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51.
Frank J. Quaeyhaegens Herman O. Desseyn Spiros P. Perlepes John C. Plakatouras Ben Bracke Albert T. H. Lenstra 《Transition Metal Chemistry》1991,16(1):92-101
Summary The synthesis of the NiII, PdII and CuII complexes of N, N-bis(aminoalkyl)oxamides (LH2) is described and structures are proposed on the basis of their physical and spectroscopic properties. With NiII and PdII only one complex is formed with general formula NiL or PdL, characterised by coordination through two deprotonated amide N-atoms and two terminal NH2 groups. With CuII it proved possible to obtain three structurally different compounds, depending on the pH, with general formulae Cu(LH2)X2, Cu2(L)X2 and CuL in which X=Cl, Br or NO3. The structure of [Cu2(C8O2N4H16](NO3)2 was solved by means ofx-ray diffraction; Mr=451.33, monoclinic, space group P21/n, a=9.503(4), b=7.614(1), c=10.407(3) Å, =98.43(3)°, V=744.3(7)Å3, Z=2, Dx=1.202 g cm–3, =1.33 cm–1, (MoK)=0.71073 Å, F(000)=520, room temperature, R=0.043, wR=0.047 for 1080 observed [I>-3(I)] not systematically absent reflections out of 1423 measurements and 137 variables. The compound has a conformational chair/boat disorder with 82% in the more stable chair form. 相似文献
52.
Salah Hassoon 《Analytica chimica acta》2004,512(1):125-132
Ultrasound-based water treatment is often applied for degradation of stable organic pollutants, such as polycyclic aromatic hydrocarbons and halogenated compounds. Monitoring the degradation process, during the application of ultrasound radiation, is of considerable economical interest. In this work, the possibility of performing on-line spectral analysis during sonication was examined and it was found that direct absorption or fluorescence readings are misleading. Optical monitoring is strongly affected by the absorption and scattering of light by cavitation micro-bubbles and ultrasound induced particulates. A model was developed to account for these effects and to allow for on-line fluorescence analysis. The model takes into account the absorption and scattering coefficients of the micro-bubbles and particulates, as well as their time dependent concentration. The model parameters are found from independent measurements where the pollutants are added to already sonicated pure water. Then, the model is tested for predicting the actual fluorescence behavior during the sonication process. It has been shown that the model allows for recovery of the true degradation data, as obtained by off-line HPLC measurements. 相似文献
53.
The open-circuit potential drop of an oxidatively pretreated nickel electrode in 0.1 M NaOH was used to develop a technique for the determination of alcohols, amino acids, carbohydrates, etc., in aqueous solution. The electrode pretreatment consisted of the formation of nickel hydrated oxides on the electrode surface with an oxidation state > 2. Both electrochemical and chemical pre-oxidation of the electrode surface were examined. The analytical signal was the enhancement of the potential drop corresponding to analyte concentration. The analytical signal was linearly related to the logarithm of the analyte concentration. The limits of determination ranged from 1 mM for low-molecular-weight to 0.02 mM for alkyl polyether alcohols. The flow-injection technique allows convenient pretreatment and direct observation of the analytical signal. Interferences from chloride and calcium can be readily eliminated by excluding them during electrode pretreatment. Potentiometric measurements were correlated with amperometric anodic responses at the nickel oxide electrode, allowing an unusual direct comparison of the two methods. 相似文献
54.
The interfering effects of various foreign ions on the determination of arsenic were studied by hydride generation inductively coupled plasma atomic emission spectrometry (HG-ICP-AES). There were serious inhibiting interferences by Cu, Pb, Co, Au, Pd and Ni. However, by using cyanide as a complexing agent these interferences could be completely eliminated over a wide range of interferent concentration. The optimum chemical parameters for continuous arsine generation were studied. A major advantage of this technique is that it only needs low acid concentrations and produces less hazardous waste. Sensivity, selectivity and accuracy of the determination of arsenic by HG-ICP-AES were investigated. The detection limit (in 1 mol/l HCl medium) for arsenic(III) was 0.82 ng/ml. The relative standard deviation for ten determinations of a solution containing 50 ng/ml arsenic was 1.3%. 相似文献
55.
Small amounts of papaverine (about 3 mg in 15 ml solution) can be determined heterometrically in the presence of thiocyanate by titration with cobaltous solution. A strong electrolyte (Na2SO4) must be added to obtain a clear endpoint. The titration can be carried out in the presence of large amounts (97%) of quinine and ephedrine. The titration takes 2–3 min and the error rarely exceeds 1%.Papaverine, quinine, and ephedrine can be determined individually by spectrophotometry as their cobaltothiocyanates, which are extracted in 30% cyclohexanone in carbon tetrachloride, and the optical density measured at 625 nm. The method is reproducible at milligram levels with a standard deviation of ±0.3% for papaverine and quinine and = 0.5% for ephedrine. 相似文献
56.
Hou Y Jaffrezic-Renault N Martelet C Tlili C Zhang A Pernollet JC Briand L Gomila G Errachid A Samitier J Salvagnac L Torbiéro B Temple-Boyer P 《Langmuir : the ACS journal of surfaces and colloids》2005,21(9):4058-4065
To make ultrathin films for the fabrication of artificial olfactory systems, odorant biosensors, we have investigated mixed Langmuir and Langmuir-Blodgett films of odorant-binding protein/amphiphile. Under optimized experimental conditions (phosphate buffer solution, pH 7.5, OBP-1F concentration of 4 mg L(-1), target pressure 35 mN m(-1)), the mixed monolayer at the air/water interface is very stable and has been efficiently transferred onto gold supports, which were previously functionalized by self-assembled monolayers (SAMs) with 1-octadecanethiol (ODT). Atomic force microscopy and electrochemical impedance spectroscopy were used to characterize mixed Langmuir-Blodgett (LB) films before and after contact with a specific odorant molecule, isoamyl acetate. AFM phase images show a higher contrast after contact with the odorant molecule due to the new structure of the OBP-1F/ODA LB film. Non-Faradaic electrochemical spectroscopy (EIS) is used to quantify the effect of the odorant based on the electrical properties of the OBP-1F/ODA LB film, as its resistance strongly decreases from 1.18 MOmega (before contact) to 25 kOmega (after contact). 相似文献
57.
The precipitation of calcium oxalate monohydrate (COM) was monitored at a Langmuir monolayer containing lipid raft domains. The raft-forming monolayer consists of a 2:1:1 mixture of 1-palmitoyl-2-oleoyl-sn-glycero-3-phosphocholine/sphingomyelin/dihydrocholesterol, where the raft liquid ordered phase is enriched in sphingomyelin and the sterol. COM crystals, monitored by Brewster angle microscopy, appear at the phase boundary between the raft domains and the expanded phase. 相似文献
58.
K. Ardhaoui J. Rogez A. Ben Chérifa M. Jemal P. Satre 《Journal of Thermal Analysis and Calorimetry》2006,86(2):553-559
Lanthanum-bearing silicate-oxyapatites or britholites, Ca10–xLax(PO4)6–x(SiO4)xO with 1≤x≤6, have been synthesized by solid state reaction
at high temperature. They were characterized by X-ray diffraction and IR spectroscopy.
Using two microcalorimeters, the heat of solution of these compounds have
been measured at 298 K in a solution of nitric and hydrofluoric acid. A strained
least squares method was applied to the experimental results to obtain the
solution enthalpies at infinite dilution, and the mixing enthalpy in two steps.
In the first step the mixing enthalpy obtained is referenced to the britholite
monosubstituted and to the oxysilicate. The mixing enthalpy referenced to
the oxyapatite and to the oxysilicate is then extrapolated. In order to determine
the enthalpies of formation of all the terms of the solution, thermochemical
cycles were proposed and complementary experiments were performed. The results
obtained show a decrease of the enthalpy of formation with the amount of Si
and La introduced in the lattice. This was explained by the difference in
the bond energies of (Ca–O, P–O) and (La–O, Si–O). 相似文献
59.
Baurin N Aboul-Ela F Barril X Davis B Drysdale M Dymock B Finch H Fromont C Richardson C Simmonite H Hubbard RE 《Journal of chemical information and computer sciences》2004,44(6):2157-2166
We have designed four generations of a low molecular weight fragment library for use in NMR-based screening against protein targets. The library initially contained 723 fragments which were selected manually from the Available Chemicals Directory. A series of in silico filters and property calculations were developed to automate the selection process, allowing a larger database of 1.79 M available compounds to be searched for a further 357 compounds that were added to the library. A kinase binding pharmacophore was then derived to select 174 kinase-focused fragments. Finally, an additional 61 fragments were selected to increase the number of different pharmacophores represented within the library. All of the fragments added to the library passed quality checks to ensure they were suitable for the screening protocol, with appropriate solubility, purity, chemical stability, and unambiguous NMR spectrum. The successive generations of libraries have been characterized through analysis of structural properties (molecular weight, lipophilicity, polar surface area, number of rotatable bonds, and hydrogen-bonding potential) and by analyzing their pharmacophoric complexity. These calculations have been used to compare the fragment libraries with a drug-like reference set of compounds and a set of molecules that bind to protein active sites. In addition, an analysis of the overall results of screening the library against the ATP binding site of two protein targets (HSP90 and CDK2) reveals different patterns of fragment binding, demonstrating that the approach can find selective compounds that discriminate between related binding sites. 相似文献
60.
Hydrazidoyl halides were condensed with 2-mercaptobenzimidazole yielding 4a-c and 7a,b which were cyclized to the corresponding 2-arylhydrazonothiazolo[3,2-a]benzimidazol-3-ones 5a,b and 3-substituted 2-arylazo thiazolo[3,2-a]benzimidazoles 8a,b respectively. Imidazo[2,1-b]thiazoles were obtained by the reaction of hydrazidoyl halides with 2-mercapto-4,5-dihydroimidazole. Also, hydrazidoyl halides 6a,b were reacted with 3-amino-4-mercapto-5-phenylpyrazole to give pyrazolo[4,3-b]thiazines 15a,b . The structures of the products were assigned on the basis of their elemental analysis and spectral data. 相似文献