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941.
R. A. Alieva S. Z. Gamidov F. M. Chyragov A. A Azizov 《Journal of Analytical Chemistry》2005,60(12):1114-1117
A method is developed for cadmium and zinc preconcentration on a minicolumn packed with a new chelating polymer sorbent. The effects of the test solution pH and volume, the sample matrix composition, the eluent volume, and the sample and eluent flow rates are studied. Zinc and cadmium in the eluate are determined by flame atomic absorption spectrometry. Under optimal conditions, the determined ion recovery is more than 95%. The detection limits (3σ, n = 20) are found to be 15.0 (Cd) and 17.2 (Zn) ng/mL. The developed method is employed for cadmium and zinc determination in samples of seawater and water obtained after oil pumping. 相似文献
942.
An amperometric detector with a small thin mercury film electrode is described. The device demonstrates advantageous operational
characteristics such as small dispersion (D<2) and “memory effect” (me<0.6%), extensive maximum sample frequency (msf −200
samples/h), and high sensitivity. It has been proven useful in flow-injection analysis at a constant potential under hydrodynamic
conditions. 相似文献
943.
Cao B Wakahara T Tsuchiya T Kondo M Maeda Y Aminur Rahman GM Akasaka T Kobayashi K Nagase S Yamamoto K 《Journal of the American Chemical Society》2004,126(30):9164-9165
A new metallofullerene, La2@C78, has been synthesized by DC arc discharge method, isolated by high-performance liquid chromatography, and characterized by laser desorption time-of-flight mass spectrometry, UV-vis-NIR absorption, differential pulse voltammetry, 13C NMR spectroscopy, and theoretical calculations. The La2@C78/CS2 solution is dark violet and presents several characteristic absorption features at 647, 561, 533, and 386 nm, with an onset around 1000 nm. With respect to empty D3-C78, the capability of La2@C78 as an electron acceptor or donor is stronger. Addition of 1,1,2,2-tetrakis(2,4,6-trimethylphenyl)-1,2-disirane to La2@C78 photochemically, as well as thermally, affords bis- and mono-adducts. Theoretical studies and 13C NMR spectroscopic analysis of La2@C78 indicate that it possesses a D3h-C78 cage (78:5). 相似文献
944.
In the course of investigations on equestrian supplemental products for the presence of doping substances, two products were found to contain forbidden substances. As reported earlier a plant extract (Mexican cactus extract) named “Energy 5” contained the anabolic androgenic steroids (AAS) stanozolol, 17β-hydroxy-17α-methyl-5α-androstane-3β-ol (3β,5α-THMT) as well as mestanolone not declared on the label. In the present study, a product called “Super Kalm Paste” was tested. Analysis by gas chromatography - mass spectrometry (GC-MS) revealed that the preparation contained the class I anti-arrhythmics quinine (trade names KinidinTM, Durules) and cinchonine. The samples were prepared according to a sample preparation procedure established for anabolic steroids in nutritional supplements for humans. The sample treatment comprised the extraction and purification of the analytes as well as the chemical conversion with N-methyl-N-trimethylsilyl-trifluoracetamide (MSTFA) to yield the trimethylsilyl (TMS)-derivatives. To verify whether the administration of such products could lead to positive doping tests, a pilot excretion study on “Energy 5” was conducted with two geldings, and urine samples were collected. Gas chromatography - high resolution mass spectrometry (GC-HRMS) after solid phase extraction and mixed derivatisation has demonstrated the presence of the stanozolol metabolite 16β-hydroxy-stanozolol in urine samples after “Energy 5” application. 相似文献
945.
Smectic layer structure of ferroelectric liquid crystal formed between fine polymer fibres 总被引:1,自引:0,他引:1
Hideo Fujikake Takashi Toyooka Takeshi Murashige Hiroto Sato Yoshiki Iino Masahiro Kawakita Hiroshi Kikuchi 《Liquid crystals》2002,29(7):881-887
This paper describes the alignment of ferroelectric liquid crystal (FLC) structures formed between aligned polymer fibres, where the FLC smectic layers are determined by polarising microscopy and X-ray diffraction. The FLC/polymer composite films were formed from a nematic phase FLC/monomer solution using a photopolymerisation-induced phase separation method. It was found that bending of the FLC smectic layers was induced in both the film plane and the cross-sectional plane at the phase transition from smectic A to chiral smectic C of the FLC material. The light transmittance properties of the composite film between crossed polarizers was analysed by light propagation simulation in several optical anisotropic media, based on the evaluated smectic layer model. 相似文献
946.
Soloshonok VA Cai C Yamada T Ueki H Ohfune Y Hruby VJ 《Journal of the American Chemical Society》2005,127(43):15296-15303
This paper describes a systematic study of addition reactions between the chiral Ni(II) complex of the Schiff base of glycine with (S)-o-[N-(N-benzylprolyl)amino]benzophenone and (S)- or (R)-3-[(E)-enoyl]-4-phenyl-1,3-oxazolidin-2-ones as a general and synthetically efficient approach to beta-substituted pyroglutamic acids and relevant compounds. These reactions were shown to occur at room temperature in the presence of nonchelating organic bases and, most notably, with very high (>98% diastereomeric excess (de)) stereoselectivity at both newly formed stereogenic centers. The stereochemical outcome of the reactions was found to be overwhelmingly controlled by the stereochemical preferences of the Michael acceptors, and the chirality of the glycine complex influenced only the reaction rate. Thus, in the reactions of both the (S)-configured Ni(II) complex and the Michael acceptors, the reaction rates were exceptionally high, allowing preparation of the corresponding products with virtually quantitative (>98%) chemical and stereochemical yields. In contrast, reactions of the (S)-configured Ni(II) complex and (R)-configured Michael acceptors proceeded at noticeably lower rates, but the addition products were obtained in high diastereo- and enantiomeric purity. To rationalize the remarkably high and robust stereoselectivity observed in these reactions, we consider an enzyme-substrate-like mode of interaction involving a topographical match or mismatch of two geometric figures. Excellent chemical and stereochemical yields, combined with the simplicity and operational convenience of the experimental procedures, render the present method of immediate use for preparing various beta-substituted pyroglutamic acids and related compounds. 相似文献
947.
Takeshi Takeda Koutaro Arai Hirohisa Shimokawa Akira Tsubouchi 《Tetrahedron letters》2005,46(5):775-778
Cyclopropanes were obtained by the titanocene(II)-promoted reaction of thioacetals with vinyl pivalate. It was also found that vinycyclopropanes were produced by a similar treatment of thioacetals with the titanocene(II) species in the presence of 1,3-dienes. 相似文献
948.
Dusanka Ž. Obadović Anikó Vajda Maya Garić A. Bubnov Vera Hamplová M. Kašpar Katalin Fodor-Csorba 《Journal of Thermal Analysis and Calorimetry》2005,80(2):519-523
Summary Thermal properties of a homologous series of ferroelectric liquid crystals S-(-)-[4-(2-n-alkoxy-propionyloxy)]biphenyl-4'-[n-alkoxy-(3,5-dimethyl)]benzoate have been investigated by polarizing optical microscopy and differential scanning calorimetry.
The mesophases were identified and confirmed by X-ray too. Three binary mixtures were prepared from the individual homologues.
In one of the mixtures (Mix1), the ferroelectric SmC* phase has broadened and became enantiotropic. This mesophase remained
monotropic in the other two mixtures (Mix2, Mix3). The chiral nematic N* phase did not appear in Mix1, but remained monotropic
for the other two mixtures. Two molecular parameters, the layer spacing and the average intermolecular distance have been
calculated from the X-ray results for the homologues and their mixtures. An intercalated tail-to-tail packing of molecules
was found both in the single compounds and their mixtures resulting in the layer spacing about half of the molecular length
of the single compounds. 相似文献
949.
Miniaturizing all dimensions of apparatus, such as electronics and computers, is the current trend followed by scientists
in various fields. The idea of Lab-on-a-Chip has significantly expanded and found its broad applications in analytical chemistry.
Microplasmas can act as a sample excitation source and are the miniaturized versions of full-sized plasmas. These can be created
in various forms, such as direct current, microwave induced, capacitively coupled and inductively coupled plasmas. Scaling
down the size would reduce the amount of gases, liquids and consumables required, as well as the sample analysis time, which
in turn would decrease the operating costs. Therefore, several research groups are involved in the development of microplasmas
for utilisation in analytical instruments. 相似文献
950.
Yoko Nambu Takeshi Endo Makoto Okawara 《Journal of polymer science. Part A, Polymer chemistry》1981,19(8):1937-1943
Reductive S-monoacylation of lipoamide with some carboxylic acids and tri-n-butylphosphine was carried out in acetonitrile to obtain the corresponding S-monoacylated compounds in excellent yield. This method was applied to the preparation of S-monoacylated dihydrolipoyl polymer with a neighboring thiol group. The acyl transfer from the polymer to cyclohexylamine was enhanced as much as 64 times by adding silver perchlorate. 相似文献