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61.
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A carbon paste electrode modified with chelating resin (ammino-isopropylmercaptan-type cross-linked chelating resins) for the voltammetric determination of gold(III) was characterized by cyclic voltammetry. The gold(III) ion is accumulated on the surface of the modified electrode only by the chelating effect of the modifier in the carbon paste, without application of a potential. After exchange of the medium the accumulated amount of gold(III) is determined by voltammetry in a blank electrolyte solution. The response depends on both the concentration of gold and the accumulation time. For a 5-min preconcentration time, a linear calibration graph was obtained in the range 3 × 10?8-1 × 10?6 M and the detection limit was about 1 × 10?8 M. A combination of chemical and electrochemical renewal allows the use of a single modified electrode in multiple analytical determinations over several days. For ten preconcentration—determination—renewal cycles [2 × 10?7 M Au(III)], the response could be reproduced with 4.7% relative standard deviation. Many parameters such as the composition of the paste and pH influence the response of the measurement. Many other metal ions have no or little effect on the determination of gold. The procedure was applied to the determination of gold in minerals, copper and anode mud, with good results. 相似文献
63.
Highly ordered rod-like large-pore periodic mesoporous organosilica (PMO) was successfully synthesized at low acid concentration with the assistance of inorganic salt using triblock copolymer P123 as a template. The roles of inorganic salt and acidity in the production of highly ordered mesostructure and the morphology control of PMOs were investigated. It was found that the inorganic salt can significantly widen the range of the synthesis parameters to produce highly ordered 2D hexagonal pore structure of p6mm symmetry. However, the uniform rod-like PMOs can only be synthesized in a narrow range of acid and salt concentrations, which were sensitive to induction time. The adsorption of lysozyme on PMO was studied at different pH values in comparison with adsorption on pure silica material under controlled morphology and pore structure. It was found that the adsorption capacity of lysozyme on the PMO was lower than that on pure SBA-15 silica material and the adsorption amounts are larger at pH 9.6 than at 7.0 for both materials. The results show that the electrostatic interaction between lysozyme and PMO/SBA-15 surface is more dominant than the hydrophobic forces and the interaction of neighboring lysozyme molecules also plays an important role. 相似文献
64.
Reactions of two preformed trinuclear W/Cu/S clusters, [A](2)[WS(4)(CuCN)(2)] (1: A = Et(4)N; 2: A = PPh(4)), with different concentrations of acetic acid in MeCN generate two interesting 2D polymeric clusters [Et(4)N](3)[(WS(4)Cu(2))(2)(mu-CN)(3)].2MeCN (3), and [PPh(4)][WS(4)Cu(3)(mu-CN)(2)].MeCN (4), respectively. Compound 4 can also be readily obtained in a high yield from the reaction of 2 with equimolar [Cu(MeCN)(4)]PF(6) in MeCN. These compounds have been characterized by elemental analysis, IR spectra, thermal analysis, and single-crystal X-ray diffraction. An X-ray analysis reveals that compound 3 retains the WS(4)Cu(2) cluster core, which serves as a 3-connecting node to link equivalent nodes via single cyanide bridges, forming an anionic 2D (6,3) net. Compound 4 consists of a T-shaped WS(4)Cu(3) core, which also acts as a 3-connecting node, with links to 3 equivalent clusters either through single or double cyanide bridges, affording a different anionic 2D (6,3) network. The acetic acid induced aggregation of 3 and 4 from the two cluster precursors 1 and 2 suggests that this simple synthetic strategy is likely to be applicable to many related systems. 相似文献
65.
在自制的硅基纤维素-三(3,5-二甲基苯基氨基甲酸酯)高效液相色谱手性固定相上(HPLC-CSP),优化了1-(6'-甲氧基萘)乙醇氢酯基化反应产物-萘普生甲酯手性分离的条件,测定了相应的一系列不对称氢酯基化反应产物的对映体过剩值(e.e.值)。结果表明,在CDMPC-CSP手性柱上用HPLC测定此类不对称催化反应的光学产率,评价催化剂体系的手性选择是一种非常理想的方法。 相似文献
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Electrospray ionization tandem mass spectrometric study of the aconitines in the roots of aconite 总被引:3,自引:0,他引:3
Fragmentation pathways of aconitine-type alkaloids were investigated by electrospray ionization/ion trap multistage tandem mass spectrometry. Low-energy collision-induced dissociation of protonated aconitines follows a dominant first step, the elimination of the C(8)-substituent as acetic acid or fatty acid in MS(2) spectra. Successive losses of 1-4 CH(3)OH molecules, 1-3 H(2)O, CO, benzoic acid, and CH(3) or C(2)H(5) (N-substituents) are all fragmentation pathways observed in MS(3) and MS(4) spectra. By applying knowledge of these fragmentation pathways to the aconitines in the ethanolic extract of aconite roots, all the known aconitines were detected and also 23 unknown aconitine-type alkaloids, in which the lipo-alkaloids containing residues of 15C, 17C and 19C saturated or unsaturated fatty acids were characterized. These odd-carbon-number fatty acid substituents have not been reported previously. 相似文献
68.
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70.
Synthesis of a Photolabeling Probe for the Study of Antiviral Mechanism of Ribavirin 总被引:1,自引:0,他引:1
QiongYouwu XunZHU JinQiaoWAN FanQiQU LingPENG 《中国化学快报》2004,15(8):907-910
Ribavirin has been used in urgency to treat SARS patients recently. In order to study its antiviral mechanism by photolabeling approach, we have synthesized and characterized 5-azido-1-β-D-ribofuranosyl-1,2,4-triazole-3-carboxiamide 1 as a photolabeling probe of ribavirin. The azidotriazole nucleoside showed rapid and clean photochemical reaction, suggesting that 1 is a promising probe to study the antiviral mechanism ofribarivin by photolabeling. 相似文献