长光路光度法测定中药材中痕量硒

本文研究了用长光路光度法测定痕量硒。在酸性溶液中，Ｓｅ（Ⅳ）催化ＫＣｌＯ３氧化苯肼成偶氮离子，继而与变色酸生成红色偶氮化合物。硒含量在１．０×１０－９～２．０×１０－７ｇ／ｍＬ范围内遵守比尔定律。巯基棉分离后，测定中药材中总硒，获得满意结果。     

Deposition of Layer－by－layer Inorganic－organic Nano－hybrid Ultrathin Films onto SBA－15

Deposition of inorganic-organic nano-hybrid ultrathin films onto mesoporous silicate materials has been proven possible by using layer-by-layer assembly method. In combination with sol-gel method, titania, subsequently dye molecules (or polymer) were successfully fabricated onto the inner wall of SBA-15. Their structures were preliminarily characterized by FTIR and solid-state UV-Vis spectroscopy, thermal analysis, and BET surface area measurements,respectively.     

氧化苯乙烯和氧化二苯乙烯的区域选择性和立体选择性开环

本文报道 NaBH_4-CoCl_2可使氧化苯乙烯类化合物发生区域选择性开环,主要生成β-苯乙醇衍生物。对于氧化二苯乙烯类化合物,由于受到苯环的空间阻碍,使其开环能力减弱,如反式氧化二苯乙烯比顺式异构体更难于开环。     

一种主链含非线性光学活性基团聚合物的合成

把非线性光学(NLO)发色基团引入到聚合物主链中,既可以增大聚合物中NLO基团的含量,从而提高聚合物的宏观NLO系数,又能够提高NLO聚合物的极化稳定性。本文报道一种由酚酞环氧树脂(PPh)与对硝基苯胺(NA)得到的NLO聚合物的合成及其极化松弛。 所用酚酞环氧树脂系自制,环氧值0.427。对硝基苯胺北京化工厂产,分析纯。N,N-二甲基甲酰胺为中国医药公司售品,化学纯,用前减压蒸馏精制,乙醇、丙酮均为北京化工厂生产,分析纯。在氮气保护下将等当量的PPh与NA溶于DMF中于150℃反应6～8小时后,倒     

离子色谱法同时测定水中六种阳离子

研究了用抑制电导离子色谱法一次进样同时测定水中Li^ ,Na^ , NH4^ ,Mg^2 ,Ca^2 的色谱法条件，相对标准偏差小于0．5％，加标回收率在97．5％－104．0％。在水质分析中运用t检验法，比较了用钙、镁离子浓度计算和传统方法测定的总硬度之间是否存在显著性差异。     

Acetic anhydride as a synthetic reagent

Acetic anhydride has been used widely in synthetic organic chemistry, especially in syntheses and transformations of heterocyclic compounds. These utilities are reviewed under the following classification.     

Selective dimerization of α-methylstyrene catalyzed by a solid acid

A novel solid acid prepared from concentrated sulfuric, boric and phosphoric acid is a highly selective catalyst for the dimerization of α-methylstyrene at room temperature to generate 4-methyl-2,4-diphenyl-1-pentene.     

Preparation of ω-tetrahydropyran-2-ylsulfanylalkylmagnesium chlorides: Useful reagents for the synthesis of 1-(ω-mercaptoalkyl)-1,2-dihydrobuckminsterfullerenes (C60)

ω-Tetrahydropyran-2-ylsulfanylalkylmagnesium chlorides are prepared as Grignard reagents containing protected mercaptoalkyl chains, which are useful for the direct introduction of ω-mercaptoalkyl chains to electrophiles. In order to prove the usefulness of these reagents, they were reacted with buckminsterfullerene (C₆₀) to give 1-(ω-mercaptoalkyl)-1,2-dihydrobuck minsterfullerenes after the deprotection of THP group with TFA.     

Separation of salidroside from Rhodiola crenulata by high-speed counter-current chromatography

High-speed counter-current chromatography (HSCCC) was used to purify salidroside from an extract of Rhodiola crenulata with two steps using a two-phase solvent system composed of ethyl acetate-n-butanol-water (1:4:5, v/v) in the first run and chloroform-methanol-isopropanol-water (5:6:1:4) in the second run. The method yielded 21.9 mg of salidroside from 1.216 g of the crude sample at 98% purity determined by HPLC analyses. Identification was performed by 1H NMR, 13C NMR, and MS.