant particle size sensitivity in ethane hydrogenolysis over the size range of 1-7 nm. The Pt/SBA-15 catalysts also exhibited particle size dependent product selectivity in cyclohexene hydrogenation, crotonaldehyde hydrogenation, and pyrrole hydrogenation. The Rh loaded SBA-15 silica catalyst showed structure sensitivity in CO oxidation reaction. In

  1. Tank characterization reference guide

    Characterization of the Hanford Site high-level waste storage tanks supports safety issue resolution; operations and maintenance requirements; and retrieval, pretreatment, vitrification, and disposal technology development. Technical, historical, and programmatic information about the waste tanks is often scattered among many sources, if it is documented at all. This Tank Characterization Reference Guide, therefore, serves as a common location for much of the generic tank information that is otherwise contained in many documents. The report is intended to be an introduction to the issues and history surrounding the generation, storage, and management of the liquid process wastes, and a presentation of the sampling, analysis, and modeling activities that support the current waste characterization. This report should provide a basis upon which those unfamiliar with the Hanford Site tank farms can start their research

  2. Characterization of leaky faults

    Leaky faults provide a flow path for fluids to move underground. It is very important to characterize such faults in various engineering projects. The purpose of this work is to develop mathematical solutions for this characterization. The flow of water in an aquifer system and the flow of air in the unsaturated fault-rock system were studied. If the leaky fault cuts through two aquifers, characterization of the fault can be achieved by pumping water from one of the aquifers, which are assumed to be horizontal and of uniform thickness. Analytical solutions have been developed for two cases of either a negligibly small or a significantly large drawdown in the unpumped aquifer. Some practical methods for using these solutions are presented. 45 refs., 72 figs., 11 tabs

  3. Geostatistics for fracture characterization

    As the critical role of fractures has become more apparent in fluid flow and contaminant transport studies, the characterization of fracture networks has received considerable attention in a wide variety of applications such as nuclear waste repository design. The application of geostatistics to fracture characterization has traditionally involved modelling fractures as thin disks; assumptions about the frequency, orientation, length and width of these disks allow the construction of a 3D model of the fracture network. This paper examines alternatives whose statistical parameters are more relevant for contaminant transport studies and are also easier to infer and validate. A new algorithm for conditional simulation is presented, one that is able to honor multipoint statistics through annealing. By honoring statistics that capture with two-point spatial convariances, this algorithm offers an important new tool not only for the specific problem of fracture characterization but also for the more general problem of spatial simulation

  4. Preparation and characterization of a composite hydrogel with graphene oxide as an acid catalyst.

    Jiang, Ting; Sui, Zhu-Yin; Yang, Quan-Sheng; Zhang, Xuetong; Han, Bao-Hang

    2015-04-28

    In this study, a facile method for synthesizing a novel graphene oxide/pyrrole-formaldehyde (GOP-1) composite hydrogel was developed via in situ polymerization of pyrrole and formaldehyde in the presence of graphene oxide sheets without any additional catalyst. During the polymerization, graphene oxide can act as a two-dimensional template to regulate the aggregation state of polymer and as an acid catalyst to accelerate the reaction rate of pyrrole and formaldehyde. The morphology and microstructure were investigated by scanning electron microscopy, transmission electron microscopy, and X-ray diffraction, respectively. The chemical properties were analyzed via X-ray photoelectron spectroscopy, infrared spectroscopy, and Raman spectroscopy. The freeze-dried GOP-1 composite hydrogel exhibited a large specific surface area, high nitrogen content, and three-dimensional network structure. Based on the above features, the freeze-dried GOP-1 composite hydrogel used as a gas adsorbent showed a high carbon dioxide uptake capacity at 1.0 bar and 273 K (11.1 wt%), in sharp contrast to that of graphene oxide (7.4 wt%). Furthermore, the as-prepared composite hydrogel may possess attractive potential in the fields of electrode material, tissue engineering, and water treatment. PMID:25760407

  5. Characterizing teleportation in optics

    Ralph, T. C.; Polkinghorne, R. E. S.; Lam, P.K.

    1999-01-01

    We discuss the characterization of continuous variable, optical quantum teleportation in terms of the two quadrature signal transfer and conditional variances between the input and output states. We derive criteria which clearly define the classical limits and highlight interesting operating points which are not obvious from a calculation of the fidelity of the teleportation alone.

  6. Characterization of Photovoltaic Generators

    Boitier, V.; Cressault, Y.

    2011-01-01

    This paper discusses photovoltaic panel systems and reviews their electrical properties and use in several industrial fields. We explain how different photovoltaic panels may be characterized by undergraduate students at university using simple methods to retrieve their electrical properties (power, current and voltage) and compare these values…

  7. Characterization of revenue equivalence

    Heydenreich, Birgit; Müller, Rudolf; Uetz, Marc; Vohra, Rakesh

    2008-01-01

    The property of an allocation rule to be implementable in dominant strategies by a unique payment scheme is called \\emph{revenue equivalence}. In this paper we give a characterization of revenue equivalence based on a graph theoretic interpretation of the incentive compatibility constraints. The cha

  8. Signal integrity characterization techniques

    Bogatin, Eric

    2009-01-01

    "Signal Integrity Characterization Techniques" addresses the gap between traditional digital and microwave curricula all while focusing on a practical and intuitive understanding of signal integrity effects within the data transmission channel. High-speed interconnects such as connectors, PCBs, cables, IC packages, and backplanes are critical elements of differential channels that must be designed using today's most powerful analysis and characterization tools.Both measurements and simulation must be done on the device under test, and both activities must yield data that correlates with each other. Most of this book focuses on real-world applications of signal integrity measurements - from backplane for design challenges to error correction techniques to jitter measurement technologies. The authors' approach wisely addresses some of these new high-speed technologies, and it also provides valuable insight into its future direction and will teach the reader valuable lessons on the industry.

  9. Characterization of shocked beryllium

    Explosively driven arrested beryllium experiments were performed with post mortem characterization to evaluate the failure behaviors. The test samples were encapsulated in an aluminum assembly that was large relative to the sample, and the assembly features both axial and radial momentum traps. The sample carrier was inserted from the explosively-loaded end and has features to lock the carrier to the surrounding cylinder using the induced plastic flow. Calculations with Lagrangian codes showed that the tensile stresses experienced by the Be sample were below the spall stress. Metallographic characterization of the arrested Be showed radial cracks present in the samples may have been caused by bending moments. Fractography showed the fractures propagated from the side of the sample closest to the explosives, the side with the highest tensile stress. There was evidence that the fractures may have propagated from the circumferential crack outward and downward radially.

  10. Site characterization techniques

    U.S. Geological Survey

    1995-01-01

    Geoelectrical methods have been used since the 1920's to search for metallic ore deposits. During the last decade, traditional mining geophysical techniques have been adapted for environmental site characterization. Geoelectrical geophysics is now a well developed engineering specialty, with different methods to focus both on a range of targets and on depths below the surface. Most methods have also been adapted to borehole measurements.

  11. Probabilistic Logical Characterization

    Hermanns, Holger; Parma, Augusto; Segala, Roberto; Wachter, Björn; Zhang, Lijun

    2011-01-01

    Probabilistic automata exhibit both probabilistic and non-deterministic choice. They are therefore a powerful semantic foundation for modeling concurrent systems with random phenomena arising in many applications ranging from artificial intelligence, security, systems biology to performance model...... modeling. Several variations of bisimulation and simulation relations have proved to be useful as means to abstract and compare different automata. This paper develops a taxonomy of logical characterizations of these relations on image-finite and image-infinite probabilistic automata....

  12. Unary Resolution: Characterizing Ptime.

    Seiller, Thomas; Aubert, Clément; Bagnol, Marc

    2016-01-01

    We give a characterization of deterministic polynomial time computation based on an algebraic structure called the resolution semiring, whose elements can be understood as logic programs or sets of rewriting rules over first-order terms. This construction stems from an interactive interpretation of the cut-elimination procedure of linear logic known as the geometry of interaction.This framework is restricted to terms (logic programs, rewriting rules) using only unary symbols, and this restric...

  13. VECSEL gain characterization

    Mangold, Mario; Wittwer, Valentin J; Sieber, Oliver D.; Hoffmann, Martin; Krestnikov, Igor L; Livshits, Daniil A.; Golling, Matthias; Südmeyer, Thomas; Keller, Ursula

    2012-01-01

    We present the first full gain characterization of two vertical external cavity surface emitting laser (VECSEL) gain chips with similar designs operating in the 960-nm wavelength regime. We optically pump the structures with continuous-wave (cw) 808-nm radiation and measure the nonlinear reflectivity for 130-fs and 1.4-ps probe pulses as function of probe pulse fluence, pump power, and heat sink temperature. With this technique we are able to measure the saturation behavior for VECSEL gain ch...

  14. ATR neutron spectral characterization

    The Advanced Test Reactor (ATR) at INEL provides intense neutron fields for irradiation-effects testing of reactor material samples, for production of radionuclides used in industrial and medical applications, and for scientific research. Characterization of the neutron environments in the irradiation locations of the ATR has been done by means of neutronics calculations and by means of neutron dosimetry based on the use of neutron activation monitors that are placed in the various irradiation locations. The primary purpose of this report is to present the results of an extensive characterization of several ATR irradiation locations based on neutron dosimetry measurements and on least-squares-adjustment analyses that utilize both neutron dosimetry measurements and neutronics calculations. This report builds upon the previous publications, especially the reference 4 paper. Section 2 provides a brief description of the ATR and it tabulates neutron spectral information for typical irradiation locations, as derived from the more historical neutron dosimetry measurements. Relevant details that pertain to the multigroup neutron spectral characterization are covered in section 3. This discussion includes a presentation on the dosimeter irradiation and analyses and a development of the least-squares adjustment methodology, along with a summary of the results of these analyses. Spectrum-averaged cross sections for neutron monitoring and for displacement-damage prediction in Fe, Cr, and Ni are given in section 4. In addition, section4 includes estimates of damage generation rates for these materials in selected ATR irradiation locations. In section 5, the authors present a brief discussion of the most significant conclusions of this work and comment on its relevance to the present ATR core configuration. Finally, detailed numerical and graphical results for the spectrum-characterization analyses in each irradiation location are provided in the Appendix

  15. Proton Beam Energy Characterization

    Marus, Lauren A.; Engle, J.W.; John, K. D.; Birnbaum, E. R.; Nortier, F. M.

    2015-01-01

    Introduction The Los Alamos Isotope Production Facility (IPF) is actively engaged in the development of isotope production technologies that can utilize its 100 MeV proton beam. Characterization of the proton beam energy and current is vital for optimizing isotope production and accurately conducting research at the IPF. Motivation In order to monitor beam intensity during research irradiations, aluminum foils are interspersed in experimental stacks. A theoretical yield of 22Na from...

  16. Asexuality: Classification and characterization

    Prause, Nicole; Graham, Cynthia A.

    2007-01-01

    This is a post-print version of the article. The official published version can be obtaineed at the link below. The term “asexual” has been defined in many different ways and asexuality has received very little research attention. In a small qualitative study (N = 4), individuals who self-identified as asexual were interviewed to help formulate hypotheses for a larger study. The second larger study was an online survey drawn from a convenience sample designed to better characterize asexual...

  17. Characterizing Individual Communication Patterns

    Malmgren, R. Dean; Hofman, Jake M.; Amaral, Luis A. N.; Watts, Duncan J.

    2009-01-01

    The increasing availability of electronic communication data, such as that arising from e-mail exchange, presents social and information scientists with new possibilities for characterizing individual behavior and, by extension, identifying latent structure in human populations. Here, we propose a model of individual e-mail communication that is sufficiently rich to capture meaningful variability across individuals, while remaining simple enough to be interpretable. We show that the model, a ...

  18. Characterizing Modular Ontologies

    Ben Abbès, Sarra; Scheuermann, Andreas; Meilender, Thomas; D'Aquin, Mathieu

    2012-01-01

    Since large monolithic ontologies are di cult to handle and reuse ontology modularization has attracted increasing attention. Several approaches and tools have been developed to support ontology modularization. Despite these e orts, a lack of knowledge about characteristics of modularly organized ontologies prevents further development. This work aims at characterizing modular ontologies. Therefore, we analyze existing modular ontologies by applying selected metrics from software engineering ...

  19. On Characterizing Particle Shape

    Ennis, Bryan J.; Rickman, Douglas; Rollins, A. Brent; Ennis, Brandon

    2014-01-01

    It is well known that particle shape affects flow characteristics of granular materials, as well as a variety of other solids processing issues such as compaction, rheology, filtration and other two-phase flow problems. The impact of shape crosses many diverse and commercially important applications, including pharmaceuticals, civil engineering, metallurgy, health, and food processing. Two applications studied here include the dry solids flow of lunar simulants (e.g. JSC-1, NU-LHT-2M, OB-1), and the flow properties of wet concrete, including final compressive strength. A multi-dimensional generalized, engineering method to quantitatively characterize particle shapes has been developed, applicable to both single particle orientation and multi-particle assemblies. The two-dimension, three dimension inversion problem is also treated, and the application of these methods to DEM model particles will be discussed. In the case of lunar simulants, flow properties of six lunar simulants have been measured, and the impact of particle shape on flowability - as characterized by the shape method developed here -- is discussed, especially in the context of three simulants of similar size range. In the context of concrete processing, concrete construction is a major contributor to greenhouse gas production, of which the major contributor is cement binding loading. Any optimization in concrete rheology and packing that can reduce cement loading and improve strength loading can also reduce currently required construction safety factors. The characterization approach here is also demonstrated for the impact of rock aggregate shape on concrete slump rheology and dry compressive strength.

  20. Dig Face Characterization

    The Department of Energy (DOE) has numerous sites that contain buried radioactive waste. DOE buried waste sites typically includes transuranic-contaminated (TRU) radioactive waste, low-level radioactive waste (LLW), hazardous waste, mixed TRU waste, and mixed LLW. Waste at these sites was typically disposed of in containers such as steel drums, wooden boxes, and cardboard cartons. The wastes have breached the containers in many instances. Wastes exist in the form of solids, liquids, and sludges. Remediation of these sites will be accomplished using one of three options or some combination thereof. The three options include waste retrieval and ex-situ treatment, in situ treatment, and containment/stabilization. The retrieval and ex situ treatment system is likely considered to be the baseline. However, many uncertainties exist using this approach. The site must first be characterized to assess the problem and design the excavation operations. Real-time characterization during excavation could significantly reduce costs by minimizing the amount of material to be excavated and could significantly reduce the risks to worker safety. Systems to perform real-time characterization data during excavation are needed

  1. Gloss Characterization: a Cyclic Approach

    Viénot, Françoise

    2012-01-01

    In this paper, an approach to gloss characterization is described. We examine how information is transferred from the physical domain to the visual domain and how material properties are inferred from a cognitive interpretation, completing the characterization cycle.

  2. Probabilistic characterization of strong convexity

    Teresa Rajba; Szymon Wąsowicz

    2011-01-01

    Strong convexity is considered for real functions defined on a real interval. Probabilistic characterization is given and its geometrical sense is explained. Using this characterization some inequalities of Jensen-type are obtained.

  3. Measurements and Characterization (Fact Sheet)

    2011-06-01

    Capabilities fact sheet for the National Center for Photovoltaics: Measurements and Characterization that includes scope, core competencies and capabilities, and contact/web information for Analytical Microscopy, Electro-Optical Characterization, Surface Analysis, and Cell and Module Performance.

  4. Network Characterization Service (NCS)

    Jin, Guojun [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Yang, George [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Crowley, Brian [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Agarwal, Deborah [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)

    2001-06-06

    Distributed applications require information to effectively utilize the network. Some of the information they require is the current and maximum bandwidth, current and minimum latency, bottlenecks, burst frequency, and congestion extent. This type of information allows applications to determine parameters like optimal TCP buffer size. In this paper, we present a cooperative information-gathering tool called the network characterization service (NCS). NCS runs in user space and is used to acquire network information. Its protocol is designed for scalable and distributed deployment, similar to DNS. Its algorithms provide efficient, speedy and accurate detection of bottlenecks, especially dynamic bottlenecks. On current and future networks, dynamic bottlenecks do and will affect network performance dramatically.

  5. Spectroscopic Characterization of Metallofullerenes

    Bethune, D. S.; de Vries, M. S.; Macfarlane, R.; Wittman, G.; Grannan, S.; Birmingham, J.; Richards, P.; Stevenson, S.; Glass, T.; Burbank, P.; Sun, Z.; Dorn, H. C.

    1996-03-01

    Scandium and Erbium metallofullerenes have been isolated using HPLC techniques and characterized by NMR, optical and far IR spectroscopy. In particular, Sc NMR spectra of Sc_2@C_2n species for several n have been obtained, and far infrared spectra of both discandium and and dierbium metallofullerenes have been measured. These show structure in the 20-200 cm-2 where vibrations of the encapsulated metal atoms are expected. Fluorescence spectra from dierbium metallofullerenes in the 1.5 μm region have been obtained at He and room temperatures.

  6. Characterizing Black Hole Mergers

    Baker, John; Boggs, William Darian; Kelly, Bernard

    2010-01-01

    Binary black hole mergers are a promising source of gravitational waves for interferometric gravitational wave detectors. Recent advances in numerical relativity have revealed the predictions of General Relativity for the strong burst of radiation generated in the final moments of binary coalescence. We explore features in the merger radiation which characterize the final moments of merger and ringdown. Interpreting the waveforms in terms of an rotating implicit radiation source allows a unified phenomenological description of the system from inspiral through ringdown. Common features in the waveforms allow quantitative description of the merger signal which may provide insights for observations large-mass black hole binaries.

  7. Characterization of clay minerals

    The natural clays are the more abundant minerals on the crust. They are used for making diverse industrial products. Due to the adsorption and ion exchange properties of these, a great interest for developing research directed toward the use of natural clays for the waste water treatment has been aroused. As part of such researches it is very important to carry out previously the characterization of the interest materials. In this work the results of the mineral and elemental chemical composition are presented as well as the morphological characteristics of clay minerals from different regions of the Mexican Republic. (Author)

  8. Characterization of solar cells

    Haerkoenen, J.; Tuominen, E.; Nybergh, K.; Ezer, Y.; Yli-Koski, M.; Sinkkonen, J. [Helsinki Univ. of Technology, Otaniemi (Finland). Dept. of Electrical and Communications Engineering

    1998-10-01

    Photovoltaic research in the Electron Physics Laboratory started in 1993, when laboratory joined the national TEKES/NEMO 2 research program. Since the beginning of the project, characterization as well as experimentally orientated development of the fabrication process of the solar cells were carried out parallery. The process development research started by the initiatives of the Finnish industry. At the moment a large amount of the laboratory personnel works on solar cell research and the financing comes mainly from external projects. The funding for the research has come from TEKES, Ministry of Education, Finnish Academy, GETA graduate school, special equipment grants of the university, and from the laboratory

  9. Battery Thermal Characterization

    Keyser, Matthew; Saxon, Aron; Powell, Mitchell; Shi, Ying

    2016-06-07

    This poster shows the progress in battery thermal characterization over the previous year. NREL collaborated with U.S. DRIVE and USABC battery developers to obtain thermal properties of their batteries, obtained heat capacity and heat generation of cells under various power profiles, obtained thermal images of the cells under various drive cycles, and used the measured results to validate thermal models. Thermal properties are used for the thermal analysis and design of improved battery thermal management systems to support achieve life and performance targets.

  10. Waste Characterization: Approaches and Methods

    Lagerkvist, A.; Ecke, H.; Christensen, Thomas Højlund

    2011-01-01

    is often narrowly defined to meet specific needs for information. This may however limit the general usefulness of the information gained, for example, if the specific purpose limited the characterization to a subset of variables. In general, data available in the solid waste area are limited and often...... with limited representation. This chapter describes common approaches and methods in waste characterization including common terms, sampling, characterization methods and data evaluation. The focus is on the characterization of waste as it is generated or collected, while specific issues on characterization...

  11. TRU waste characterization chamber gloveboxes

    Argonne National Laboratory-West (ANL-W) is participating in the Department of Energy's (DOE) National Transuranic Waste Program in support of the Waste Isolation Pilot Plant (WIPP). The Laboratory's support currently consists of intrusive characterization of a selected population of drums containing transuranic waste. This characterization is performed in a complex of alpha containment gloveboxes termed the Waste Characterization Gloveboxes. Made up of the Waste Characterization Chamber, Sample Preparation Glovebox, and the Equipment Repair Glovebox, they were designed as a small production characterization facility for support of the Idaho National Engineering and Environmental Laboratory (INEEL). This paper presents salient features of these gloveboxes

  12. FRACTURING FLUID CHARACTERIZATION FACILITY

    Subhash Shah

    2000-08-01

    Hydraulic fracturing technology has been successfully applied for well stimulation of low and high permeability reservoirs for numerous years. Treatment optimization and improved economics have always been the key to the success and it is more so when the reservoirs under consideration are marginal. Fluids are widely used for the stimulation of wells. The Fracturing Fluid Characterization Facility (FFCF) has been established to provide the accurate prediction of the behavior of complex fracturing fluids under downhole conditions. The primary focus of the facility is to provide valuable insight into the various mechanisms that govern the flow of fracturing fluids and slurries through hydraulically created fractures. During the time between September 30, 1992, and March 31, 2000, the research efforts were devoted to the areas of fluid rheology, proppant transport, proppant flowback, dynamic fluid loss, perforation pressure losses, and frictional pressure losses. In this regard, a unique above-the-ground fracture simulator was designed and constructed at the FFCF, labeled ''The High Pressure Simulator'' (HPS). The FFCF is now available to industry for characterizing and understanding the behavior of complex fluid systems. To better reflect and encompass the broad spectrum of the petroleum industry, the FFCF now operates under a new name of ''The Well Construction Technology Center'' (WCTC). This report documents the summary of the activities performed during 1992-2000 at the FFCF.

  13. PAU camera: detectors characterization

    Casas, Ricard; Ballester, Otger; Cardiel-Sas, Laia; Castilla, Javier; Jiménez, Jorge; Maiorino, Marino; Pío, Cristóbal; Sevilla, Ignacio; de Vicente, Juan

    2012-07-01

    The PAU Camera (PAUCam) [1,2] is a wide field camera that will be mounted at the corrected prime focus of the William Herschel Telescope (Observatorio del Roque de los Muchachos, Canary Islands, Spain) in the next months. The focal plane of PAUCam is composed by a mosaic of 18 CCD detectors of 2,048 x 4,176 pixels each one with a pixel size of 15 microns, manufactured by Hamamatsu Photonics K. K. This mosaic covers a field of view (FoV) of 60 arcmin (minutes of arc), 40 of them are unvignetted. The behaviour of these 18 devices, plus four spares, and their electronic response should be characterized and optimized for the use in PAUCam. This job is being carried out in the laboratories of the ICE/IFAE and the CIEMAT. The electronic optimization of the CCD detectors is being carried out by means of an OG (Output Gate) scan and maximizing it CTE (Charge Transfer Efficiency) while the read-out noise is minimized. The device characterization itself is obtained with different tests. The photon transfer curve (PTC) that allows to obtain the electronic gain, the linearity vs. light stimulus, the full-well capacity and the cosmetic defects. The read-out noise, the dark current, the stability vs. temperature and the light remanence.

  14. Mound facility physical characterization

    Tonne, W.R.; Alexander, B.M.; Cage, M.R.; Hase, E.H.; Schmidt, M.J.; Schneider, J.E.; Slusher, W.; Todd, J.E.

    1993-12-01

    The purpose of this report is to provide a baseline physical characterization of Mound`s facilities as of September 1993. The baseline characterizations are to be used in the development of long-term future use strategy development for the Mound site. This document describes the current missions and alternative future use scenarios for each building. Current mission descriptions cover facility capabilities, physical resources required to support operations, current safety envelope and current status of facilities. Future use scenarios identify potential alternative future uses, facility modifications required for likely use, facility modifications of other uses, changes to safety envelope for the likely use, cleanup criteria for each future use scenario, and disposition of surplus equipment. This Introductory Chapter includes an Executive Summary that contains narrative on the Functional Unit Material Condition, Current Facility Status, Listing of Buildings, Space Plans, Summary of Maintenance Program and Repair Backlog, Environmental Restoration, and Decontamination and Decommissioning Programs. Under Section B, Site Description, is a brief listing of the Site PS Development, as well as Current Utility Sources. Section C contains Site Assumptions. A Maintenance Program Overview, as well as Current Deficiencies, is contained within the Maintenance Program Chapter.

  15. JANUS characterization report

    The JANUS Reactor was operated from 1965 to 1992. All of the fuel was removed and shipped offsite in 1993. To provide information for use in finalizing the planning for the decommissioning of the reactor, the Health Physics Section of Argonne National Laboratory performed a characterization of the facility in January and February 1996. The characterization included measurements for radioactivity, hazardous materials, lead in wall paint, and asbestos. Measurements and smear samples for surface contamination were collected from every wall, ceiling and floor of the facility. Samples to determine activity concentrations were collected from vertical and horizontal corings into the reactor shield and foundation, and from coring into walls of the high dose and low dose rooms. Soil samples were collected outdoors from two drill holes, one south and one north of the JANUS exhaust stack. The predominant radionuclides detected were 60Co, 152Eu, and 154Eu. The highest exposure rate was 175 mR/h at the center of the reactor core. No hazardous materials were found in pits or sumps. There are 20 identified areas with asbestos and 7 objects with lead based paint

  16. Characterization of Mesoamerican jade

    Bishop, R.L.; Sayre, E.V.; van Zelst, L.

    1983-11-23

    Jadeite occurring in the Motague River Valley of Guatemala has been characterized by neutron activation analysis and forms two district, phase-related groups. Comparison of the compositional profiles of Mayan jadeite artifacts reveals many specimens having profiles matching those of the Montagua source. Of particular interest are the large number of jadeite artifacts which show internal similarity yet have compositional patterns which are significantly different from the Montagua samples and Montagua-related artifacts. A few of the analyzed Costa Rican artifacts show patterns similar to those of the Motagua yet the vast majority fall within one of the two Costa Rican compositional groups. When considering the non-Motagua related Mayan artifacts, the analytical approach appears to be sufficiently sensitive so as to distinguish differences between the Chrome-green and Chichen-green material. Even two Honduran site specific groups of albite - cultural jade - form distinct groups.

  17. Neutron beam characterization

    At the first Research Coordination Meeting in November 1999 it was agreed that each experimental participant would characterize his own neutron beam and detector system, and then use it to analyze an unknown sample. A set of five materials was prepared and distributed to aid this effort: titanium foil, gold foil, borophosphosilicate glass on silicon, boron 10-aluminum alloy sheet, and a mixture of a complex aluminosilicate and graphite. Neutron flux can be measured by the conventional foil activation method using the gold foil. The titanium foil is to be used to measure the sensitivity of the system, the product of the neutron flux and the detector efficiency. The effective velocity or wavelength of the beam can be measured with the boron samples using a prescribed procedure. Excel spreadsheets for the flux and velocity calculations were placed on the IAEA server ndsalpha.iaea.org

  18. Spectroradiometry for LED characterization

    Dam-Hansen, Carsten

    Radiospectroscopy is the absolute measurement of electromagnetic radiation within a specific wavelength range. For characterization of LED components, light sources and lamps we are interested in absolute measurement of the spectral power distribution, SPD, in the visible and near infrared region....... Using integrating spheres for light collection setups for absolute total spectral flux is realized at the LED Light Lab at DTU Fotonik, Risø Campus. From these, both total radiant and luminous flux is determined and through electrical power measurement also the efficiency is determined. From the SPD...... colorimetric quantities like color coordinates, color temperature and color rendering indices are calculated. The facilities and special issues concerning LED measurements compared to traditional light sources are explained and examples from the “LED lighting quality program”, a project supported by the Danish...

  19. ANALYTICAL CHARACTERIZATION OF PRECIPITATIONS

    Danut Tiberiu Epure

    2011-02-01

    Full Text Available The properties of precipitation are mainly determined by solid, liquid and gaseous substances that exist in suspended or dissolved form. These substances come from many complex interactions between the atmosphere – hydrosphere – lithosphere – biota. The analytical characterization of precipitation has been based on the analysis of several chemical parameters: pH, conductivity, chloride, fluoride and ammonium ions, total hardness, alkalinity, H2S and sulphides, COD (Mn, nitrites, phosphorous, metallic ions (total iron, copper and chromium. In this purpose were collected rainwater, ice and snow from different areas (cities Năvodari, Constanţa, Buzău and Mihail Kogălniceanu during November 2007 till February 2008. This study shows that chemical characteristics of the analyzed water samples vary from one region to another depending on the mineralogical composition of zones crossed, the contact time, temperature, weather conditions, the sampling period (day or night and the nature of sample (rain, snow, ice.

  20. Photoelectronic characterization of heterointerfaces.

    Brumbach, Michael Todd

    2012-02-01

    In many devices such as solar cells, light emitting diodes, transistors, etc., the performance relies on the electronic structure at interfaces between materials within the device. The objective of this work was to perform robust characterization of hybrid (organic/inorganic) interfaces by tailoring the interfacial region for photoelectron spectroscopy. Self-assembled monolayers (SAM) were utilized to induce dipoles of various magnitudes at the interface. Additionally, SAMs of molecules with varying dipolar characteristics were mixed into spatially organized structures to systematically vary the apparent work function. Polymer thin films were characterized by depositing films of varying thicknesses on numerous substrates with and without interfacial modifications. Hard X-ray photoelectron spectroscopy (HAXPES) was performed to evaluate a buried interface between indium tin oxide (ITO), treated under various conditions, and poly(3-hexylthiophene) (P3HT). Conducting polymer films were found to be sufficiently conducting such that no significant charge redistribution in the polymer films was observed. Consequently, a further departure from uniform substrates was taken whereby electrically disconnected regions of the substrate presented ideally insulating interfacial contacts. In order to accomplish this novel strategy, interdigitated electrodes were used as the substrate. Conducting fingers of one half of the electrodes were electrically grounded while the other set of electrodes were electronically floating. This allowed for the evaluation of substrate charging on photoelectron spectra (SCOPES) in the presence of overlying semiconducting thin films. Such an experiment has never before been reported. This concept was developed out of the previous experiments on interfacial modification and thin film depositions and presents new opportunities for understanding chemical and electronic changes in a multitude of materials and interfaces.

  1. Synthesis by plasma and characterization of compounds derived from polyacetylene; Sintesis por plasma y caracterizacion de compuestos derivados del poliacetileno

    Vasquez O, M

    2004-07-01

    This work presents a study on, the synthesis by plasma and the characterization of an aliphatic conjugated polymer, polyacetylene-chlorinated (Pac), and two aromatic polymers, Poly pyrrole (P Py-Cl) and Poly thiophene (Pth-Cl) synthesized with chlorine and the electrical conductivity. The last two polymers were synthesized to compare the chlorine-polymer interaction in aliphatic and aromatic polymers synthesized by plasma and their repercussion on the electrical transport of charges in the material. The structure and morphology of the polymers were studied using scanning electron microscopy (Sem), energy dispersive spectroscopy (EDS), infrared spectroscopy (Ft-IR), conductivity analysis and X-Ray photon spectroscopy (XPS). The results showed that Pac is soluble in acetone and other organic solvents, which indicates a low proportion of crosslinking in the polymers. This point is important because the crosslinking reduces the electrical conductivity in the material. The Pac conductivity is in the range of 1 x 10{sup -12} to 6 x 10{sup -4} S/cm in the internal of 35- 90% of relative humidity. A possible mechanism for the transport of electrical charges in Pac is by means of the double and simple conjugated bonds in the polymers. Pth-Cl and P Py-Cl present electric conductivity in the interval of 9 x 10{sup -5} to 1 x 10{sup -2} S/cm and show a great dependence on the relative humidity. The chlorine addition in these polymers was through simultaneous polymerization with chloroform. This last compound can decompose if the energy of the plasma is relatively high, and the fragments can link to the polymer in a hybrid process of copolymerization. An important point of this work is that the polymer is soluble, a difference of the obtained via plasma as the poli aniline, P Py-CI and Pth-Cl both studied in this work. If took in account that the Pac is single the monomer and that P Py-Cl and Pth-CI is affected by the chlorine that modifies the conductivity of the material

  2. Mixed waste characterization reference document

    Waste characterization and monitoring are major activities in the management of waste from generation through storage and treatment to disposal. Adequate waste characterization is necessary to ensure safe storage, selection of appropriate and effective treatment, and adherence to disposal standards. For some wastes characterization objectives can be difficult and costly to achieve. The purpose of this document is to evaluate costs of characterizing one such waste type, mixed (hazardous and radioactive) waste. For the purpose of this document, waste characterization includes treatment system monitoring, where monitoring is a supplement or substitute for waste characterization. This document establishes a cost baseline for mixed waste characterization and treatment system monitoring requirements from which to evaluate alternatives. The cost baseline established as part of this work includes costs for a thermal treatment technology (i.e., a rotary kiln incinerator), a nonthermal treatment process (i.e., waste sorting, macronencapsulation, and catalytic wet oxidation), and no treatment (i.e., disposal of waste at the Waste Isolation Pilot Plant (WIPP)). The analysis of improvement over the baseline includes assessment of promising areas for technology development in front-end waste characterization, process equipment, off gas controls, and monitoring. Based on this assessment, an ideal characterization and monitoring configuration is described that minimizes costs and optimizes resources required for waste characterization

  3. 105-C Facility characterization plan

    This facility characterization plan is a site-specific document that describes how quantification and qualification of the radiological sources and the radioactive contamination in the 105-C Building will be accomplished. Characterization of hazardous materials will be addressed in a separate plan. This plan was developed from review of video tapes, photographs, and records. The purpose of this characterization plan is to provide an efficient and cost-effective method for determining the distribution of radioactive contamination at the 105-C Facility

  4. Nanometer Characterization/Manipulation Facility

    Federal Laboratory Consortium — FUNCTION: Characterizes the nanometer scale of biological, chemical, physical, electronic, and mechanical properties of surfaces and thin films using scanning probe...

  5. Characterization equipment essential drawing plan

    The purpose of this document is to list the Characterization equipment drawings that are classified as Essential Drawings. Essential Drawings: Are those drawings identified by the facility staff as necessary to directly support the safe operation of the facility or equipment (HNF 1997a). The Characterization equipment drawings identified in this report are deemed essential drawings as defined in HNF-PRO-242, Engineering Drawing Requirements (HNF 1997a). These drawings will be prepared, revised, and maintained per HNF-PRO-440, Engineering Document Change Control (HNF 1997b). All other Characterization equipment drawings not identified in this document will be considered Support drawings until the Characterization Equipment Drawing Evaluation Report is completed

  6. Beryllide application-2(characterization)

    High temperature oxidation behavior of titanium beryllides (Be12Ti, Be-5at%Ti and Be-7at%Ti) was investigated in contrast with pure Be and Ti. Mass change of these metals and alloys were measured at 800degC and 1000degC in dry air up to 24h using thermogravimetric technique. Mass gains of titanium beryllides were extremely small in contrast with those of Be and Ti at the same temperature. They were as small as Ni-based super alloys in this condition. Oxidation kinetics of titanium beryllides seemed to be parabolic at 800degC which indicates that the oxidation proceeded by diffusion controlled process of oxidants across a protective corrosion product. Surface morphology of oxidized titanium beryllides were smooth and thin-filmed, corresponding to the parabolic kinetics. On the other hand, oxidation product on Be was thick and porous, that suggests its non-protective nature against oxidation. Furthermore, XPS measurement was accomplished to characterize the film formed on Be12Ti. The oxide film seemed to be BeO at the top surface and no titanium oxide was found. From all the results, it was considered that Ti has a role of forming a protective and compact BeO thin film on titanium beryllides during high temperature oxidation processes in dry air. The BeO thin film derives good oxidation resistivity. (author)

  7. Simplex characterization of equilibrium

    Minimization of the reaction isotherm absolute value by the sequential simplex method may be used to characterize the equilibrium valence state distribution of plutonium in aqueous solutions. Sequential simplex procedure is an empirical method of locating maxima or minima in the response of a function of several variables. Where the objective function is entirely mathematical, a computer may be used to perform the simplex operations in a rapid and accurate manner, so that maxima and minima can often be located quickly and easily. The disproportionation of tetravalent plutonium is considered to be the consequence of two sequential reactions: 2Pu4+ + 2HOH = Pu3+ + PuO2+ + 4H+ P (1). Pu4+ + PuO2+ = Pu3+ + PuO2+ Q (2). If P is the frequency of occurrence of Eq. (1), and Q is the frequency of occurrence of Eq. (2), then it is assumed, that P=Q, and Eqs (1) and (2) may be added directly. 3Pu4+ + 2HOH = 2Pu3+ + PuO22+ + 4H+ (3). The persistence of pentavalent plutonium in aqueous plutonium solutions suggests that reactions 1 and 2 are not of equal frequency, and that their proportion for purposes of addition is not exactly equal to 1:1. (T.I.)

  8. Plant Phenotype Characterization System

    Daniel W McDonald; Ronald B Michaels

    2005-09-09

    This report is the final scientific report for the DOE Inventions and Innovations Project: Plant Phenotype Characterization System, DE-FG36-04GO14334. The period of performance was September 30, 2004 through July 15, 2005. The project objective is to demonstrate the viability of a new scientific instrument concept for the study of plant root systems. The root systems of plants are thought to be important in plant yield and thus important to DOE goals in renewable energy sources. The scientific study and understanding of plant root systems is hampered by the difficulty in observing root activity and the inadequacy of existing root study instrumentation options. We have demonstrated a high throughput, non-invasive, high resolution technique for visualizing plant root systems in-situ. Our approach is based upon low-energy x-ray radiography and the use of containers and substrates (artificial soil) which are virtually transparent to x-rays. The system allows us to germinate and grow plant specimens in our containers and substrates and to generate x-ray images of the developing root system over time. The same plant can be imaged at different times in its development. The system can be used for root studies in plant physiology, plant morphology, plant breeding, plant functional genomics and plant genotype screening.

  9. Characterization of Hospital Residuals

    The main objective of this investigation is the characterization of the solid residuals. A description of the handling of the liquid and gassy waste generated in hospitals is also given, identifying the source where they originate. To achieve the proposed objective the work was divided in three stages: The first one was the planning and the coordination with each hospital center, in this way, to determine the schedule of gathering of the waste can be possible. In the second stage a fieldwork was made; it consisted in gathering the quantitative and qualitative information of the general state of the handling of residuals. In the third and last stage, the information previously obtained was organized to express the results as the production rate per day by bed, generation of solid residuals for sampled services, type of solid residuals and density of the same ones. With the obtained results, approaches are settled down to either determine design parameters for final disposition whether for incineration, trituration, sanitary filler or recycling of some materials, and storage politics of the solid residuals that allow to determine the gathering frequency. The study concludes that it is necessary to improve the conditions of the residuals handling in some aspects, to provide the cleaning personnel of the equipment for gathering disposition and of security, minimum to carry out this work efficiently, and to maintain a control of all the dangerous waste, like sharp or polluted materials. In this way, an appreciable reduction is guaranteed in the impact on the atmosphere. (Author)

  10. Characterization of supercapacitors matrix

    This paper treats supercapacitors matrix characterization. In order to cut off transient power peaks and to compensate for the intrinsic limitations in embedded sources, the use of supercapacitors as a storage system is quite suitable, because of their appropriate electrical characteristics (huge capacitance, small series resistance, high specific energy, high specific power), direct storage (energy ready for use), and easy control by power electronic conversion. This use requires supercapacitors modules where several cells connected in serial and/or in parallel, thus a bypass system to balance the charging or the discharging of supercapacitors is required. In the matrix of supercapacitors, six elements of three parallel BCAP0350 supercapacitors in serial connections have been considered. This topology permits to reduce the number of the bypass circuits and it can work in degraded mode. Actually, it allows the system to have more reliability by providing power continually to the load even when there are one or more cells failed. Simulation and experimental results are presented and discussed.

  11. Compactable reactor waste characterization

    Compactable reactor wastes were characterized in respect of physical composition. β/γ activity levels, radionuclide inventory, and tritium and carbon-14 content. 1072 bags of waste representing 18 bales with a volume of 9 m3 were examined. This waste is extremely heterogeneous and can contain any item or material used at nuclear generating stations. The β/γ activity level of the waste is low; at the time of manufacture the 18 bales ranged between 1.0 and 6.94 mCi most of which was attributable to radionuclides with a half-life of one year or less. After ten years' decay the activity of any bale will have decreased to a maximum of 1.5 mCi and the only β/γ radionuclides of significance will be 60Co and 137Cs. Tritium and carbon-14 were found in most of the waste bags and it is estimated that a cubic metre of waste could contain 8.4 to 11.3 Ci of tritium and 0.8 to 5.4 μCi carbon-14. It is considered there is no need for further conditioning of this waste for disposal

  12. Tank characterization technical sampling basis

    Brown, T.M.

    1998-04-28

    Tank Characterization Technical Sampling Basis (this document) is the first step of an in place working process to plan characterization activities in an optimal manner. This document will be used to develop the revision of the Waste Information Requirements Document (WIRD) (Winkelman et al. 1997) and ultimately, to create sampling schedules. The revised WIRD will define all Characterization Project activities over the course of subsequent fiscal years 1999 through 2002. This document establishes priorities for sampling and characterization activities conducted under the Tank Waste Remediation System (TWRS) Tank Waste Characterization Project. The Tank Waste Characterization Project is designed to provide all TWRS programs with information describing the physical, chemical, and radiological properties of the contents of waste storage tanks at the Hanford Site. These tanks contain radioactive waste generated from the production of nuclear weapons materials at the Hanford Site. The waste composition varies from tank to tank because of the large number of chemical processes that were used when producing nuclear weapons materials over the years and because the wastes were mixed during efforts to better use tank storage space. The Tank Waste Characterization Project mission is to provide information and waste sample material necessary for TWRS to define and maintain safe interim storage and to process waste fractions into stable forms for ultimate disposal. This document integrates the information needed to address safety issues, regulatory requirements, and retrieval, treatment, and immobilization requirements. Characterization sampling to support tank farm operational needs is also discussed.

  13. Tank characterization technical sampling basis

    Tank Characterization Technical Sampling Basis (this document) is the first step of an in place working process to plan characterization activities in an optimal manner. This document will be used to develop the revision of the Waste Information Requirements Document (WIRD) (Winkelman et al. 1997) and ultimately, to create sampling schedules. The revised WIRD will define all Characterization Project activities over the course of subsequent fiscal years 1999 through 2002. This document establishes priorities for sampling and characterization activities conducted under the Tank Waste Remediation System (TWRS) Tank Waste Characterization Project. The Tank Waste Characterization Project is designed to provide all TWRS programs with information describing the physical, chemical, and radiological properties of the contents of waste storage tanks at the Hanford Site. These tanks contain radioactive waste generated from the production of nuclear weapons materials at the Hanford Site. The waste composition varies from tank to tank because of the large number of chemical processes that were used when producing nuclear weapons materials over the years and because the wastes were mixed during efforts to better use tank storage space. The Tank Waste Characterization Project mission is to provide information and waste sample material necessary for TWRS to define and maintain safe interim storage and to process waste fractions into stable forms for ultimate disposal. This document integrates the information needed to address safety issues, regulatory requirements, and retrieval, treatment, and immobilization requirements. Characterization sampling to support tank farm operational needs is also discussed

  14. Characterization Of Robot Work Cell

    Anderson, Ronald R.; Paternoster, Vincent Y.; Guthmiller, Wayne A.

    1990-01-01

    Iterative process of measurement and computation used to characterize work cell of robot, increasing accuracy of mathematical model of work cell. Characterization needed because model used in off-line programming (OLP) to compute paths to control motion of robot. Increases accuracies of model and paths.

  15. Revealed Cores: Characterizations and Structure

    Stefano Vannucci

    2010-01-01

    Characterizations of the choice functions that select the cores or the externally stable cores induced by an underlying revealed dominance digraph are provided. Relying on such characterizations, the basic order-theoretic structure of the corresponding sets of revealed cores is also analyzed

  16. Spectral characterization of abstract functions

    Let G be locally compact abelian group and GAMMA its dual group. Let X be locally convex complete space and X* its dual space. In this paper we give spectral characterization of bounded uniformly continuous functions from G to X. Also, we give applications to the characterization of solutions of functional differential equations. (author)

  17. Characterizing protein crystal nucleation

    Akella, Sathish V.

    We developed an experimental microfluidic based technique to measure the nucleation rates and successfully applied the technique to measure nucleation rates of lysozyme crystals. The technique involves counting the number of samples which do not have crystals as a function of time. Under the assumption that nucleation is a Poisson process, the fraction of samples with no crystals decays exponentially with the decay constant proportional to nucleation rate and volume of the sample. Since nucleation is a random and rare event, one needs to perform measurements on large number of samples to obtain good statistics. Microfluidics offers the solution of producing large number of samples at minimal material consumption. Hence, we developed a microfluidic method and measured nucleation rates of lysozyme crystals in supersaturated protein drops, each with volume of ˜ 1 nL. Classical Nucleation Theory (CNT) describes the kinetics of nucleation and predicts the functional form of nucleation rate in terms of the thermodynamic quantities involved, such as supersaturation, temperature, etc. We analyzed the measured nucleation rates in the context of CNT and obtained the activation energy and the kinetic pre-factor characterizing the nucleation process. One conclusion is that heterogeneous nucleation dominates crystallization. We report preliminary studies on selective enhancement of nucleation in one of the crystal polymorprhs of lysozyme (spherulite) using amorphous mesoporous bioactive gel-glass te{naomi06, naomi08}, CaO.P 2O5.SiO2 (known as bio-glass) with 2-10 nm pore-size diameter distribution. The pores act as heterogeneous nucleation centers and claimed to enhance the nucleation rates by molecular confinement. The measured kinetic profiles of crystal fraction of spherulites indicate that the crystallization of spherulites may be proceeding via secondary nucleation pathways.

  18. Characterization Methods of Encapsulates

    Zhang, Zhibing; Law, Daniel; Lian, Guoping

    , reliable methods which can be used to characterize these properties of encapsulates are vital. In this chapter, the state-of-art of these methods, their principles and applications, and release mechanisms are described as follows.

  19. Particle characterization for geothermal operations

    Vetter, O.J.; Kandarpa, V.

    1981-01-06

    A detailed summary of an ongoing evaluation of existing particle measuring methodology with emphasis on (a) adapting of existing methods in geothermal operations and (b) further development of existing instrumentation for field use is presented. The various instruments and methods used and/or suggested for particle characterization are described in detail. Theoretical and practical aspects of particle characterizations are outlined. A plan for further laboratory and field experiments is outlined. The instrumentations to be selected after some additional lab and field tests will be used in the studies on (a) formation damage through particle invasion and (b) characterizing and monitoring of particle suspensions in geothermal operations.

  20. Uruguayan tallow characterization

    Cecilia Rodríguez

    2011-04-01

    Full Text Available Eatable tallow is the product  obtained fusing oily, from clean and  healthy tissues (included the fats of clippings, and from muscles or bones adherents of bovine animals (Bos tsurus,  lambs (Ovis aries in good conditions of health in the moment of its sacrifice and whose has been treated and therefore are considered suitable for the human consumption.To obtain fat from the raw, this material must surrender to a previous treatment that breaks the adipose cells, by  mechanical destruction, boiling or by treatment with alcáli. The easiest  way  consists of the mechanical disintegration (breakup under heat, using steam in direct or indirect form. This product can be obtained by one of the following : discontinuous merger, humid constant merger and  continues merger at low temperature. At present is used in the  cosmetic industry (production of soaps, for nutrition (raw material for margarine, ranching (for the manufacture of food concentrated for animals, for the self propelling industry (raw material for the production of biodiesel. The major purpose of this work is the tallow characterization from the determination of the following parameters :Moisture and Volatile Matter (g/100g of sample, Melting Point (1C, Free Acidity (g. Oleic acid /100g of sample, Colour (yellow and red and Insoluble Matter (g/100g.de shows of 15 samples of animal tallow from Uruguay, in order to provide useful information for the selection of the material. The Norm used as reference was the AOCS (American Oil Chemistry Society. With the obtained information it has been realized a statistical exploratory analysis. The preliminary results, due to the high variability of the studied factors, do not allow to establish with the current number of samples a  model who explains the above mentioned variability, neither at first, to reduce the quantity of factors to consider; in effect, the regression of the moisture against the rest of the factors determined the

  1. 324 Building Baseline Radiological Characterization

    R.J. Reeder, J.C. Cooper

    2010-06-24

    This report documents the analysis of radiological data collected as part of the characterization study performed in 1998. The study was performed to create a baseline of the radiological conditions in the 324 Building.

  2. CCD characterization and measurements automation

    Modern mosaic cameras have grown both in size and in number of sensors. The required volume of sensor testing and characterization has grown accordingly. For camera projects as large as the LSST, test automation becomes a necessity. A CCD testing and characterization laboratory was built and is in operation for the LSST project. Characterization of LSST study contract sensors has been performed. The characterization process and its automation are discussed, and results are presented. Our system automatically acquires images, populates a database with metadata information, and runs express analysis. This approach is illustrated on 55Fe data analysis. 55Fe data are used to measure gain, charge transfer efficiency and charge diffusion. Examples of express analysis results are presented and discussed.

  3. Hanford site waste tank characterization

    This paper describes the on-going work in the characterization of the Hanford-Site high-level waste tanks. The waste in these tanks was produced as part of the nuclear weapons materials processing mission that occupied the Hanford Site for the first 40 years of its existence. Detailed and defensible characterization of the tank wastes is required to guide retrieval, pretreatment, and disposal technology development, to address waste stability and reactivity concerns, and to satisfy the compliance criteria for the various regulatory agencies overseeing activities at the Hanford Site. The resulting Tank Characterization Reports fulfill these needs, as well as satisfy the tank waste characterization milestones in the Hanford Federal Facility Agreement and Consent Order

  4. RA radiological characterization database application

    Radiological characterization of the RA research reactor is one of the main activities in the first two years of the reactor decommissioning project. The raw characterization data from direct measurements or laboratory analyses (defined within the existing sampling and measurement programme) have to be interpreted, organized and summarized in order to prepare the final characterization survey report. This report should be made so that the radiological condition of the entire site is completely and accurately shown with the radiological condition of the components clearly depicted. This paper presents an electronic database application, designed as a serviceable and efficient tool for characterization data storage, review and analysis, as well as for the reports generation. Relational database model was designed and the application is made by using Microsoft Access 2002 (SP1), a 32-bit RDBMS for the desktop and client/server database applications that run under Windows XP. (author)

  5. Holographic characterization of protein aggregates

    Wang, Chen; Zhong, Xiao; Ruffner, David; Stutt, Alexandra; Philips, Laura; Ward, Michael; Grier, David

    Holographic characterization directly measures the size distribution of subvisible protein aggregates in suspension and offers insights into their morphology. Based on holographic video microscopy, this analytical technique records and interprets holograms of individual aggregates in protein solutions as they flow down a microfluidic channel, without requiring labeling or other exceptional sample preparation. The hologram of an individual protein aggregate is analyzed in real time with the Lorenz-Mie theory of light scattering to measure that aggregate's size and optical properties. Detecting, counting and characterizing subvisible aggregates proceeds fast enough for time-resolved studies, and lends itself to tracking trends in protein aggregation arising from changing environmental factors. No other analytical technique provides such a wealth of particle-resolved characterization data in situ. Holographic characterization promises accelerated development of therapeutic protein formulations, improved process control during manufacturing, and streamlined quality assurance during storage and at the point of use. Mrsec and MRI program of the NSF, Spheryx Inc.

  6. Microsystems for biological cell characterization

    Rissanen, Anna

    2012-01-01

    This thesis describes three techniques for the characterization of living cells using micro-electro-mechanical systems (MEMS) based devices. The study of cellular function and structure is essential for bioprocess control, disease diagnosis, patient treatment and drug discovery. Microsystem technology enables characterization of very small samples, minimal use of expensive reagents, testing of multiple samples in parallel, and point-of-care testing, all of which increase throughput and reduce...

  7. Characterizing Financial and Statistical Literacy

    Di Girolamo, Amalia; Harrison, Glenn W.; Lau, Morten;

    We characterize the literacy of an individual in a domain by their elicited subjective belief distribution over the possible responses to a question posed in that domain. We consider literacy across several financial, economic and statistical domains. We find considerable demographic heterogeneity...... extensions of our approach to characterize financial capability, the consequences of non-literacy, social literacy, and the information content of hypothetical survey measures of literacy....

  8. Characterization of radioactive hazardous waste

    The characterization of radioactive hazardous waste, also known as transuranic 'mixed waste' has to be completed before it can be classified for proper treatment (incinerator, mechanical compaction or thermal treatment), packing, and transport. The characterization of the TRU mixed waste is not only complex process but rather an expensive undertaking. The process knowledge is the basic foundation of characterization. It is the documented knowledge of processes and materials that generated the waste. The transuranic waste Quality Assurance Program Plan (QAPP) defines the Data Quality Objectives (DQO's) and provides the scope of analytical parameters and methods required to accurately characterize the radioactive mixed waste. Based on the historical data and process knowledge a sampling and analysis plan can be developed to characterize the radioactive hazardous waste. Based on the characterization, an assessment of the regulatory status can be made before the waste could be accepted for disposal at the WIPP facility. The Waste Acceptance Criteria (WAC) developed by WIPP defines the parameters for receiving and final disposal of the TRU waste. The sets of criteria, such as: heat generated, fissile gram equivalent (FGE), plutonium-equivalent (PE) curies, and specifications of a dose rate have to be met before the waste is accepted for deep geological disposal. The characterization of radioactive waste becomes even more complex due to the presence of iron base metals/alloys, aluminum base metals/alloys, organic, chelating agents that are mixed with plastic, rubber, cellulose, soils and cement. Some of the modern characterization technologies that are under development and currently used for TRU mixed wastes are: nondestructive examination, nondestructive assay, headspace gas analysis, and drum coring for Resources Conservation Recovery Act (RCRA) sampling. (author)

  9. Colorimetric characterization of LED luminaires

    Costa, C. L. M.; Vieira, R. R.; Pereira, R. C.; Silva, P. V. M.; Oliveira, I. A. A.; Sardinha, A. S.; Viana, D. D.; Barbosa, A. H.; Souza, L. P.; Alvarenga, A. D.

    2015-01-01

    The Optical Metrology Division of Inmetro - National Institute of Metrology, Quality and Technology has recently started the colorimetric characterization of lamps by implementing Correlated Color Temperature (CCT) and Color Rendering Index (CRI) measurements of incandescent lamps, followed by the CFL, and LED lamps and luminaires. Here we present the results for the verification of the color characterization of samples of SSL luminaires for public as well as indoor illumination that are sold in Brazil.

  10. Colorimetric characterization of LED luminaires

    The Optical Metrology Division of Inmetro – National Institute of Metrology, Quality and Technology has recently started the colorimetric characterization of lamps by implementing Correlated Color Temperature (CCT) and Color Rendering Index (CRI) measurements of incandescent lamps, followed by the CFL, and LED lamps and luminaires. Here we present the results for the verification of the color characterization of samples of SSL luminaires for public as well as indoor illumination that are sold in Brazil

  11. High Speed On-Wafer Characterization Laboratory

    Federal Laboratory Consortium — At the High Speed On-Wafer Characterization Laboratory, researchers characterize and model devices operating at terahertz (THz) and millimeter-wave frequencies. The...

  12. Characterization of nanometer tungsten powders

    LI Huiqian; LIN Tao; SHAO Huiping; WU Chengyi; GUO Zhimeng; LUO Ji

    2008-01-01

    Three types of tungsten powders were prepared by hydrogen reduction of three precursor powders at low temperature,which were used as samples,and were then characterized by Brunauer-Emmer-Teller (BET) method,scanning electron microscopy (SEM),transmission electronic microscopy (TEM),small angle X-ray scattering (SAXS),and field-emission scanning electron microscopy (FESEM) respectively.The results showed that although BET and SEM could not characterize the particle size of nanometer powders,they were important means of assistance to exclude non-nanometer powders.TEM and FESEM could directly measure the particle size of nanometer powders,but this needs a lot of time,to count the average particle size and particle size distribution.SAXS could not describe the state of agglomeration.By the combination of FESEM and SAXS,the particle size,particle size distribution,and particle shape of nanorneter powders could be preciscly characterized.

  13. INFLUENCE OF ELECTROPOLYMERIZATION METHOD ON MORPHOLOGIES AND CAPACITIVE PROPERTIES OF POLYPYRROLE FILMS GROWING ON SILICON

    IMENE CHIKOUCHE; ALI SAHARI; AHMED ZOUAOUI

    2014-01-01

    Two methods of Pyrrole electropolymerization were investigated to prepare polypyrrole films growing onto n-doped silicon n-Si (111): Polypyrrole films prepared by galvanostatic method exhibits toroidal morphology for thin films, and mixture of toroidal and globular morphologies for thick films. Polypyrrole films obtained from this method were characterized by lower surface roughness. Electropolymerization of pyrrole by potentiodynamic method provided Polypyrrole films with beans-like structur...

  14. Materials Characterization Center program plan

    The Materials Characterization Center (MCC) has been established at Pacific Northwest Laboratory as part of the Materials Characterization Organization for providing an authoritative, referenceable basis for establishing nuclear waste material properties and test methods. The MCC will provide a data base that will include information on the components of the waste emplacement package - the spent fuel or processed waste form and the engineered barriers - and their interaction with each other and as affected by the environment. The MCC will plan materials testing, develop and document procedures, collect and analyze existing materials data, and conduct tests as necessary

  15. Feedstock characterization and recommended procedures

    Using biomass for non-conventional applications such as feedstocks for fuels, chemicals, new materials, and electric power production requires knowledge of biomass characteristics important to these processes, and characterization techniques that are more appropriate than those employed today for conventional applications of food, feed, and fiber. This paper reviews feedstock characterization and standardization methodologies, and identifies research and development needs. It reviews the international cooperation involved in determining biomass characteristics and standards that has culminated in preparing four biomass samples currently available from the National Institute of Standards and Technology (NIST)

  16. Set Containment Characterization and Mathematical Programming

    Suzuki, Satoshi; Kuroiwa, Daishi

    2009-01-01

    Recently, many researchers studied set containment characterizations. In this paper, we introduce some set containment characterizations for quasiconvex programming. Furthermore, we show a duality theorem for quasiconvex programming by using set containment characterizations. Notions of quasiconjugate for quasiconvex functions, especially 1, -1-quasiconjugate, 1-semiconjugate, H-quasiconjugate and R-quasiconjugate, play important roles to derive characterizations of the set containments.

  17. Synthesis, FT–IR characterization and crystal structure of aqua(5,10,15,20-tetraphenylporphyrinato-κ4Nmanganese(III trifluoromethanesulfonate

    Wafa Harhouri

    2016-05-01

    Full Text Available In the title salt, [Mn(C44H28N4(H2O](CF3SO3 or [MnIII(TPP(H2O](CF3SO3 (where TPP is the dianion of 5,10,15,20-tetraphenylporphyrin, the MnIII cation is chelated by the four pyrrole N atoms of the porphyrinate anion and additionally coordinated by an aqua ligand in an apical site, completing the distorted square-pyramidal coordination environment. The average Mn—N(pyrrole bond length is 1.998 (9 Å and the Mn—O(aqua bond length is 2.1057 (15 Å. The central MnIII ion is displaced by 0.1575 (5 Å from the N4C20 mean plane of the porphyrinate anion towards the apical aqua ligand. The porphyrinate macrocycle exhibits a moderate ruffling and strong saddle deformations. In the crystal lattice, the [MnIII(TPP(H2O]+ cation and the trifluoromethanesulfonate counter-ions are arranged in alternating planes packed along [001]. The components are linked together through O—H...O hydrogen bonds and much weaker C—H...O and C—H...F interactions. The crystal packing is further stabilized by weak C—H...π interactions involving the pyrrole and phenyl rings of the porphyrin moieties.

  18. Remote sensing for site characterization

    Kuehn, Friedrich, (Edited By); King, Trude V.; Hoerig, Bernhard; Peters, Douglas C.

    2000-01-01

    This volume, Remote Sensing for Site Characterization, describes the feasibility of aircraft- and satellite-based methods of revealing environmental-geological problems. A balanced ratio between explanations of the methodological/technical side and presentations of case studies is maintained. The comparison of case studies from North America and Germany show how the respective territorial conditions lead to distinct methodological approaches.

  19. Material stabilization characterization management plan

    This document presents overall direction for characterization needs during stabilization of SNM at the Plutonium Finishing Plant (PFP). Technical issues for needed data and equipment are identified. Information on material categories and links to vulnerabilities are given. Comparison data on the material categories is discussed to assist in assessing the relative risks and desired processing priority

  20. On Characterization of Quadratic Splines

    Chen, B. T.; Madsen, Kaj; Zhang, Shuzhong

    2005-01-01

    representation can be refined in a neighborhood of a non-degenerate point and a set of non-degenerate minimizers. Based on these characterizations, many existing algorithms for specific convex quadratic splines are also finite convergent for a general convex quadratic spline. Finally, we study the relationship...

  1. Electron Spectroscopy for Material Characterization

    Süzer, Şefik

    1998-01-01

    Basic principles of the two electron spectroscopic techniques, the x-ray photoelectron spectroscopy, XPS, and the Auger electron spectroscopy, AES, are given. Their utilization in material characterization are introduced through examples with application of these techniques to various surface related problems.

  2. FCLib: The Feature Characterization Library.

    Gentile, Ann C.; Doyle, Wendy S. K.; Kegelmeyer, W. Philip [Sandia National Laboratories, Livermore, CA; Ulmer, Craig D. [Sandia National Laboratories, Livermore, CA

    2008-11-01

    The Feature Characterization Library (FCLib) is a software library that simplifies the process of interrogating, analyzing, and understanding complex data sets generated by finite element applications. This document provides an overview of the library, a description of both the design philosophy and implementation of the library, and examples of how the library can be utilized to extract understanding from raw datasets.

  3. Characterization of Injection Molded Structures

    Sun, Ling; Søgaard, Emil; Andersen, Nis Korsgaard;

    and limitations. Therefore, it would be difficult to characterize complex, especially hierarchical structures by using only one method. Here we present a combined optical microscopy, scanning electron microscopy (SEM), and scanning probe microscopy study on injection molded structures. These...... understand structure-properties relationship of the injection molded polymer samples. These results are very important in optimizing injection molding parameters....

  4. FTIR characterization of advanced materials

    Young, P. R.; Chang, A. C.

    1986-01-01

    This paper surveys the application of Fourier transform infrared spectroscopy to the characterization of advanced materials. FTIR sampling techniques including internal and external reflectance and photoacoustic spectroscopy are discussed. Representative examples from the literature of the analysis of resins, fibers, prepregs and composites are reviewed. A discussion of several promising specialized FTIR techniques is also presented.

  5. Holographic characterization of chain photopolymerization

    Engin, D.; Kewitsch, A. S.; Yariv, A.

    1999-01-01

    A holographic characterization technique is developed in accordance with a general photopolymerization model. The technique allows detailed quantification of the chemical parameters, including their variation from the Trommsdorff effect. The holographic procedure is especially suited for studying the diffusion of the chemical reactants.

  6. Raman spectroscopy for nanomaterials characterization

    2012-01-01

    First volume of a 40-volume series on nanoscience and nanotechnology, edited by the renowned scientist Challa S.S.R. Kumar. This handbook gives a comprehensive overview about Raman spectroscopy for the characterization of nanomaterials. Modern applications and state-of-the-art techniques are covered and make this volume essential reading for research scientists in academia and industry.

  7. CCD characterization and measurements automation

    Kotov, I.V.; Frank, J.; Kotov, A.I.; Kubánek, Petr; O´Connor, P.; Prouza, Michael; Radeka, V.; Takacs, P.

    2012-01-01

    Roč. 695, Dec (2012), 188-192. ISSN 0168-9002 R&D Projects: GA MŠk ME09052 Institutional research plan: CEZ:AV0Z10100502 Keywords : CCD * characterization * test automation Subject RIV: BN - Astronomy, Celestial Mechanics, Astrophysics Impact factor: 1.142, year: 2012

  8. A Mobile Automated Characterization System (MACS) for indoor floor characterization

    The Savannah River Technology Center (SRTC) and Oak Ridge National Laboratory are developing an advanced Mobile Automated Characterization System (MACS) to characterize indoor contaminated floors. MACS is based upon Semi-Intelligent Mobile Observing Navigator (SIMON), an earlier floor characterization system developed at SRTC. MACS will feature enhanced navigation systems, operator interface, and an interface to simplify integration of additional sensors. The enhanced navigation system will provide the capability to survey large open areas much more accurately than is now possible with SIMON, which is better suited for hallways and corridors that provide the means for recalibrating position and heading. MACS operator interface is designed to facilitate MACS's use as a tool for health physicists, thus eliminating the need for additional training in the robot's control language. Initial implementation of MACS will use radiation detectors. Additional sensors, such as PCB sensors currently being developed, will be integrated on MACS in the future. Initial use of MACS will be focused toward obtaining comparative results with manual methods. Surveys will be conducted both manually and with MACS to compare relative costs and data quality. While clear cost benefits anticipated, data quality benefits should be even more significant

  9. Microstructure Characterization of RERTR Fuel

    J. Gan; B. D. Miller; D. D. Keiser; T. R. Allen; D. M. Wachs

    2008-09-01

    A variety of phases have the potential to develop in the irradiated fuels for the reduced enrichment research test reactor (RERTR) program. To study the radiation stability of these potential phases, three depleted uranium alloys were cast. The phases of interest were identified including U(Si,Al)3, (U,Mo)(Si,Al)3, UMo2Al20, UAl4, and U6Mo4Al43. These alloys were irradiated with 2.6 MeV protons at 200ºC up to 3.0 dpa. The microstructure is characterized using SEM and TEM. Microstructural characterization for an archive dispersion fuel plate (U-7Mo fuel particles in Al-2%Si cladding) was also carried out. TEM sample preparation for the irradiated dispersion fuel has been developed.

  10. AFIP-6 Characterization Summary Report

    Dr. Dennis D. Keiser

    2011-12-01

    The AFIP-6 (ATR Full-size-plate In center flux trap Position) Characterization Summary Report outlines the fresh fuel characterization efforts performed during the AFIP-6 experiment. The AFIP-6 experiment was designed to evaluate the performance of monolithic uranium-molybdenum (U-Mo) fuels at a scale prototypic of Advanced Test Reactor (ATR) fuel plates (45-inches long). The AFIP-6 test was the first test with plates that were swaged into the rails of the assembly. This test served to examine the effects of a plate in a swaged condition with longer fuel zones (22.5-inches long), that were centered in the plate. AFIP-6 test plates employed a zirconium interlayer that was co-rolled with the fuel foil. Previous mini-plate and AFIP irradiation experiments performed in ATR have demonstrated the stable behavior of the interface between the U-Mo fuel and the zirconium interlayer.

  11. Surface characterization of ceramic materials

    In recent years several techniques have become available to characterize the structure and chemical composition of surfaces of ceramic materials. These techniques utilize electron scattering and scattering of ions from surfaces. Low-energy electron diffraction is used to determine the surface structure, Auger electron spectroscopy and other techniques of electron spectroscopy (ultraviolet and photoelectron spectroscopies) are employed to determine the composition of the surface. In addition the oxidation state of surface atoms may be determined using these techniques. Ion scattering mass spectrometry and secondary ion mass spectrometry are also useful in characterizing surfaces and their reactions. These techniques, their applications and the results of recent studies are discussed. 12 figures, 52 references, 2 tables

  12. Geometric characterization of macroshell targets

    We are investigating methods of fabricating and characterizing large diameter, thin-walled glass capsules for Inertial Fusion (IF) experiments. Dimensional requirements for the capsules specify diameters of two to ten millimeters and a wide range of aspect ratios (diameter/wall). These shells are larger in diameter than shells made in drop towers. Because of their larger size, they have been given the designation, macroshell. Glass macroshell targets are transparent, seamless, fuel containers which are currently used in beta-heating experiments at KMSF. The capsules are also potentially useful for neutron production experiments with IF drivers like Nova. The technology developed to fabricate these fuel containers may be useful in the fabrication of polymer shells necessary for the proposed Laboratory Microfusion Facility (LMF); some work with polymers has started. Accurate target characterization is essential to ensure the accurate measurement of fuel layers produced by radioactively induced sublimation of cyrogenically cooled deuterium-tritium (DT) fuel. 3 refs., 4 figs

  13. Aerosol characterization during project POLINAT

    Hagen, D.E.; Hopkins, A.R.; Paladino, J.D.; Whitefield, P.D. [Missouri Univ., Rolla, MO (United States). Cloud and Aerosol Sciences Lab.; Lilenfeld, H.V. [McDonnell Douglas Aerospace-East, St. Louis, MO (United States)

    1997-12-31

    The objectives of the aerosol/particulate characterization measurements of project POLINAT (POLlution from aircraft emissions In the North ATlantic flight corridor) are: to search for aerosol/particulate signatures of air traffic emissions in the region of the North Atlantic Flight Corridor; to search for the aerosol/particulate component of large scale enhancement (`corridor effects`) of air traffic related species in the North Atlantic region; to determine the effective emission indices for the aerosol/particulate component of engine exhaust in both the near and far field of aircraft exhaust plumes; to measure the dispersion and transformation of the aerosol/particulate component of aircraft emissions as a function of ambient condition; to characterize background levels of aerosol/particulate concentrations in the North Atlantic Region; and to determine effective emission indices for engine exhaust particulates for regimes beyond the jet phase of plume expansion. (author) 10 refs.

  14. Fabrication and Characterization of NEMS

    JIAO Ji-wei; YANG Heng; LI Tie; LI Xin-xin; WANG Yue-lin

    2007-01-01

    We proposed a called "nano-fabrication based on MEMS technology" approach to realize the typical nano-electromechanical structures,such as integrated nano probe,ultrathin cantilever,silicon nano wire,and doubly clamped nano beam,to demonstrate the feasibility and advantages. We also introduced the characterization of nano structures based on laser vibrometer and piezoresistive effect,the latter method was first time applied to investigate a doubly daped nanobeam with a thickness of about 200 nm.

  15. Towards Characterizing International Routing Detours

    Shah, Anant; Fontunge, Romain; Papadopoulos, Christos

    2016-01-01

    There are currently no requirements (technical or otherwise) that BGP paths must be contained within national boundaries. Indeed, some paths experience international detours, i.e., originate in one country, cross international boundaries and return to the same country. In most cases these are sensible traffic engineering or peering decisions at ISPs that serve multiple countries. In some cases such detours may be suspicious. Characterizing international detours is useful to a number of player...

  16. Chemical characterization of element 112.

    Eichler, R; Aksenov, N V; Belozerov, A V; Bozhikov, G A; Chepigin, V I; Dmitriev, S N; Dressler, R; Gäggeler, H W; Gorshkov, V A; Haenssler, F; Itkis, M G; Laube, A; Lebedev, V Ya; Malyshev, O N; Oganessian, Yu Ts; Petrushkin, O V; Piguet, D; Rasmussen, P; Shishkin, S V; Shutov, A V; Svirikhin, A I; Tereshatov, E E; Vostokin, G K; Wegrzecki, M; Yeremin, A V

    2007-05-01

    The heaviest elements to have been chemically characterized are seaborgium (element 106), bohrium (element 107) and hassium (element 108). All three behave according to their respective positions in groups 6, 7 and 8 of the periodic table, which arranges elements according to their outermost electrons and hence their chemical properties. However, the chemical characterization results are not trivial: relativistic effects on the electronic structure of the heaviest elements can strongly influence chemical properties. The next heavy element targeted for chemical characterization is element 112; its closed-shell electronic structure with a filled outer s orbital suggests that it may be particularly susceptible to strong deviations from the chemical property trends expected within group 12. Indeed, first experiments concluded that element 112 does not behave like its lighter homologue mercury. However, the production and identification methods used cast doubt on the validity of this result. Here we report a more reliable chemical characterization of element 112, involving the production of two atoms of (283)112 through the alpha decay of the short-lived (287)114 (which itself forms in the nuclear fusion reaction of 48Ca with 242Pu) and the adsorption of the two atoms on a gold surface. By directly comparing the adsorption characteristics of (283)112 to that of mercury and the noble gas radon, we find that element 112 is very volatile and, unlike radon, reveals a metallic interaction with the gold surface. These adsorption characteristics establish element 112 as a typical element of group 12, and its successful production unambiguously establishes the approach to the island of stability of superheavy elements through 48Ca-induced nuclear fusion reactions with actinides. PMID:17476264

  17. Chemical characterization of element 112

    Eichler, R.; Aksenov, N. V.; Belozerov, A. V.; Bozhikov, G. A.; Chepigin, V. I.; Dmitriev, S. N.; Dressler, R.; Gäggeler, H. W.; Gorshkov, V. A.; Haenssler, F.; Itkis, M. G.; Laube, A.; Lebedev, V. Ya.; Malyshev, O. N.; Oganessian, Yu. Ts.; Petrushkin, O. V.; Piguet, D.; Rasmussen, P.; Shishkin, S. V.; Shutov, A. V.; Svirikhin, A. I.; Tereshatov, E. E.; Vostokin, G. K.; Wegrzecki, M.; Yeremin, A. V.

    2007-05-01

    The heaviest elements to have been chemically characterized are seaborgium (element 106), bohrium (element 107) and hassium (element 108). All three behave according to their respective positions in groups 6, 7 and 8 of the periodic table, which arranges elements according to their outermost electrons and hence their chemical properties. However, the chemical characterization results are not trivial: relativistic effects on the electronic structure of the heaviest elements can strongly influence chemical properties. The next heavy element targeted for chemical characterization is element 112; its closed-shell electronic structure with a filled outer s orbital suggests that it may be particularly susceptible to strong deviations from the chemical property trends expected within group 12. Indeed, first experiments concluded that element 112 does not behave like its lighter homologue mercury. However, the production and identification methods used cast doubt on the validity of this result. Here we report a more reliable chemical characterization of element 112, involving the production of two atoms of 283112 through the alpha decay of the short-lived 287114 (which itself forms in the nuclear fusion reaction of 48Ca with 242Pu) and the adsorption of the two atoms on a gold surface. By directly comparing the adsorption characteristics of 283112 to that of mercury and the noble gas radon, we find that element 112 is very volatile and, unlike radon, reveals a metallic interaction with the gold surface. These adsorption characteristics establish element 112 as a typical element of group 12, and its successful production unambiguously establishes the approach to the island of stability of superheavy elements through 48Ca-induced nuclear fusion reactions with actinides.

  18. A characterization of Einstein manifolds

    Stelmastchuk, S. N.

    2009-01-01

    In this work we wish characterize the Einstein manifolds $(M,g)$, however without the necessity of hypothesis of compactness over $M$ and unitary volume of $g$, which are well known in many works. Our result says that if all eingenvalues $\\lambda$ of $r_{g}$, with respect to $g$, satisfy $\\lambda \\geq \\frac{1}{n}s_{g}$, then $(M,g)$ is an Einstein manifold, where $r_{g}$ and $s_{g}$ denote the Ricci and scalar curvatures, respectively.

  19. RF Characterization of Superconducting Samples

    Junginger, T; Welsch, C

    2009-01-01

    At CERN a compact Quadrupole Resonator has been re-commissioned for the RF characterization of superconducting materials at 400 MHz. In addition the resonator can also be excited at multiple integers of this frequency. Besides Rs it enables determination of the maximum RF magnetic field, the thermal conductivity and the penetration depth of the attached samples, at different temperatures. The features of the resonator will be compared with those of similar RF devices and first results will be presented.

  20. Characterization of Human Thymic Exosomes

    Gabriel Skogberg; Judith Gudmundsdottir; Sjoerd van der Post; Kerstin Sandström; Sören Bruhn; Mikael Benson; Lucia Mincheva-Nilsson; Vladimir Baranov; Esbjörn Telemo; Olov Ekwall

    2013-01-01

    Exosomes are nanosized membrane-bound vesicles that are released by various cell types and are capable of carrying proteins, lipids and RNAs which can be delivered to recipient cells. Exosomes play a role in intercellular communication and have been described to mediate immunologic information. In this article we report the first isolation and characterization of exosomes from human thymic tissue. Using electron microscopy, particle size determination, density gradient measurement, flow cytom...

  1. Characterization of hereditarily reversible posets

    Kukieła, Michał

    2013-01-01

    A poset P is called reversible if every order preserving bijective self map of P is an order automorphism. P is called hereditarily reversible if every subposet of P is reversible. We give a complete characterization of hereditarily reversible posets in terms of forbidden subsets. A similar result is stated also for preordered sets. As a corollary we extend the list of known examples of hereditarily reversible topological spaces.

  2. Physicochemical characterization of Gozitan Honey

    Everaldo Attard; Joseph Mizzi

    2013-01-01

    Honey quality is clearly defined in the EU Directive 2001/110/EC, and by Codex Alimentarius (Codex Stan 12-1981) and the International Honey Commission (IHC, 2002). Our investigation aimed to characterize the physicochemical properties of honey produced on a small island, Gozo which is situated near Malta.  Ten randomly collected honey samples were analysed for moisture content, pH, free acidity, water insoluble content, hydroxymethylfurfural (HMF) content and total phenolic compounds.  Moist...

  3. Some Characterizations of Krull Monoids

    Hwankoo Kim; Myeong Og Kim; Young Soo Park

    2007-01-01

    In this paper,Kaplansky-type theorems are given to characterize GCD-monoids and valuation monoids.Also,(unique) r-factorable monoids are defined and it is shown that S is a Krull monoid if and only if S is a unique t-factorable (resp.,w-factorable)monoid if and only if S is a t-factorable (resp.,w-factorable) t-Pr(u)fer monoid.

  4. Temporary storage area characterization report

    The preferred alternative identified in the Remedial Investigation/Feasibility Study (RI/FS) for the Weldon Spring Quarry Bulk Wastes is to remove the wastes from the quarry and transport them by truck to temporary storage facility at the chemical plant site. To support the RI/FS, this report provides data to characterize the temporary storage area (TSA) site and to ensure the suitability of the proposed location. 31 refs., 14 figs., 7 tabs

  5. Parametric characterization of aggregation functions

    Mesiar, Radko; Kolesárová, A.

    2009-01-01

    Roč. 160, č. 6 (2009), s. 816-831. ISSN 0165-0114 R&D Projects: GA ČR GA402/08/0618 Institutional research plan: CEZ:AV0Z10750506 Keywords : Aggregation function * Conjunction measure * Disjunction measure * Global/local parametric characterization * Idempotency measure Subject RIV: BA - General Mathematics Impact factor: 2.138, year: 2009 http://library.utia.cas.cz/separaty/2009/E/mesiar-parametriccharacterizationofaggregationfunctions.pdf

  6. Characterization of ultrafine aluminum nanoparticles

    Aluminum nanopowders with particle sizes ranging from ∼25 nm to 80 nm were characterized by a variety of methods. We present and compare the results from common powder characterization techniques including transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), BET gas adsorption surface area analysis, thermogravimetric analysis (TGA), photon correlation spectroscopy (PCS), and low angle laser light scattering (LALLS). Aluminum nanoparticles consist of an aluminum core with an aluminum oxide coating. HRTEM measurements of both the particle diameter and oxide layer thickness tend to be larger than those obtained from BET and TGA. LALLS measurements show a large degree of particle agglomeration in solution; therefore, primary particle sizes could not be determined. Furthermore, results from small-angle scattering techniques (SAS), including small-angle neutron (SANS) and x-ray (SAXS) scattering are presented and show excellent agreement with the BET, TGA, and HRTEM. The suite of analytical techniques presented in this paper can be used as a powerful tool in the characterization of many types of nanosized powders.

  7. Instrumentation for CTA site characterization

    Fruck, Christian; Ernenwein, Jean-Pierre; Mandát, Dušan; Schweizer, Thomas; Häfner, Dennis; Bulik, Tomasz; Cieslar, Marek; Costantini, Heide; Dominik, Michal; Ebr, Jan; Garczarczyk, Markus; Lorentz, Eckart; Pareschi, Giovanni; Pech, Miroslav; Puerto-Giménez, Irene; Teshima, Masahiro

    2015-01-01

    Many atmospheric and climatic criteria have to be taken into account for the selection of a suitable site for the next generation of imaging air-shower Cherenkov telescopes, the "Cherenkov Telescope Array" CTA. Such data are not available with sufficient precision or the comparability to allow for a comprehensive characterization of the proposed sites to be made. Identical cross-calibrated instruments have been developed which allow for precise comparison between sites, the cross-validation of existing data, and the ground-validation of satellite data. The site characterization work package of the CTA consortium opted to construct and deploy 9 copies of an autonomous multi-purpose weather sensor, incorporating an infrared cloud sensor a newly developed sensor for measuring the light of the night sky, and an All-Sky-Camera, the whole referred to as Autonomous Tool for Measuring Observatory Site COnditions PrEcisely (ATMOSCOPE). We present here the hardware that was combined into the ATMOSCOPE and characterize ...

  8. Sustainability Characterization for Additive Manufacturing.

    Mani, Mahesh; Lyons, Kevin W; Gupta, S K

    2014-01-01

    Additive manufacturing (AM) has the potential to create geometrically complex parts that require a high degree of customization, using less material and producing less waste. Recent studies have shown that AM can be an economically viable option for use by the industry, yet there are some inherent challenges associated with AM for wider acceptance. The lack of standards in AM impedes its use for parts production since industries primarily depend on established standards in processes and material selection to ensure the consistency and quality. Inability to compare AM performance against traditional manufacturing methods can be a barrier for implementing AM processes. AM process sustainability has become a driver due to growing environmental concerns for manufacturing. This has reinforced the importance to understand and characterize AM processes for sustainability. Process characterization for sustainability will help close the gaps for comparing AM performance to traditional manufacturing methods. Based on a literature review, this paper first examines the potential environmental impacts of AM. A methodology for sustainability characterization of AM is then proposed to serve as a resource for the community to benchmark AM processes for sustainability. Next, research perspectives are discussed along with relevant standardization efforts. PMID:26601038

  9. Waste characterization: What's on second?

    Waste characterization is the process whereby the physical properties and chemical composition of waste are determined. Waste characterization is an important element which is necessary to certify that waste meets the acceptance criteria for storage, treatment, or disposal. Department of Energy (DOE) Orders list and describe the germane waste form, package, and container criteria for the storage of both solid low-level waste package, and container criteria for the storage of both solid low-level waste (SLLW) and transuranic (TRU) waste, including chemical composition and compatibility, hazardous material content (e.g., lead), fissile material content, radioisotopic inventory, particulate content, equivalent alpha activity, thermal heat output, and absence of free liquids, explosives, and compressed gases. At the Oak Ridge National Laboratory (ORNL), the responsibility for waste characterization begins with the individual or individuals who generate the waste. The generator must be able to document the type and estimate the quantity of various materials (e.g., waste forms -- physical characteristics, chemical composition, hazardous materials, major radioisotopes) which have been placed into the waste container. Analyses of process flow sheets and a statistically valid sampling program can provide much of the required information as well as a documented level of confidence in the acquired data. A program is being instituted in which major generator facilities perform radionuclide assay of small packets of waste prior to being placed into a waste drum. 17 refs., 1 fig., 4 tabs

  10. Seismic characterization of fracture properties

    A critical component of site characterization and performance assessment involves the demonstration that any fluid flow which might reach the accessible environment is within acceptable limits. Various methods of analyzing flow in fractured rocks have been proposed, but choice of an appropriate method and its application to a specific site probably requires some knowledge of the spacing and length (or density) of fractures, their orientation and their hydraulic conductivity. Some of this information will undoubtedly come from geologic mapping on surface and in excavations, as well as from boreholes, cores and laboratory tests. However, it will be necessary to detect and characterize fractures in the rock mass between these direct observations. The remote detection and characterization of fractures by geophysical methods is, therefore, of considerable interest in connection with geologic repositories. The purpose of this paper is to show that there is a relationship, both empirical and theoretical, between the measured seismic response, the mechanical stiffness of fractures and their hydraulic conductivity. Laboratory measurements of the mechanical stiffness, hydraulic conductivity and seismic properties of natural fractures are summarized. A theoretical model for the amplitude and group time delay for compressional and shear waves transmitted across a single fracture is presented. Predictions based on this model are compared with laboratory measurements. Finally, the results for a single fracture are extended to multiple parallel fractures

  11. Sofia Observatory Performance and Characterization

    Temi, Pasquale; Miller, Walter; Dunham, Edward; McLean, Ian; Wolf, Jurgen; Becklin, Eric; Bida, Tom; Brewster, Rick; Casey, Sean; Collins, Peter; Jakob, Holger; Killebrew, Jana; Lampater, Ulrich; Mandushev, Georgi; Marcum, Pamela; Meyer, Allan; Pfueller, Enrico; Reinacher, Andreas; Roeser, Hans-Peter; Savage, Maureen; Teufel, Stefan; Wiedemann, Manuel

    2012-01-01

    The Stratospheric Observatory for Infrared Astronomy (SOFIA) has recently concluded a set of engineering flights for Observatory performance evaluation. These in-flight opportunities have been viewed as a first comprehensive assessment of the Observatory's performance and will be used to address the development activity that is planned for 2012, as well as to identify additional Observatory upgrades. A series of 8 SOFIA Characterization And Integration (SCAI) flights have been conducted from June to December 2011. The HIPO science instrument in conjunction with the DSI Super Fast Diagnostic Camera (SFDC) have been used to evaluate pointing stability, including the image motion due to rigid-body and flexible-body telescope modes as well as possible aero-optical image motion. We report on recent improvements in pointing stability by using an Active Mass Damper system installed on Telescope Assembly. Measurements and characterization of the shear layer and cavity seeing, as well as image quality evaluation as a function of wavelength have been performed using the HIPO+FLITECAM Science Instrument configuration (FLIPO). A number of additional tests and measurements have targeted basic Observatory capabilities and requirements including, but not limited to, pointing accuracy, chopper evaluation and imager sensitivity. SCAI activities included in-flight partial Science Instrument commissioning prior to the use of the instruments as measuring engines. This paper reports on the data collected during the SCAI flights and presents current SOFIA Observatory performance and characterization.

  12. Ultrasonic Characterization of Aerospace Composites

    Leckey, Cara; Johnston, Patrick; Haldren, Harold; Perey, Daniel

    2015-01-01

    Composite materials have seen an increased use in aerospace in recent years and it is expected that this trend will continue due to the benefits of reduced weight, increased strength, and other factors. Ongoing work at NASA involves the investigation of the large-scale use of composites for spacecraft structures (SLS components, Orion Composite Crew Module, etc). NASA is also involved in work to enable the use of composites in advanced aircraft structures through the Advanced Composites Project (ACP). In both areas (space and aeronautics) there is a need for new nondestructive evaluation and materials characterization techniques that are appropriate for characterizing composite materials. This paper will present an overview of NASA's needs for characterizing aerospace composites, including a description of planned and ongoing work under ACP for the detection of composite defects such as fiber waviness, reduced bond strength, delamination damage, and microcracking. The research approaches include investigation of angle array, guided wave, and phase sensitive ultrasonic methods. The use of ultrasonic simulation tools for optimizing and developing methods will also be discussed.

  13. Mineralogical characterization of mine waste

    Highlights: • Mineral characterization in mine waste is critical for prediction of metal leaching. • Analytical methods and examples are reviewed, including advanced techniques. • Quantitative mineralogy is described as a promising new method. • Example shows that understanding secondary arsenic minerals improves risk assessment. - Abstract: The application of mineralogical characterization to mine waste has the potential to improve risk assessment, guide appropriate mine planning for planned and active mines and optimize remediation design at closed or abandoned mines. Characterization of minerals, especially sulphide and carbonate phases, is particularly important for predicting the potential for acidic drainage and metal(loid) leaching. Another valuable outcome from mineralogical studies of mine waste is an understanding of the stability of reactive and metal(loid)-bearing minerals under various redox conditions. This paper reviews analytical methods that have been used to study mine waste mineralogy, including conventional methods such as X-ray diffraction and scanning electron microscopy, and advanced methods such as synchrotron-based microanalysis and automated mineralogy. We recommend direct collaboration between researchers and mining companies to choose the optimal mineralogical techniques to solve complex problems, to co-publish the results, and to ensure that mineralogical knowledge is used to inform mine waste management at all stages of the mining life cycle. A case study of arsenic-bearing gold mine tailings from Nova Scotia is presented to demonstrate the application of mineralogical techniques to improve human health risk assessment and the long-term management of historical mine wastes

  14. Synthesis and characterization of copper, polyimide and TIPS-pentacene layers for the development of a solution processed fibrous transistor

    B. Van Genabet

    2011-12-01

    Full Text Available A study was performed for the development of a flexible organic field effect transistor starting from a polyester fibre as substrate material. Focus of subsequent layer deposition was on low temperature soluble processes to allow upscaling. Gate layer consists out of a pyrrole polymerization and copper coating step. Polyimide dielectric layer was deposited using dipcoating. Gold electrodes were vacuum evaporated and patterned via mask fibre shadowing. The active layer consisted of a soluble p-type TIPS-pentacene organic semiconductor. Different deposition techniques have been examined. Considerable progress in development of a transistor has been made.

  15. NCL Objective #3 - Nanotechnology Characterization Lab (NCL)

    The Nanotechnology Characterization Lab (NCL) Objective #3: Identify and Characterize Critical Parameters Related to Nanomaterials' Absorption, Distribution, Metabolism, Excretion, and Acute Toxicity (ADME/Tox) Profile in Animal Models.

  16. Gas characterization system software acceptance test report

    This document details the results of software acceptance testing of gas characterization systems. The gas characterization systems will be used to monitor the vapor spaces of waste tanks known to contain measurable concentrations of flammable gases

  17. Gas characterization system software acceptance test procedure

    This document details the Software Acceptance Testing of gas characterization systems. The gas characterization systems will be used to monitor the vapor spaces of waste tanks known to contain measurable concentrations of flammable gases

  18. 10 CFR 60.15 - Site characterization.

    2010-01-01

    ... 10 Energy 2 2010-01-01 2010-01-01 false Site characterization. 60.15 Section 60.15 Energy NUCLEAR... Preapplication Review § 60.15 Site characterization. (a) Prior to submittal of an application for a license to be issued under this part DOE shall conduct a program of site characterization with respect to the site...

  19. 10 CFR 63.15 - Site characterization.

    2010-01-01

    ... 10 Energy 2 2010-01-01 2010-01-01 false Site characterization. 63.15 Section 63.15 Energy NUCLEAR... MOUNTAIN, NEVADA Licenses Preapplication Review § 63.15 Site characterization. (a) DOE shall conduct a program of site characterization with respect to the Yucca Mountain site before it submits an...

  20. A Characterization of the Negative Binomial Distribution

    Kolev, Nikolay(Department of Physics, University of Regina, SK S4S 0A2, Canada); Minkova, Leda

    2000-01-01

    Only a few characterizations have been obtained in literatute for the negative binomial distribution (see Johnson et al., Chap. 5, 1992). In this article a characterization of the negative binomial distribution related to random sums is obtained which is motivated by the geometric distribution characterization given by Khalil et al. (1991). An interpretation in terms of an unreliable system is given.

  1. The Rings Characterized by Minimal Left Ideals

    Jun Chao WEI

    2005-01-01

    We study these rings with every minimal left ideal being a projective, direct summand and a p-injective module, respectively. Some characterizations of these rings are given, and the relations among them are obtained. With these rings, we characterize semisimple rings. Finally, we introduce MC2 rings, and give some characterizations of MC2 rings.

  2. Characterization of Mineralogy Across Vesta

    De Sanctis, M. C.; Ammannito, E.; Capria, M. T.; Capaccioni, F.; Carraro, F.; Fonte, S.; Frigeri, A.; Magni, G.; Marchi, S.; Palomba, E.; Tosi, F.; Zambon, F.; McCord, T. B.; McFadden, L. A.; McSween, H.; Mittlefehldt, D. W.; Pieters, C. M.; Raymond, C. A.; Russell, C. T.

    2012-01-01

    Dawn VIR spectra are characterized by pyroxene absorptions and no clear evidence for abundant other minerals are observed at the scale of the present measurements. Even though Vesta spectra are dominated by pyroxenes, spectral variation at regional and local scales are evident and distinct color units are identified. Although almost all of the surface materials exhibit spectra like those of howardites, some large units can be interpreted to be material richer in diogenite (based on pyroxenes band depths and band centers) and some others like eucrite-rich howardite units. VIR data strongly indicate that the south polar region (Rheasilvia) has its own spectral characteristics, indicating the presence of Mg-pyroxene-rich terrains (diogenite-like), while the equatorial areas have swallower band depths and average band centers at slightly longer wavelengths, consistent with more eucrite rich materials. Vesta surface shows considerable diversity at smaller scales (tens of km), in terms of spectral reflectance and emission, band depths and slopes. Many bright and dark spots are present on Vesta. Dark spots have low reflectance at visible wavelengths and are spectrally characterized by shallower 1 and 2 micron bands with respect the surrounding terrains. Bright materials have high reflectance and are often spectrally characterized by deep pyroxenes absorption bands. Vesta presents complex geology/topography and the mineral distribution is often correlated with geological and topographical structures. Ejecta from large craters have distinct spectral behaviors, and materials exposed in the craters show distinct spectra on floors and rims. VIR reveals the mineralogical variation of Vesta s crustal stratigraphy on local and global scales. Maps of spectral parameters show surface and subsurface unit compositions in their stratigraphic context. The hypothesis that Vesta is the HED parent body is consistent with, and strengthened by, the geologic and spectral context for pyroxene

  3. Manganese borohydride; synthesis and characterization

    Richter, Bo; Ravnsbæk, Dorthe B.; Tumanov, Nikolay; Filinchuk, Yaroslav; Jensen, Torben R.

    2015-01-01

    Solvent-based synthesis and characterization of α-Mn(BH4)2 and a new nanoporous polymorph of manganese borohydride, γ-Mn(BH4)2, via a new solvate precursor, Mn(BH4)2·1/2S(CH3)2, is presented. Manganese chloride is reacted with lithium borohydride in a toluene/dimethylsulfide mixture at room temperature, which yields halide and solvent-free manganese borohydride after extraction with dimethylsulfide (DMS) and subsequent removal of residual solvent. This work constitutes the first example of es...

  4. Advanced Fine Particulate Characterization Methods

    Steven Benson; Lingbu Kong; Alexander Azenkeng; Jason Laumb; Robert Jensen; Edwin Olson; Jill MacKenzie; A.M. Rokanuzzaman

    2007-01-31

    The characterization and control of emissions from combustion sources are of significant importance in improving local and regional air quality. Such emissions include fine particulate matter, organic carbon compounds, and NO{sub x} and SO{sub 2} gases, along with mercury and other toxic metals. This project involved four activities including Further Development of Analytical Techniques for PM{sub 10} and PM{sub 2.5} Characterization and Source Apportionment and Management, Organic Carbonaceous Particulate and Metal Speciation for Source Apportionment Studies, Quantum Modeling, and High-Potassium Carbon Production with Biomass-Coal Blending. The key accomplishments included the development of improved automated methods to characterize the inorganic and organic components particulate matter. The methods involved the use of scanning electron microscopy and x-ray microanalysis for the inorganic fraction and a combination of extractive methods combined with near-edge x-ray absorption fine structure to characterize the organic fraction. These methods have direction application for source apportionment studies of PM because they provide detailed inorganic analysis along with total organic and elemental carbon (OC/EC) quantification. Quantum modeling using density functional theory (DFT) calculations was used to further elucidate a recently developed mechanistic model for mercury speciation in coal combustion systems and interactions on activated carbon. Reaction energies, enthalpies, free energies and binding energies of Hg species to the prototype molecules were derived from the data obtained in these calculations. Bimolecular rate constants for the various elementary steps in the mechanism have been estimated using the hard-sphere collision theory approximation, and the results seem to indicate that extremely fast kinetics could be involved in these surface reactions. Activated carbon was produced from a blend of lignite coal from the Center Mine in North Dakota and

  5. Multifractal approach for seafloor characterization

    Chakraborty, B.; Haris, K.; Latha, G.; Maslov, N.; Menezes, A.A.A.

    of submerged objects have an extremely wide range of spatio-temporal scales necessitating application of ‘power law’ to carry out the analyses. The ‘power law’ behavior in such instances requires multifractal analyses [1] in order to determine if both... space. One way to characterize the statistics of stochastic processes is to use its statistical moments. The statistical moments of a multifractal process is a power law that can be expressed as )(qKq λφλ >=< , where φλ is the scale by scale conserved...

  6. Characterization of Photoreceivers for LISA

    Cervantes, F. Guzman; Livas, J.; Silverberg, R.; Buchanan, E.; Stebbins, R.

    2010-01-01

    LISA will use quadrant photo receivers as front-end devices for the phase meter measuring the motion of drag-free test masses in both angular orientation and separation. We have set up a laboratory testbed for the characterization of photo receivers. Some of the limiting noise sources have been identified and their contribution has been either measured or determined from the measured data. We have built a photo receiver with a 0.5 mm diameter quadrant photodiode with an equivalent input noise of better than 1.8 pA/(square root of)Hz below 20 MHz and a 3 dB bandwidth of 34 MHz.

  7. Characterization of Mexican zeolite minerals

    50% of the Mexican territory is formed by volcanic sequences of the Pliocene type, which appear extensively in the northwest states (Sonora, Sinaloa, Chihuahua, Durango) and west of Mexico (Jalisco and Nayarit), in central Mexico (Zacatecas, Guanajuato, San Luis Potosi, Queretaro, Hidalgo) and south of Mexico (Guerrero, Oaxaca); therefore, it is to be expected that in our country big locations of natural zeolites exist in its majority of the clinoptilolite type. The present study was focused toward the characterization of two Mexican natural zeolite rocks presumably of the clinoptilolite and filipsite types, one of them comes from the state of Chihuahua and the other of a trader company of non metallic minerals, due that these materials are not characterized, its are not known their properties completely and therefore, the uses that can be given to these materials. In this investigation work it was carried out the characterization of two Mexican zeolite rocks, one coming from the Arroyo zone, municipality of La Haciendita, in the state of Chihuahua; and the other one was bought to a trader company of non metallic minerals. The two zeolites so much in their natural form as conditioned with sodium; they were characterized by means of X-ray diffraction, scanning electron microscopy of high vacuum and elementary microanalysis (EDS), surface area analysis (BET), thermal gravimetric analysis. To differentiate the heulandite crystalline phase of the other clinoptilolite rock, its were carried out thermal treatments. The quantification of Al, Na, Ca, K, Mg, Fe was carried out in solution, by means of atomic absorption spectroscopy and the quantity of Si was determined by gravimetry. The zeolite rocks presented for the major part the crystalline heulandite and clinoptilolite phases for the most part, and it was found that the zeolite coming from the state of Chihuahua possesses a bigger content of heulandite and the denominated filipsite it is really a zeolite

  8. Neutron Characterization for Additive Manufacturing

    Watkins, Thomas; Bilheux, Hassina; An, Ke; Payzant, Andrew; DeHoff, Ryan; Duty, Chad; Peter, William; Blue, Craig; Brice, Craig A.

    2013-01-01

    Oak Ridge National Laboratory (ORNL) is leveraging decades of experience in neutron characterization of advanced materials together with resources such as the Spallation Neutron Source (SNS) and the High Flux Isotope Reactor (HFIR) shown in Fig. 1 to solve challenging problems in additive manufacturing (AM). Additive manufacturing, or three-dimensional (3-D) printing, is a rapidly maturing technology wherein components are built by selectively adding feedstock material at locations specified by a computer model. The majority of these technologies use thermally driven phase change mechanisms to convert the feedstock into functioning material. As the molten material cools and solidifies, the component is subjected to significant thermal gradients, generating significant internal stresses throughout the part (Fig. 2). As layers are added, inherent residual stresses cause warping and distortions that lead to geometrical differences between the final part and the original computer generated design. This effect also limits geometries that can be fabricated using AM, such as thin-walled, high-aspect- ratio, and overhanging structures. Distortion may be minimized by intelligent toolpath planning or strategic placement of support structures, but these approaches are not well understood and often "Edisonian" in nature. Residual stresses can also impact component performance during operation. For example, in a thermally cycled environment such as a high-pressure turbine engine, residual stresses can cause components to distort unpredictably. Different thermal treatments on as-fabricated AM components have been used to minimize residual stress, but components still retain a nonhomogeneous stress state and/or demonstrate a relaxation-derived geometric distortion. Industry, federal laboratory, and university collaboration is needed to address these challenges and enable the U.S. to compete in the global market. Work is currently being conducted on AM technologies at the ORNL

  9. FNAS materials processing and characterization

    Golben, John P.

    1991-01-01

    Research on melt-sintered high temperature superconducting materials is presented. The vibrating sample magnetometer has become a useful characterization tool for the study of high temperature superconductors. Important information regarding the superconducting properties of a sample can be obtained without actually making contact with the sample itself. A step toward microgravity processing of high temperature superconductors was taken. In the future, the samples need to be optimized prior to this processing of the sample before the specific effects of the microgravity environment can be isolated. A series of melt-sintered samples show that bulk processing of high temperature superconductors is getting better.

  10. Instrumentation for tropospheric aerosol characterization

    Shi, Z.; Young, S.E.; Becker, C.H.; Coggiola, M.J. [SRI International, Menlo Park, CA (United States); Wollnik, H. [Giessen Univ. (Germany)

    1997-12-31

    A new instrument has been developed that determines the abundance, size distribution, and chemical composition of tropospheric and lower stratospheric aerosols with diameters down to 0.2 {mu}m. In addition to aerosol characterization, the instrument also monitors the chemical composition of the ambient gas. More than 25.000 aerosol particle mass spectra were recorded during the NASA-sponsored Subsonic Aircraft: Contrail and Cloud Effects Special Study (SUCCESS) field program using NASA`s DC-8 research aircraft. (author) 7 refs.

  11. Acoustic characterization of rehabilitated cloisters

    A. P. O. Carvalho; S. R. C. Vilela

    2008-01-01

    This paper presents the results of field measurements in eight rehabilitated cloisters of old monasteries in Portugal (length: 20 to 35 m and height: 3.3 to 6.3 m) regarding their acoustic behavior to two objective parameters: RT and RASTI. The goal is to characterize the acoustic effect of the rehabilitation done on theses spaces to adapt them to new uses. All these cloisters had recently their galleries#8217; openings to the central yard closed with glass panels. Simple formulas were obtain...

  12. Active thermography for potato characterization

    Hsieh, Sheng-Jen; Sun, Chih-Chen

    2008-03-01

    This paper describes the design of a semi-automated heating and scanning system and analytic method for potato characterization. Potatoes are heated using lamps in a heating chamber and then transferred on a movable fixture to an imaging chamber. A non-linear model was designed to predict which potatoes have excessive sugar defects and the model was evaluated with good results. Results from this research will benefit potato growers and manufacturers/producers of potato-based products such as chips and fries.

  13. Baseline Graphite Characterization: First Billet

    Mark C. Carroll; Joe Lords; David Rohrbaugh

    2010-09-01

    The Next Generation Nuclear Plant Project Graphite Research and Development program is currently establishing the safe operating envelope of graphite core components for a very high temperature reactor design. To meet this goal, the program is generating the extensive amount of quantitative data necessary for predicting the behavior and operating performance of the available nuclear graphite grades. In order determine the in-service behavior of the graphite for the latest proposed designs, two main programs are underway. The first, the Advanced Graphite Creep (AGC) program, is a set of experiments that are designed to evaluate the irradiated properties and behavior of nuclear grade graphite over a large spectrum of temperatures, neutron fluences, and compressive loads. Despite the aggressive experimental matrix that comprises the set of AGC test runs, a limited amount of data can be generated based upon the availability of space within the Advanced Test Reactor and the geometric constraints placed on the AGC specimens that will be inserted. In order to supplement the AGC data set, the Baseline Graphite Characterization program will endeavor to provide supplemental data that will characterize the inherent property variability in nuclear-grade graphite without the testing constraints of the AGC program. This variability in properties is a natural artifact of graphite due to the geologic raw materials that are utilized in its production. This variability will be quantified not only within a single billet of as-produced graphite, but also from billets within a single lot, billets from different lots of the same grade, and across different billets of the numerous grades of nuclear graphite that are presently available. The thorough understanding of this variability will provide added detail to the irradiated property data, and provide a more thorough understanding of the behavior of graphite that will be used in reactor design and licensing. This report covers the

  14. Characterization of minerals, metals and materials

    Hwang, Jiann-Yang; Bai, Chengguang; Carpenter, John; Cai, Mingdong; Firrao, Donato; Kim, Byoung-Gon

    2012-01-01

    This state-of-the-art reference contains chapters on all aspects of the characterization of minerals, metals, and materials. The title presents papers from one of the largest yearly gatherings of materials scientists in the world and thoroughly discusses the characterization of minerals, metals, and materials The scope includes current industrial applications and research and developments in the following areas:  Characterization of Ferrous Metals Characterization of Non-Ferrous Materials Characterization of Minerals and Ceramics Character

  15. BNFL Report Glass Formers Characterization

    The objective of this task was to obtain powder property data on candidate glass former materials, sufficient to guide conceptual design and estimate the cost of glass former handling facilities as requested under Part B1 of BNFL Technical and Development Support. Twenty-nine glass forming materials were selected and obtained from vendors for the characterization of their physical properties, durability in caustic solution, and powder flow characteristics. A glass former was selected based on the characterization for each of the ten oxide classes required for Envelope A, B, and C mixtures. Three blends (A, B, and C) were prepared based on formulations provided by Vitreous State Laboratory and evaluated with the same methods employed for the glass formers. The properties obtained are presented in a series of attached Tables. It was determined that five of the ten glass formers, (kyanite, iron oxide, titania, zircon, and zinc oxide) have the potential to cause some level of solids f low problems. In addition, all of the blends may require consideration for their handling. A number of engineering considerations and recommendations were prepared based on the experimental findings, experience, and other process considerations. Recommendations for future testing are included. In conjunction with future work, it is recommended that a professional consultant be engaged to guide and assist with testing and design input

  16. Solar Filament Extraction and Characterizing

    Yuan, Yuan; Shih, F. Y.; Jing, J.; Wang, H.

    2010-05-01

    This paper presents a new method to extract and characterize solar filaments from H-alpha full-disk images produced by Big Bear Solar Observatory. A cascading Hough Transform method is designed to identify solar disk center location and radius. Solar disks are segmented from the background, and unbalanced illumination on the surface of solar disks is removed using polynomial surface fitting. And then a localized adaptive thresholding is employed to extract solar filament candidates. After the removal of small solar filament candidates, the remaining larger candidates are used as the seeds of region growing. The procedure of region growing not only connects broken filaments but also generate complete shape for each filament. Mathematical morphology thinning is adopted to produce the skeleton of each filament, and graph theory is used to prune branches and barbs to get the main skeleton. The length and the location of the main skeleton is characterized. The proposed method can help scientists and researches study the evolution of solar filament, for instance, to detect solar filament eruption. The presented method has already been used by Space Weather Research Lab of New Jersey Institute of Technology (http://swrl.njit.edu) to generate the solar filament online catalog using H-alpha full-disk images of Global H-alpha Network (http://swrl.njit.edu/ghn_web/).

  17. Quantitative Characterization of Nanostructured Materials

    Dr. Frank (Bud) Bridges, University of California-Santa Cruz

    2010-08-05

    The two-and-a-half day symposium on the "Quantitative Characterization of Nanostructured Materials" will be the first comprehensive meeting on this topic held under the auspices of a major U.S. professional society. Spring MRS Meetings provide a natural venue for this symposium as they attract a broad audience of researchers that represents a cross-section of the state-of-the-art regarding synthesis, structure-property relations, and applications of nanostructured materials. Close interactions among the experts in local structure measurements and materials researchers will help both to identify measurement needs pertinent to real-world materials problems and to familiarize the materials research community with the state-of-the-art local structure measurement techniques. We have chosen invited speakers that reflect the multidisciplinary and international nature of this topic and the need to continually nurture productive interfaces among university, government and industrial laboratories. The intent of the symposium is to provide an interdisciplinary forum for discussion and exchange of ideas on the recent progress in quantitative characterization of structural order in nanomaterials using different experimental techniques and theory. The symposium is expected to facilitate discussions on optimal approaches for determining atomic structure at the nanoscale using combined inputs from multiple measurement techniques.

  18. BNFL Report Glass Formers Characterization

    Schumacher, R.F.

    2000-07-27

    The objective of this task was to obtain powder property data on candidate glass former materials, sufficient to guide conceptual design and estimate the cost of glass former handling facilities as requested under Part B1 of BNFL Technical and Development Support. Twenty-nine glass forming materials were selected and obtained from vendors for the characterization of their physical properties, durability in caustic solution, and powder flow characteristics. A glass former was selected based on the characterization for each of the ten oxide classes required for Envelope A, B, and C mixtures. Three blends (A, B, and C) were prepared based on formulations provided by Vitreous State Laboratory and evaluated with the same methods employed for the glass formers. The properties obtained are presented in a series of attached Tables. It was determined that five of the ten glass formers, (kyanite, iron oxide, titania, zircon, and zinc oxide) have the potential to cause some level of solids f low problems. In addition, all of the blends may require consideration for their handling. A number of engineering considerations and recommendations were prepared based on the experimental findings, experience, and other process considerations. Recommendations for future testing are included. In conjunction with future work, it is recommended that a professional consultant be engaged to guide and assist with testing and design input.

  19. BNFL Report Glass Formers Characterization

    Schumacher, R.F.

    2000-07-27

    The objective of this task was to obtain powder property data on candidate glass former materials, sufficient to guide conceptual design and estimate the cost of glass former handling facilities as requested under Part B1 of BNFL Technical and Development Support. Twenty-nine glass forming materials were selected and obtained from vendors for the characterization of their physical properties, durability in caustic solution, and powder flow characteristics. A glass former was selected based on the characterization for each of the ten oxide classes required for Envelope A, B, and C mixtures. Three blends (A, B, and C) were prepared based on formulations provided by Vitreous State Laboratory and evaluated with the same methods employed for the glass formers. The properties obtained are presented in a series of attached Tables. It was determined that five of the ten glass formers, (kyanite, iron oxide, titania, zircon, and zinc oxide) have the potential to cause some level of solids f low problems. The problems might include arching or ratholing in the silo/hopper. In addition, all of the blends may require consideration for their handling.

  20. Characterization of Polymeric Nanofiltration Membranes

    Simoncic, B.

    2007-11-01

    Full Text Available As membrane processes are increasingly used in industrial applications, there is a growing interest in methods of membrane characterization. Traditional membrane characteristics, such as cut-off value and pore size distribution, are being supplemented by membrane surface characteristics, such as charge density or zeta potential and hydrophobicity. This study, therefore, characterizes the three different polymeric membranes used (NFT-50, DL and DK. The molecular mass cut-off (MMCO value was determined using a set of reference solutes within the molecular range 150-600 Da, whereas streaming potential measurements enabled quantification of the surface charge characteristics. Hydrophobicity was studied using contact angle measurements. The results indicated that even though all three membranes had very similar layer compositions which consisted of poly(piperazneamide, as top layers they showed different values of measured quantitive. The NFT-50 membrane had the lowest MMCO value and the most hydrophilic membrane surface, followed by DK and DL. Membrane fouling as measured by flux reduction was determined by streaming potential measurements and accompanied by a positive change in zeta potential.

  1. BNFL Report Glass Formers Characterization

    The objective of this task was to obtain powder property data on candidate glass former materials, sufficient to guide conceptual design and estimate the cost of glass former handling facilities as requested under Part B1 of BNFL Technical and Development Support. Twenty-nine glass forming materials were selected and obtained from vendors for the characterization of their physical properties, durability in caustic solution, and powder flow characteristics. A glass former was selected based on the characterization for each of the ten oxide classes required for Envelope A, B, and C mixtures. Three blends (A, B, and C) were prepared based on formulations provided by Vitreous State Laboratory and evaluated with the same methods employed for the glass formers. The properties obtained are presented in a series of attached Tables. It was determined that five of the ten glass formers, (kyanite, iron oxide, titania, zircon, and zinc oxide) have the potential to cause some level of solids f low problems. The problems might include arching or ratholing in the silo/hopper. In addition, all of the blends may require consideration for their handling

  2. Nanodosimetric characterization of ion beams

    Bug, Marion Ute; Hilgers, Gerhard; Baek, Woon Yong; Rabus, Hans

    2014-08-01

    The characterization of particle track structure is essential for an estimation of radiobiological effects, particularly in the case of densely ionizing radiation. The particle track structure can be characterized by nanodosimetric quantities which are measurable by means of a nanodosimeter. Results obtained from experiments with the nanodosimeter can be used to validate track structure simulations, which are essential for estimating track structure parameters in biological material. For this purpose, the dedicated Monte Carlo code PTra has been developed to simulate the nanodosimeter setup as well as nanometric targets consisting of water. Recently, electron-impact cross section data of DNA constituents measured at PTB were implemented into PTra. A calculation of nanodosimetric quantities in DNA-analog media shows considerable differences to results obtained in water medium, particularly for electron energies lower than 200 eV. These discrepancies become more considerable when nanodosimetric quantities are used to estimate biological effects. This paper aims to provide an overview of the present status of nanodosimetry, focusing on the experimental and simulation work at PTB. Furthermore, the suitability of simple models directly linking nanodosimetric track structure characteristics and radiobiological effectiveness is discussed.

  3. Characterization and Metrology for Nanoelectronics

    Diebold, Alain C.

    2007-09-01

    Despite the challenges associated with the cost and technological innovation, the semiconductor industry has introduced nanoelectronics into the market place. By extending traditional CMOS (complimentary metal oxide semiconductor transistors) through new materials in both the devices and on-chip interconnect, planar CMOS is already manufactured with transistor gate lengths less than 50 nm. Further extending CMOS will not only require new materials, but it may also drive the use of new non-planar device structures for transistors and new approaches for on and off-chip interconnection. At some point, CMOS extension may no longer be possible, and then a new switch would be necessary. The transition between CMOS extension and planar CMOS could involve the gradual incorporation of Beyond CMOS technology. The number of candidates continues to grow even as some possible technology is removed from consideration. Characterization and Metrology is finding each step in this transition to be a great challenge. This paper overviews the characterization and metrology necessary for both CMOS extension and beyond CMOS semiconductor technology. The International Technology Roadmap for Semiconductors is used a guide that provides a roadmap for both metrology and process technology that extends to beyond CMOS materials and devices.(1)

  4. Characterization of soils containing adipocere.

    Fiedler, S; Schneckenberger, K; Graw, M

    2004-11-01

    The formation of adipocere (commonly known as grave wax), a spontaneous inhibition of postmortem changes, has been extensively analyzed in forensic science. However, soils in which adipocere formation occurs have never been described in detail. Therefore, this study is intended as a first step in the characterization of soils containing adipocere. Two grave soils (Gleyic Anthrosols) that prevent the timely reuse of graves due to the occurrence of adipocere and a control soil (Gleyic Luvisol) were selected from a cemetery in the Central Black Forest (Southwest Germany). Descriptions of soil morphology and a wide assay of physical, chemical, and microbiologic soil characteristics were accomplished. In contrast to the control soil, the grave soils were characterized by lower bulk density and pH. The degradation of the soil structure caused by digging led to a higher water table and the expansion of the reducing conditions in the graves where the prevalent absence of oxygen in range of the coffins inhibited decomposition processes. Although the formation of adipocere led to the conservation of the buried corpses, phosphorus, dissolved organic carbon, and cadavarine leaching from the graves was observed. Microbial biomass and microbial activity were higher in the control soil and hence reflected the inert character of adipocere. The study results clearly show the need for additional approaches in forensic, pedologic, and microbiologic research. PMID:15499507

  5. Topographic characterization of glazed surfaces

    Detailed characterization of surface microstructure, i.e. phase composition and surface geometry, has become an important criterion of glazed ceramics. Topographic characterization is an important parameter in, e.g. estimating the influence of additional films on the average roughness of a surface. Also, the microscaled and nanoscaled roughnesses correlate with the cleanability and the self-cleaning properties of the surfaces. In this work the surface geometry of several matte glazes were described by topography and roughness as given by whitelight confocal microscopy and atomic force microscopy. Different measuring parameters were compared to justify the usefulness of the techniques in giving a comprehensive description of the surface microstructure. The results suggest that confocal microscopy is well suited for giving reliable topographical parameters for matte surfaces with microscaled crystals in the surfaces. Atomic force microscopy was better suited for smooth surfaces or for describing the local topographic parameters of closely limited areas, e.g. the surroundings of separate crystals in the surface

  6. Synthesis and TDDFT Investigation of New Maleimide Derivatives Bearing Pyrrole and Indole Ring

    Yasuhiro Shigemitsu

    2009-01-01

    density-functional theory (TDDFT calculations were systematically performed in order to elucidate their structure-color relationships, using a set of exchange-correlation (XC functionals. The TDDFT computational scheme employing PCM-TDDFT/6-31+G(d,p//DFT/6-311G(d,p level of theory gave qualitatively satisfactory results in their max predictions.

  7. Synthesis, photochromism and holographic optical recording of a novel diarylethene bearing a pyrrole unit

    A unsymmetrical photochromic diarylethene, 1-[2-methyl-5-(3-fluorophenyl)-3-thienyl]-2 -(2-cyano-1,5-dimethyl-4-pyrryl)hexafluorocyclopentene (1o), was synthesized. The photoconversion ratios from open-ring to closed-ring isomers at photostationary state under UV irradiation in hexane solution was measured by HPLC, and the properties, including photochromism and fluorescence properties were also investigated systematically. The results showed that this compound had good thermal stability and exhibited reversible photochromism, changing from colorless to blue after irradiation with UV light both in solution and in PMMA amorphous film. The open-ring isomer of the diarylethene 1 exhibited relatively strong fluorescence at 427 nm in hexane solution (5x10-5 mol/L) when excited at 340 nm. The fluorescence intensity decreased along with the photochromism upon irradiation with 297 nm light and its closed-ring isomer showed almost no fluorescence. Using diarylethene 1 as recording medium, polarization holographic optical recording was carried out successfully.

  8. Synthesis, photochromism and holographic optical recording of a novel diarylethene bearing a pyrrole unit

    Liu Gang; Liu Ming; Pu Shouzhi; Fan Congbin, E-mail: pushouzhi@tsinghua.org.cn [Jiangxi Key Laboratory of Organic Chemistry, Jiangxi Science and Technology Normal University, Nanchang 330013 (China)

    2011-02-01

    A unsymmetrical photochromic diarylethene, 1-[2-methyl-5-(3-fluorophenyl)-3-thienyl]-2 -(2-cyano-1,5-dimethyl-4-pyrryl)hexafluorocyclopentene (1o), was synthesized. The photoconversion ratios from open-ring to closed-ring isomers at photostationary state under UV irradiation in hexane solution was measured by HPLC, and the properties, including photochromism and fluorescence properties were also investigated systematically. The results showed that this compound had good thermal stability and exhibited reversible photochromism, changing from colorless to blue after irradiation with UV light both in solution and in PMMA amorphous film. The open-ring isomer of the diarylethene 1 exhibited relatively strong fluorescence at 427 nm in hexane solution (5x10{sup -5} mol/L) when excited at 340 nm. The fluorescence intensity decreased along with the photochromism upon irradiation with 297 nm light and its closed-ring isomer showed almost no fluorescence. Using diarylethene 1 as recording medium, polarization holographic optical recording was carried out successfully.

  9. The Influence of Preparation Conditions on the Electrical Conductivity of Poly N-Methyl-pyrrole Films

    Vidanapathirana, K.; Careem, M.A.; Skaarup, Steen; West, Keld

    electrical conductivity has been investigated. The conductivity was measured by the in situ method using a specially prepared two-band microelectrode. The current density used during the polymerization has a considerable influence on the conductivity, as earlier observed for polypyrrole in non......-aqueous electrolytes. The conductivity changes with the size of the anion and the concentration of the electrolyte as well as on the temperature at which the polymerization was carried out. Polymer films formed at relatively higher temperatures had lower conductivities and were not able to insert as many counterions...

  10. Site-selective nanoscale-polymerization of pyrrole on gold nanoparticles via plasmon induced charge separation

    Takahashi, Y.; Furukawa, Y.; Ishida, T.; Yamada, S.

    2016-04-01

    We proposed a nanoscale oxidative polymerization method which enables site-selective deposition on the surface of gold nanoparticles (AuNPs) combined with TiO2 by using plasmon induced charge separation (PICS) under visible-to-near infrared (IR) light irradiation. The method also revealed that the anodic site of PICS was located at the surface of AuNPs.We proposed a nanoscale oxidative polymerization method which enables site-selective deposition on the surface of gold nanoparticles (AuNPs) combined with TiO2 by using plasmon induced charge separation (PICS) under visible-to-near infrared (IR) light irradiation. The method also revealed that the anodic site of PICS was located at the surface of AuNPs. Electronic supplementary information (ESI) available. See DOI: 10.1039/c6nr01531j

  11. An interior needle electropolymerized pyrrole-based coating for headspace solid-phase dynamic extraction

    A headspace solid-phase dynamic extraction (HS-SPDE) technique was developed by the use of polypyrrole (PPy) sorbent, electropolymerized inside the surface of a needle, as a possible alternative to solid-phase microextraction (SPME). Thermal desorption was subsequently, employed to transfer the extracted analytes into the injection port of a gas chromatography-mass spectrometry (GC-MS). The PPy sorbent including polypyrrole-dodecyl sulfate (PPy-DS) was deposited on the interior surface of a stainless steel needle from the corresponding aqueous electrolyte by applying a constant deposition potential. The homogeneity and the porous surface structure of the coating were examined using the scanning electron microscopy (SEM). The developed method was applied to the trace level extraction of some polycyclic aromatic hydrocarbons (PAHs) from aqueous sample. In order to enhance the extraction efficiency and increase the partition coefficient of analytes, the stainless steel needle was cooled at 5 deg. C, while the sample solution was kept at 80 deg. C. Optimization of influential experimental conditions including the voltage of power supply, the time of PPy electrodeposition, the extraction temperature, the ionic strength and the extraction time were also investigated. The detection limits of the method under optimized conditions were in the range of 0.002-0.01 ng mL-1. The relative standard deviations (R.S.D.) at a concentration level of 0.1 ng mL-1 were obtained between 7.54 and 11.4% (n = 6). The calibration curves of PAHs showed linearity in the range of 0.01-10 ng mL-1. The proposed method was successfully applied to the extraction of some selected PAHs from real-life water samples and the relative recoveries were higher than 90% for all the analytes

  12. An interior needle electropolymerized pyrrole-based coating for headspace solid-phase dynamic extraction

    Bagheri, Habib [Department of Chemistry, Sharif University of Technology, Azadi Av., P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of)], E-mail: bagheri@sharif.edu; Babanezhad, Esmaeil; Khalilian, Faezeh [Department of Chemistry, Sharif University of Technology, Azadi Av., P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of)

    2009-02-23

    A headspace solid-phase dynamic extraction (HS-SPDE) technique was developed by the use of polypyrrole (PPy) sorbent, electropolymerized inside the surface of a needle, as a possible alternative to solid-phase microextraction (SPME). Thermal desorption was subsequently, employed to transfer the extracted analytes into the injection port of a gas chromatography-mass spectrometry (GC-MS). The PPy sorbent including polypyrrole-dodecyl sulfate (PPy-DS) was deposited on the interior surface of a stainless steel needle from the corresponding aqueous electrolyte by applying a constant deposition potential. The homogeneity and the porous surface structure of the coating were examined using the scanning electron microscopy (SEM). The developed method was applied to the trace level extraction of some polycyclic aromatic hydrocarbons (PAHs) from aqueous sample. In order to enhance the extraction efficiency and increase the partition coefficient of analytes, the stainless steel needle was cooled at 5 deg. C, while the sample solution was kept at 80 deg. C. Optimization of influential experimental conditions including the voltage of power supply, the time of PPy electrodeposition, the extraction temperature, the ionic strength and the extraction time were also investigated. The detection limits of the method under optimized conditions were in the range of 0.002-0.01 ng mL{sup -1}. The relative standard deviations (R.S.D.) at a concentration level of 0.1 ng mL{sup -1} were obtained between 7.54 and 11.4% (n = 6). The calibration curves of PAHs showed linearity in the range of 0.01-10 ng mL{sup -1}. The proposed method was successfully applied to the extraction of some selected PAHs from real-life water samples and the relative recoveries were higher than 90% for all the analytes.

  13. 1,5-Bis(2,5-dimethyl-1H-pyrrol-1-ylnaphthalene

    A. C. Santos

    2009-11-01

    Full Text Available In the title compound, C22H22N2, the asymmetric unit contains one half-molecule. A crystallographic inversion centre is located at the mid-point of the bond common to both rings, in the central naphthalene unit. Quantum-mechanical ab initio calculations on the isolated molecule showed that the minimum energy configuration occurs when the naphthalene ring system and the pyrrolyl groups deviate only slightly from perpendicularity. In the crystal, due to the effects of crystal packing, the molecule deviates by approximately 4° from the a priori expected ideal value of 90° [C—C—N—C torsion angle = 86.11 (15°].

  14. Estimate Secondary Oil Migration Distance Using Pyrrolic Nitrogen Compounds in Petroleum

    Li Maowen

    1997-01-01

    @@ Secondary oil migration represents one of the most important, yet least understood, geological processes responsible for the petroleum accumulation in a sedimentary basin. During secondary migration, petroleum moves updip as high-petroleum saturation rivers driven largely by buoyancy over migration distances ranging from millimeters to hundreds of kilometers. Mass balance calculations indicate that the oil-saturated portions of the carrier bed are in the order of 1%~10% of the carrier bed volume. In most cases, however, the actual dimensions of migration conduits cannot be defined by direct observation,thus preventing useful volumetric estimates of oil charges to structures, or prospect-scale deterministic modeling of secondary migration for predictive purpose.

  15. 5-(4-Methylphenylsulfonyl-1,3-dithiolo[4,5-c]pyrrole-2-thione

    Ning-Juan Zheng

    2012-04-01

    Full Text Available The asymmetric unit of the title compound, C12H9NO2S4, contains one half-molecule with the N, two S amd four C atoms lying on a mirror plane. The molecule exhibits a V-shaped conformation, with a dihedral angle of 87.00 (7° between the benzene and dithiolopyrrole rings. The methyl group was treated as rotationally disordered between two orientations in a 1:1 ratio. In the crystal, weak C—H...O hydrogen bonds link the molecules into chains in [010].

  16. An iterative nonribosomal peptide synthetase assembles the pyrrole-amide antibiotic congocidine in Streptomyces ambofaciens

    Juguet, M.; Lautru, S.; Francou, F.-X.; Nezbedová, Šárka; Leblond, P.; Gondry, M.; Pernodet, J. L.

    2009-01-01

    Roč. 16, č. 4 (2009), s. 421-431. ISSN 1074-5521 Institutional research plan: CEZ:AV0Z50200510 Keywords : ADENYLATION DOMAINS * ESCHERICHIA-COLI * FUNCTIONAL-ANALYSIS Subject RIV: CE - Biochemistry Impact factor: 6.523, year: 2009

  17. 1-Benzyl-6-phenylimino-5-(pyrrol-2-ylidenehexahydropyrimidine-2,4-dione

    Ashot Martirosyan

    2008-02-01

    Full Text Available In the title compound, C21H20N4O2, a potential anti-human immunodeficiency virus type 1 (HIV-1 non-nucleoside reverse transcriptase inhibitor, the pyrrolidine ring adopts an envelope conformation, while the hydrogenated pyrimidine ring adopts a weakly expressed twist conformation. The molecules are connected into infinite chains via N—H...O hydrogen bonds.

  18. 1-Benzyl-6-phenylimino-5-(pyrrol-2-ylidene)hexahydropyrimidine-2,4-dione

    Ashot Martirosyan; Kristine Avagyan; Vahan Martirosyan; Armen Ayvazyan; Rafael Tamazyan

    2008-01-01

    In the title compound, C21H20N4O2, a potential anti-human immunodeficiency virus type 1 (HIV-1) non-nucleoside reverse transcriptase inhibitor, the pyrrolidine ring adopts an envelope conformation, while the hydrogenated pyrimidine ring adopts a weakly expressed twist conformation. The molecules are connected into infinite chains via N—H...O hydrogen bonds.

  19. [Synthesis and bronchodilator action of 4-(methoxycarbonylalkylsulfinyl)-4-pyrrol carboxylic esters].

    Eiden, F; Grusdt, U

    1989-11-01

    The dihydro-dimethoxyfuran carboxylic ester 3 reacts with different mercaptoalkyl carboxylates to give the carbomethoxyalkylthio-tetrahydrofuran carboxylic esters 4. Methanol elimination of 4 yields the dihydrofuran derivatives 5. 4 and 5 can be oxidized to afford the sulfoxides 6 and the sulfones 7, respectively. 4 reacts with primary amines to give the title compounds 8. Derivatives of 8 can be cyclized to afford the thienopyrroles 11 and 12 as well as the thienopyranopyrrole 14. The mercaptopyrrole carboxylic ester 10 is obtained from 8f by elimination of propenic acid. 8e shows bronchodilatoric activity in low concentration. PMID:2624526

  20. 1,2-Bis(1H-pyrrol-2-ylmethylenediazane monohydrate

    Lin Yan

    2009-08-01

    Full Text Available The molecular structure of title compound, C10H10N4·H2O, has an inversion centre located on the mid-point of the N—N bond of the molecule. A twofold rotation axis passes through the water O atom. In the crystal structure, a two-dimensional network is constructed through N—H...O and O—H...N hydrogen bonds.

  1. Technology characterization: liquified natural gas

    None

    1976-12-01

    A technology characterization for liquefied natural gas (LNG) was made. The scope of work was confined to a literature review of LNG processes including natural gas production, liquefaction, and revaporization. The work was divided into five major categories as follows: (1) status of LNG projects, (2) general process description, (3) environmental aspects, (4) safety, and (5) economics. Each of these categories forms a major heading for this report. In addition, an LNG reference system of 250 million standard cubic feet per day (MMSCFD) is included in the report at Argonne National Laboratory's (Argonne) request. Information concerning this system was derived from other LNG systems in the literature. The report does not include an assessment of the market potential for the product gas or its end use. Published cost estimates in the literature have been identified but the original cost estimates have not been provided. Plant layouts, conceptual designs, and socioeconomic analysis are not provided.

  2. Characterizing stellar and exoplanetary environments

    Khodachenko, Maxim

    2015-01-01

    In this book an international group of specialists discusses studies of exoplanets subjected to extreme stellar radiation and plasma conditions. It is shown that such studies will help us to understand how terrestrial planets and their atmospheres, including the early Venus, Earth and Mars, evolved during the host star’s active early phase. The book presents an analysis of findings from Hubble Space Telescope observations of transiting exoplanets, as well as applications of advanced numerical models for characterizing the upper atmosphere structure and stellar environments of exoplanets. The authors also address detections of atoms and molecules in the atmosphere of “hot Jupiters” by NASA’s Spitzer telescope. The observational and theoretical investigations and discoveries presented are both timely and important in the context of the next generation of space telescopes. 
 The book is divided into four main parts, grouping chapters on exoplanet host star radiation and plasma environments, exoplanet u...

  3. Engineered decoherence: Characterization and suppression

    Hegde, Swathi S.; Mahesh, T. S.

    2014-06-01

    Due to omnipresent environmental interferences, quantum coherences inevitably undergo irreversible transformations over certain time scales, thus leading to the loss of encoded information. This process, known as decoherence, has been a major obstacle in realizing efficient quantum information processors. Understanding the mechanism of decoherence is crucial in developing tools to inhibit it. Here we utilize a method proposed by Teklemariam et al. [Phys. Rev. A 67, 062316 (2003), 10.1103/PhysRevA.67.062316] to engineer artificial decoherence in the system qubits by randomly perturbing their surrounding ancilla qubits. Using a two-qubit nuclear magnetic resonance quantum register, we characterize the artificial decoherence by noise spectroscopy and quantum process tomography. Further, we study the efficacy of dynamical decoupling sequences in suppressing the artificial decoherence. Here we describe the experimental results and their comparisons with theoretical simulations.

  4. Molecular characterization of zoogenetics resources

    Full text: A resume of research papers based on gene technology that has been developed during the year 2002 at National University of Colombia campus Palmira on native bovines (Harton del Valle), Native Swine and poultry, Tilapia (Oreochromis spp) and equines, is given below. (1) Bovine Harton del Valle: Colombia possesses the major variety of criolle Bovine of America; one of them, Harton del Valle cattle originated from the cattle brought by the Spanish in the XV century and has adapted to conditions and general environment of Valle del Cauca (Colombia) with high rates of reproduction and survival and low susceptibility to diseases. The 'Harton' inventory has been estimated to be 5000 animals of a total of 24 millions cattle in the country. A resources program was established between the National University of Colombia and Agricultural Secretary (Ministerio de Agricultura) and breeders association (ASOHARTON) and as of 1996 the following research has been conducted: Inventory and characterization of production systems; genetic improvement, crossbreeding and quality characterization of milk, blood and physiological constants and identification of endocrine values. The project has a germoplasm bank in vivo and in vitro. In order to identify the genetic diversity to establish conservation criteria and for breeding criteria, at present genetic variation is being evaluated by RAPD's markers. Allelic variants of k-cassein are being determined and microsatellites characterization has been initiated. The aim in the short terms is to evaluate adaptability characteristics, resistance to diseases and parasites, and in the medium term the selection assisted by markers. (2) Criolle Swine: The actual size of the population is unknown, however it is believed there is close to 1 million which are established in small farm production systems. At present genetic diversity has been characterized by RAPD's markers with the purpose to evaluate genetic distances between three groups

  5. Characterizing and modeling citation dynamics

    Eom, Young-Ho; 10.1371/journal.pone.0024926

    2011-01-01

    Citation distributions are crucial for the analysis and modeling of the activity of scientists. We investigated bibliometric data of papers published in journals of the American Physical Society, searching for the type of function which best describes the observed citation distributions. We used the goodness of fit with Kolmogorov-Smirnov statistics for three classes of functions: log-normal, simple power law and shifted power law. The shifted power law turns out to be the most reliable hypothesis for all citation networks we derived, which correspond to different time spans. We find that citation dynamics is characterized by bursts, usually occurring within a few years since publication of a paper, and the burst size spans several orders of magnitude. We also investigated the microscopic mechanisms for the evolution of citation networks, by proposing a linear preferential attachment with time dependent initial attractiveness. The model successfully reproduces the empirical citation distributions and accounts...

  6. Synthesis and Characterization of Multithiouracils

    WANG Wei; LIU Hui-Min; ZHANG Wei; ZHANG Wen-Qin

    2003-01-01

    @@ Alkylation of bases group of nucleic acid, thymine and uracil, has attracted great attention. In order to investigate the intermolecular interactions, [1,2] and the photoreactions[3,4] between bases group of nucleic acid, many studies were focused on the synthesis of bisbases in the formation of B-(CH2)n-B (B′) in which trimethylene was commonly used as linker. Thiouracil is an important derivative of nucleic acid bases, and it can interfere with the synthesis of thyroxine, especially in the treatment of hyperthyroidism and angina. However, to our knowledge, the synthesis of bisthiouracils, even trithiouracils, using flexible or rigid linkers has not been reported. Herein, we have synthesized eight thiouracil derivatives by nucleophilic reaction between thiouracil and varied bromides. All the compounds have been characterized by IR, 1H NMR and element analysis.

  7. Spatially Characterizing Effective Timber Supply

    Berry, J. K.; Sailor, J.

    1982-01-01

    The structure of a computer-oriented cartographic model for assessing roundwood supply for generation of base load electricity is discussed. The model provides an analytical procedure for coupling spatial information of harvesting economics and owner willingness to sell stumpages. Supply is characterized in terms of standing timber; of accessibility considering various harvesting and hauling factors; and of availability as affected by ownership and residential patterns. Factors governing accessibility to timber include effective harvesting distance to haulic roads as modified by barriers and slopes. Haul distance is expressed in units that take into account the relative ease of travel along various road types to a central processing facility. Areas of accessible timber are grouped into spatial units, termed 'timbersheds', of common access to particular haul road segments that belong to unique 'transport zones'. Timber availability considerations include size of ownership parcels, housing density and excluded areas. The analysis techniques are demonstrated for a cartographic data base in western Massachusetts.

  8. Characterization of DPOAE fine structure

    Reuter, Karen; Hammershøi, Dorte

    has recently been demonstrated to exist in low level equal-loudness contours. The character of the DPOAE fine structure depends on several parameters, i.e., level, frequencies, and frequency of the two primaries, but also level and character of the noise floor. The prevalence and character of the fine......The distortion product otoacoustic emission (DPOAE) fine structure is revealed, when measuring DPOAE with a very fine frequency resolution. It is characterized by consistent maxima and minima with notches of up to 20 dB depth. The fine structure is known also from absolute hearing thresholds, and...... structures are highly individual, and till now no standardized method has been suggested for a consistent categorization. In the present paper a method developed for the categorization of fine structures is presented. The method has been used in two previous studies on the prevalence of fine structures, 1...

  9. Low Coherence Optic Source Characterization

    This work presents the results of characterization of the coherence length of an optic source using interferometric techniques and digital signal processing. Optic sources are not ideal because of random behavior in the emission process and spectral dispersion. Optical coherence is the ability of light to generate interference, either temporal or spatial. In time domain, coherence is expressed by the autocorrelation function. In case of monochromatic laser, it has larger coherence length, in the order of tenths to hundredth of meters, rather than a superluminiscent diode (SLD), which is shorter, in the orders of millimeters. This work presents a method for measuring coherence length using an automated Michelson interferometer and a SLD with central wavelength λ0 = 1302.4 nm and acquisition system.by means of a soundcard in a personal computer

  10. Hydraulic characterization of " Furcraea andina

    Rivera-Velasquez, M. F.; Fallico, C.; Molinari, A.; Santillan, P.; Salazar, M.

    2012-04-01

    The present level of pollution, increasingly involving groundwaters, constitutes a serious risk for environment and human health. Therefore the remediation of saturated and unsaturated soils, removing pollutant materials through innovative and economic bio-remediation techniques is more frequently required. Recent studies on natural fiber development have shown the effectiveness of these fibers for removal of some heavy metals, due to the lignin content in the natural fibers which plays an important role in the adsorption of metal cations (Lee et al., 2004; Troisi et al., 2008; C. Fallico, 2010). In the context of remediation techniques for unsaturated and/or saturated zone, an experimental approach for the hydraulic characterization of the "Furcraea andina" (i.e., Cabuya Blanca) fiber was carried out. This fiber is native to Andean regions and grows easily in wild or cultivated form in the valleys and hillsides of Colombia, Ecuador, and Peru. Fibers of "Furcraea andina" were characterized by experimental tests to determine their hydraulic conductivity or permeability and porosity in order to use this medium for bioremediation of contaminated aquifer exploiting the physical, chemical and microbial capacity of natural fiber in heavy metal adsorption. To evaluate empirically the hydraulic conductivity, laboratory tests were carried out at constant head specifically on the fibers manually extracted. For these tests we used a flow cell (used as permeameter), containing the "Furcraea andina" fibers to be characterized, suitably connected by a tygon pipe to a Marriott's bottle, which had a plastic tube that allow the adjustment of the hydraulic head for different tests to a constant value. By this experiment it was also possible to identify relationships that enable the estimation of permeability as a function of density, i.e. of the compaction degree of the fibers. Our study was carried out for three values of hydraulic head (H), namely 10, 18, and 25 cm and for each

  11. Structural characterization of electrodeposited boron

    Ashish Jain; C Ghosh; T R Ravindran; S Anthonysamy; R Divakar; E Mohandas; G S Gupta

    2013-12-01

    Structural characterization of electrodeposited boron was carried out by using transmission electron microscopy and Raman spectroscopy. Electron diffraction and phase contrast imaging were carried out by using transmission electron microscopy. Phase identification was done based on the analysis of electron diffraction patterns and the power spectrum calculated from the lattice images from thin regions of the sample. Raman spectroscopic examination was carried out to study the nature of bonding and the allotropic form of boron obtained after electrodeposition. The results obtained from transmission electron microscopy showed the presence of nanocrystallites embedded in an amorphous mass of boron. Raman microscopic studies showed that amorphous boron could be converted to its crystalline form at high temperatures.

  12. Photoacoustic characterization of ovarian tissue

    Aguirre, Andres; Gamelin, John; Guo, Puyun; Yan, Shikui; Sanders, Mary; Brewer, Molly; Zhu, Quing

    2009-02-01

    Ovarian cancer has the highest mortality of all gynecologic cancers with a five-year survival rate of only 30%. Because current imaging techniques (ultrasound, CT, MRI, PET) are not capable of detecting ovarian cancer early, most diagnoses occur in later stages (III/IV). Thus many women are not correctly diagnosed until the cancer becomes widely metastatic. On the other hand, while the majority of women with a detectable ultrasound abnormality do not harbor a cancer, they all undergo unnecessary oophorectomy. Hence, new imaging techniques that can provide functional and molecular contrasts are needed for improving the specificity of ovarian cancer detection and characterization. One such technique is photoacoustic imaging, which has great potential to reveal early tumor angiogenesis through intrinsic optical absorption contrast from hemoglobin or extrinsic contrast from conjugated agents binding to appropriate molecular receptors. To better understand the cancer disease process of ovarian tissue using photoacoustic imaging, it is necessary to first characterize the properties of normal ovarian tissue. We have imaged ex-vivo ovarian tissue using a 3D co-registered ultrasound and photoacoustic imaging system. The system is capable of volumetric imaging by means of electronic focusing. Detecting and visualizing small features from multiple viewing angles is possible without the need for any mechanical movement. The results show strong optical absorption from vasculature, especially highly vascularized corpora lutea, and low absorption from follicles. We will present correlation of photoacoustic images from animals with histology. Potential application of this technology would be the noninvasive imaging of the ovaries for screening or diagnostic purposes.

  13. 324 Building Baseline Radiological Characterization

    This report documents the analysis of radiological data collected as part of the characterization study performed in 1998. The study was performed to create a baseline of the radiological conditions in the 324 Building. A total of 85 technical (100 square centimeter (cm2)) smears were collected from the Room 147 hoods, the Shielded Materials Facility (SMF), and the Radiochemical Engineering Cells (REC). Exposure rate readings (window open and window closed) were taken at a distance of 2.5 centimeters (cm) and 30 cm from the surface of each smear. Gross beta-gamma and alpha counts of each smear were also performed. The smear samples were analyzed by gamma energy analysis (GEA). Alpha energy analysis (AEA) and strontium-90 analysis were also performed on selected smears. GEA results for one or more samples reported the presence of manganese-54, cobalt-60, silver-108m antimony-125, cesium-134, cesium-137, europium-154, europium-155, and americium-241. AEA results reported the presence of plutonium-239/240, plutonium-238/241Am, curium-243/244, curium-242, and americium-243. Tables 5 through 9 present a summary by location of the estimated maximum removable and total contamination levels in the Room 147 hoods, the SMF, and the REC. The smear sample survey data and laboratory analytical results are presented in tabular form by sample in Appendix A. The Appendix A tables combine survey data documented in radiological survey reports found in Appendix B and laboratory analytical results reported in the 324 Building Physical and Radiological Characterization Study (Berk, Hill, and Landsman 1998), supplemented by the laboratory analytical results found in Appendix C.

  14. Reservoir characterization using wavelet transforms

    Rivera Vega, Nestor

    Automated detection of geological boundaries and determination of cyclic events controlling deposition can facilitate stratigraphic analysis and reservoir characterization. This study applies the wavelet transformation, a recent advance in signal analysis techniques, to interpret cyclicity, determine its controlling factors, and detect zone boundaries. We tested the cyclostratigraphic assessments using well log and core data from a well in a fluvio-eolian sequence in the Ormskirk Sandstone, Irish Sea. The boundary detection technique was tested using log data from 10 wells in the Apiay field, Colombia. We processed the wavelet coefficients for each zone of the Ormskirk Formation and determined the wavelengths of the strongest cyclicities. Comparing these periodicities with Milankovitch cycles, we found a strong correspondence of the two. This suggests that climate exercised an important control on depositional cyclicity, as had been concluded in previous studies of the Ormskirk Sandstone. The wavelet coefficients from the log data in the Apiay field were combined to form features. These vectors were used in conjunction with pattern recognition techniques to perform detection in 7 boundaries. For the upper two units, the boundary was detected within 10 feet of their actual depth, in 90% of the wells. The mean detection performance in the Apiay field is 50%. We compared our method with other traditional techniques which do not focus on selecting optimal features for boundary identification. Those methods resulted in detection performances of 40% for the uppermost boundary, which lag behind the 90% performance of our method. Automated determination of geologic boundaries will expedite studies, and knowledge of the controlling deposition factors will enhance stratigraphic and reservoir characterization models. We expect that automated boundary detection and cyclicity analysis will prove to be valuable and time-saving methods for establishing correlations and their

  15. Synthesis, characterization and enhanced photoconductivity from a mesoporous titania on dye doping.

    Pal, Nabanita; Paul, Manidipa; Bera, Ashoke; Basak, Durga; Bhaumik, Asim

    2010-07-26

    New wormhole-like mesoporous TiO(2) material has been synthesized through a convenient sol-gel method in the presence of a Schiff base secondary amine hexadecyl-2-pyrrole-methylamine (HPMA) containing chelating donor sites as template or structure directing agent (SDA). SDA molecules can be easily removed from the composite to generate mesoporosity and upon removal of the SDA molecule, this mesoporous TiO(2) material showed very high surface area (480+/-10 m(2)/g) with an average pore diameter of 2.57+/-0.05 nm. When Rose Bengal dye is entrapped inside the nanopores of this material, it showed a drastic enhancement (ca. 40-folds) in the photoconductivity vis-à-vis mesoporous TiO(2) alone under white light illumination. PMID:20638505

  16. THERMOGRAVIMETRIC CHARACTERIZATION OF GLOVEBOX GLOVES

    Korinko, P.

    2012-02-29

    An experimental project was initiated to characterize mass loss when heating different polymer glovebox glove material samples to three elevated temperatures, 90, 120, and 150 C. Samples from ten different polymeric gloves that are being considered for use in the tritium gloveboxes were tested. The intent of the study was to determine the amount of material lost. These data will be used in a subsequent study to characterize the composition of the material lost. One goal of the study was to determine which glove composition would least affect the glovebox atmosphere stripper system. Samples lost most of the mass in the initial 60 minutes of thermal exposure and as expected increasing the temperature increased the mass loss and shortened the time to achieve a steady state loss. The most mass loss was experienced by Jung butyl-Hypalon{reg_sign} at 146 C with 12.9% mass loss followed by Piercan Hypalon{reg_sign} at 144 C with 11.4 % mass loss and Jung butyl-Viton{reg_sign} at 140 C with 5.2% mass loss. The least mass loss was experienced by the Jung Viton{reg_sign} and the Piercan polyurethane. Unlike the permeation testing (1) the vendor and fabrication route influences the amount of gaseous species that is evolved. Additional testing to characterize these products is recommended. Savannah River Site (SRS) has many gloveboxes deployed in the Tritium Facility. These gloveboxes are used to protect the workers and to ensure a suitable environment in which to handle tritium gas products. The gas atmosphere in the gloveboxes is purified using a stripper system. The process gas strippers collect molecules that may have hydrogen or its isotopes attached, e.g., waters of hydration, acids, etc. Recently, sulfur containing compounds were detected in the stripper system and the presence of these compounds accelerates the stripper system's aging process. This accelerated aging requires the strippers to be replaced more often which can impact the facility's schedule and

  17. Characterization of Prototype LSST CCDs

    OCONNOR,P.; FRANK, J.; GEARY, J.C.; GILMORE, D.K.; KOTOV, I.; RADEKA, V.; TAKACS, P.; TYSON, J.A.

    2008-06-23

    The ambitious science goals of the Large Synoptic Survey Telescope (LSST) will be achieved in part by a wide-field imager that will achieve a new level of performance in terms of area, speed, and sensitivity. The instrument performance is dominated by the focal plane sensors, which are now in development. These new-generation sensors will make use of advanced semiconductor technology and will be complemented by a highly integrated electronics package located inside the cryostat. A test laboratory has been set up at Brookhaven National Laboratory (BNL) to characterize prototype sensors and to develop test and assembly techniques for eventual integration of production sensors and electronics into modules that will form the final focal plane. As described in [1], the key requirements for LSST sensors are wideband quantum efficiency (QE) extending beyond lpm in the red, control of point spread function (PSF), and fast readout using multiple amplifiers per chip operated in parallel. In addition, LSST's fast optical system (f71.25) places severe constraints on focal plane flatness. At the chip level this involves packaging techniques to minimize warpage of the silicon die, and at the mosaic level careful assembly and metrology to achieve a high coplanarity of the sensor tiles. In view of the long lead time to develop the needed sensor technology, LSST undertook a study program with several vendors to fabricate and test devices which address the most critical performance features [2]. The remainder of this paper presents key results of this study program. Section 2 summarizes the sensor requirements and the results of design optimization studies, and Section 3 presents the sensor development plan. In Section 4 we describe the test bench at BNL. Section 5 reports measurement results obtained to date oh devices fabricated by several vendors. Section 6 presents a summary of the paper and an outlook for the future work. We present characterization methods and results on

  18. NMR characterization of pituitary tumors

    Twelve patients (5 male, 7 female, mean age 37.9 +- 20) with pituitary tumors were extensively evaluated with NMR imaging using a 1.5K gauss resistive magnet. Saturation recovery (SR), inversion recovery (IR) and spin echo (SE) pulse sequences were used for qualitative characterization of the lesions. T/sub 1/ calculations were also performed for brain and pituitary. Tumor histology and endocrine status were correlated with NMR data. All tumors were large with suprasellar extension (6 with prolactin secretion, 6 without). Pituitary T/sub 1/'s ranged from .2 to .64, the mean T/sub 1/ being longer than that of brain (Brain = .4 +- .04; Pit = .48 +- .14). 3 patients with histological evidence of homogeneous adenomas had long T/sub 1/'s (0.58 +- .05). 3 patients with evidence of recent or old hemorhage into the pituitary had much shorter T/sub 1/'s (0.29 +- .12). There was no relationship between prolactin secretion and T/sub 1/. Qualitative T/sub 1/ and T/sub 2/ information can be obtained by using a combination of SR, IR, and SE images. Using this method in the patients, homogeneous adenomas had similar T/sub 1/'s and longer T/sub 2/'s compared to the brain, while patients with bleeds had shorter T/sub 1/'s and T/sub 2/'s. Image T/sub 1/ characteristics correlated well with the calculated T/sub 1/ values. The range of T/sub 1/ (and potentially T/sub 2/) values which occur in apparently similar lesions are most likely due to anatomical and pathophysiological variations in these lesions. It may be ultimately possible to separate different types of pathological processes based on NMR image T/sub 1/ and T/sub 2/ characteristics after careful comparative studies of NMR and histological data are completed. The combination of calculated T/sub 1/ and T/sub 2/ with image T/sub 1/ and T/sub 2/ information may also be useful in further characterization of lesions

  19. Hydrostructural Characterization of Fracture Networks

    Doe, T. W.; Hermanson, J.

    2007-12-01

    Over the past 30 years, research in underground laboratories for radioactive waste has led to the development of integrated site investigation and modeling methods for fracture networks. These activities began with the Stripa Project in central Sweden from 1977 to 1992 and have continued worldwide. Experiments on the scale of 100- 200 meter blocks have demonstrated the effectiveness of integrating testing during drilling, pressure monitoring, geologic description, flow logging, pressure transient testing, and groundwater chemistry to define fracture network geometries, particularly with respect to the identification of major features, background fractures, and compartmentalization. Major features are those large fractures or fracture zones that control the flow at the scale of interest, and must be simulated as deterministic features. Background fractures are defined stochastically, and provide connectivity between deterministic features. Based on the experience of block-scale investigations, it is possible to develop a clear picture of hydraulic networks using an integrated structural geologic, hydraulic, and hydrochemical approach. Although fracture network characterization requires a good geologic description of fractures and fracture zones from core and image logging, not all geologic features are water-conducting. Identifying water-conducting fractures begins with measurements of flow during drilling and flow logging immediately afterwards to identify significant conducting features. Major flow features must be hydraulically isolated using multiple point piezometer systems, if subsequent investigation methods are to be successful. Once installed, the pressure responses in the piezometers to subsequent drilling provide key information on connectivity and compartmentalization. Generally with three holes are sufficient to develop initial conceptual models of the major, controlling features. Subsequent boreholes test these geometric hypotheses and provide bases

  20. High-G Thermal Characterization Centrifuge

    Federal Laboratory Consortium — High-G testing of thermal components enables improved understanding of operating behavior under military-relevant environments. The High-G Thermal Characterization...