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951.
Uyguner CS Hellriegel C Otto W Larive CK 《Analytical and bioanalytical chemistry》2004,378(6):1579-1586
Humic substances are precursors of carcinogenic trihalomethanes (THMs) formed during disinfection by chlorination in water treatment processes. In an effort to understand the relationship between trihalomethane formation potential (THMFP) and physicochemical properties of humic substances, UV-visible absorbance, fluorescence in emission and synchronous scan modes, and NMR spectra were measured for several aquatic fulvic and humic acids. For comparison, a soil fulvic acid was also examined using these methods. The feasibility of the gradient modified spin-echo (GOSE) NMR experiment to selectively measure singlet resonances arising from isolated protons was examined. In addition, diffusion coefficients were measured for DMSO solutions of the fulvic acids using BPPLED and GOSE-edited pulse sequences. Although none of the methods tested produced results that correlated with THMFP, the GOSE intensities determined for different regions of the NMR spectra did reflect the relative abundance of different types of functional groups produced by lignin oxidation. In addition, the GOSE-edited diffusion results suggest that the isolated protons, those most reactive to chlorination, are more likely contained in the larger molecular weight fractions of fulvic acids. 相似文献
952.
M. Lj. Mihailovi J. Forek Lj. Lorenc Z. Maksimovic H. Fuhrer J. Kalvoda 《Helvetica chimica acta》1969,52(2):459-478
Treatment of 3-oxo-4, 5-oxido steroids with lead tetraacetate results in acetoxylation in the 2α-position as could be shown by independent synthesis of the acetoxylated compounds. The products of this reaction rearrange even under very mild conditions (chromatography on silicagel or alumina) to the corresponding 2,3-dioxo-Δ4 compounds. The influence of structure and conformation of the various intermediates on their NMR.-spectra is discussed. A mechanism for this new transformation is proposed. 相似文献
953.
F. Sauter J. Fröhlich A. Z. M. S. Chowdhury C. Hametner 《Monatshefte für Chemie / Chemical Monthly》1997,128(5):503-508
Summary A variety of partly novel tri- and tetracyclic hetero systems were obtained by reaction of heteroaromatic 2-aminoesters with 2-(methylthio)-2-thiazoline, yielding double-annelation of a thiazolo[2,3-b]pyrimido moiety in a one-pot process.On leave from University of Chittagong, Bangladesh 相似文献
954.
A sensitive flotation—spectrophotometric method, based on the ion associate formed by the anionic thiocyanate complex of osmium with the basic dye methylene blue (MB) is described. The ion associate precipitates when the aqueous solution is shaken with toluene, and the separated and washed compound is dissolved in acetone. The molar absorptivity is 2.2 × 105 l mol-1 cm-1 at 655 nm. Beer's law is obeyed. The molar ratio of Os:SCN:MB in the separated and washed ion associate is 1:6:3. Ruthenium reacts similarly. The method is applied to the determination of traces of osmium in crucible platinum after separation of osmium by distillation as tetroxide. 相似文献
955.
A new, fast and simple inorganic chemiluminescence method for the determination of trace amounts of manganese is described. When MnO(-)(4) is injected into 0.40M Na(2)CO(3)-0.70M KOH mixed solution in a reaction cell, the strong chemiluminescence occurs and is recorded. The detection limit is 0.1 ppb Mn and the linear range extends from 0.1 to 10 ppb Mn. A 5-ppb Mn concentration can be determined with a relative standard deviation of 5.6% (15 replicates). The commonly encountered cations do not interfere with the determinations. This method has been successfully applied to the direct determination of manganese in bauxite. The reaction mechanism is also briefly discussed. 相似文献
956.
[reaction: see text] A new nonchain 5-endo radical cyclization starting with xanthates was exploited in a short synthesis of (+/-)-alpha-lycorane and the erythrina ring system. 相似文献
957.
Methyl-5-benzoyl-2-benzimidazole carbamate (mebendazole) is a drug used as an anthelmintic. A high performance liquid chromatography method has been developed in this study to determine mebendazole and its degradation product in the pharmaceutical dosage forms (tablets and suspension). The expected major degradation product of mebendazole in the dosage forms has been prepared, and identified as 2-amino-5-benzoylbenzimidazole. The proposed HPLC assay was found to be selective, accurate (% recoveries were in the range of 99.9-100.9) for both, mebendazole and the degradation product, repeatable and reproducible (replicate measurements for short and long term measurements showed % RSD of =1.4). The methodology could be considered as a stability indicating method for mebendazole in pharmaceutical dosage forms. 相似文献
958.
M.Z. Kassaee S.M. Musavi M. Ghambarian M.R. Khalili Zanjani 《Journal of organometallic chemistry》2006,691(13):2933-2944
For 30 C2GeHX germylenic isomers, one cyclic structure, X-germacyclopropenylidene, and three acyclics are considered, which include: ethynyl-X-germylene, X-vinylidenegermylene, and (X-ethynyl)germylene (X = H, F, Cl, and Br). The global minimum among six isomeric C2GeH2 (where X = H), is found to be cyclic, aromatic, singlet germacyclopropenylidene. In contrast, among the 24 corresponding halogermylenes, C2GeHX (where X = F, Cl, and Br), the global minima switch to acyclic, singlet ethynylhalogermylenes, at eight reasonably high ab initio and DFT levels. The direct resonance interaction between X and the divalent center Ge in the singlet acyclic ethynylhalogermylene structures, is claimed to justify switching of the calculated global minima in the halo derivatives. GIAO-NICS calculations indicate that the X-germacyclopropenylidene isomer is more aromatic for X = H than X = F, Cl, or Br. The angle ∠XGeC bending potential energy curves show the singlet and triplet ethynylgermylene crossing at ≈146°, for X = H. 相似文献
959.
Taha EA 《Analytical and bioanalytical chemistry》2003,376(7):1131-1136
Two simple and sensitive kinetic methods for the determination of dothiepin hydrochloride are described. The first method is based on kinetic investigation of the oxidation reaction of the drug with alkaline potassium permanganate at room temperature for a fixed time of 25 min. The absorbance of the colored manganate ions is measured at 610 nm. The second method is based on the reaction of dothiepin hydrochloride with 4-chloro-7-nitrobenzofurazan (NBD-Cl) in the presence of 0.1 mol L–1 sodium bicarbonate. Spectrophotometric measurement was achieved by recording the absorbance at 470 nm for a fixed time of 60 min. All variables affecting the development of the color were investigated and the conditions were optimized. Plots of absorbance against concentration in both procedures were rectilinear over the ranges 4–24 and 50–250 g mL–1, with mean recoveries 99.33±0.42 and 99.88±0.53, respectively. The proposed methods were successfully applied for the determination of dothiepin hydrochloride in bulk powder and in capsule dosage form. The results obtained were found to agree statistically with those given by the non-aqueous B.P. method. Furthermore the methods were validated according to USP guidelines and also assessed by applying the standard addition technique. The determination of dothiepin hydrochloride by the fixed concentration method is feasible with the calibration equations obtained, but the fixed time method proves to be more applicable. 相似文献
960.
Identification of selenium species in urine by ion-pairing HPLC–ICP–MS using laboratory-synthesized standards 总被引:1,自引:0,他引:1
Wrobel K Wrobel K Kannamkumarath SS Caruso JA 《Analytical and bioanalytical chemistry》2003,377(4):670-674
This study focused on the detection/identification of possible selenium metabolites in human urine. Organoselenium compounds not commercially unavailable were synthesized and characterized by electrospray mass spectrometry. Separation of selenomethionine, methylselenomethionine, trimethylselonium, selenoethionine, and selenoadenosylmethionine was achieved by ion-pairing HPLC with a mobile phase of 2 mmol L–1 hexanesulfonic acid, 0.4% acetic acid, 0.2% triethanolamine (pH 2.5), and 5% methanol. The column effluent was introduced on-line to inductively coupled plasma–mass spectrometry for selenium-specific detection (77Se and 78Se). For selenium speciation in urine, solid-phase extraction was carried out using C18 cartridges modified with hexanesulfonic acid. Selective retention of cationic species was observed from acidified urine (perchloric acid, pH 2.0). After elution with methanol, evaporation, and dissolution in the mobile phase, the sample was introduced to the HPLC–ICP–MS system and the chromatographic peaks were assigned by adding standards. The species identified in urine were selenomethionine, trimethylselonium ion, and selenoadenosylmethionine. The last species was detected for the first time and our results suggest that selenomethionine might enter the metabolic pathway of its sulfur analog in the activated methylation cycle.Kazimierz Wrobel and Katarzyna Wrobel are on the leave from the Institute of Scientific Research, University of Guanajuato, L. de Retana No. 5, 36000 Guanajuato, Gto., Mexico 相似文献