催化动力学光度法测定痕量钼的研究

研究了在氨水介质中钼（Ⅵ）催化过氧化氢氧化噻嗪红Ｒ的褪色反应其动力学条件，建立了一种高灵敏，高选择性测定食品和水中痕量钼（Ⅵ）的新方法，可测定０．０１－１．０μｇ／２５ｍｌ范围内的钼（Ⅵ），方法当敏度为６．４×１０＾－＾１＾０ｇ／ｍｌ。     

痕量铁的催化分光光度法研究

研究了在S2SO4介质中，以1，10－二氮菲为活化剂，铁（Ⅲ）催化过氧化氢氧化甲基橙的褪色反应的动力学条件。建立了测定痕量铁（Ⅲ）的动力学分析法。方法的灵敏度1．78×10－8g·L－1，线性范围0～1．2×10－5g·L-1。用于测定饮用水和湖水中的痕量钱，相对标准差在5％以内，平均回收率97％～106％。     

偶氮胂Ⅲ光度法测定江水中痕量铬

1引言废水中铬（Ⅵ）的外排直接威胁着人们的身体健康,对其监测是非常必要的。目前褪色法测定铬（Ⅵ）有：偶氮氮膦类显色剂（ε=2－3×104L·mol-1·cm－1）;二溴羧基偶氮胂（ε=2×105L·mol-1·cm-1）;本文观察到在硝酸介质中偶氮胂Ⅲ与具有高灵敏褪色反应,ε＝1．9×106L·mol－1·cm－1。此法操作简便,灵敏度高,条件易于控制。此法用于测定江水中痕量铬（Ⅵ）,获得了满意的结果。2实验部分2．1主要试剂和仪器1．0000glLC4［标准溶液,用时再配成0．SIng／L的工作溶液ZO．sg／L的偶氛肿ill溶液。722型分光光度计（上海第三…     

催化光度法测定痕量钼—钼（Ⅵ）—盐酸联氨—橙黄Ⅳ催化光度新体系

基于盐酸介质中，钼（Ⅵ）催化盐酸联氨还原橙黄Ⅳ的反应，建立了动力学分光光度法测定痕量钼的新方法。本法检出限为３．７×１０＾－３μｇ／ｍＬ，测定钼量范围为０．０２５～１．８μｇ／ｍＬ。已将此法用于测定绿豆中的钼及钼酸铅和钼酸钡的溶度积。     

测定电镀废水中痕量Cr(Ⅵ)的高灵敏光度法

利用偶氮胂Ⅲ与Ｃｒ２Ｏ７２ － 的褪色反应, 对含Ｃｒ６ ＋ 电镀废水中痕量铬（ Ⅵ） 进行测定。结果表明, 在硝酸介质中褪色反应具有高的灵敏度, 反应产物的摩尔吸光系数为３ ．９ ×１０６ Ｌ·ｍｏｌ － １ ·ｃｍ － １ 。铬（ Ⅵ） 含量在０ ．０ ～４０ ．０ μｇ／Ｌ 范围内服从比耳定律。 该法用于测定电镀废水中的铬（ Ⅵ） , 得到了满意的结果。     

催化动力学光度法测定痕量铬（Ⅵ）的研究

作发现铬（Ⅵ）在ｐＨ４．７的ＨＡｃ－ＮａＡｃ缓冲溶液中，能催化过氧化氢氧化邻苯二酚紫的褪色反应，研究了影响催化褪色反应速度的最佳条件，建立了测定痕量铬（Ⅵ） 的新方法，方法的检测限为１．２８×１０＾－６ｇ／Ｌ，测定范围为０～３２μｇ／ＬＣｒ（Ⅵ）。本法已用于测定环境水样，钢样以及电镀废水中痕量的铬（Ⅵ）结果令人满意。     

催化动力学法测定痕量钼的研究—盐酸联氨—Mo（Ⅵ）—邻菲罗啉—甲苯胺蓝体系

基于盐酸介质中和邻菲罗啉的存在下，钼催化盐酸联氨还原甲苯妥蓝褪色反应，建立了一种高灵敏，高选择性测定痕量钼的新方法。方法的检出限为７．６９×１０＾－７ｇ／Ｌ，线性范围０－０．１μｇ／２５ｍＬ，成功用于水和豆类中钼的测定。     

二溴对甲基偶氮羧褪色光度法测定铬（Ⅵ）

研究了新显色剂二溴对甲基偶氮羧与Ｃｒ２Ｏ２－的褪色反应。发现它们在硝酸介质中具有高灵敏的褪色反应,Ｃｒ（Ⅵ）量在 ０～１６０μｇ／Ｌ内符合比耳定律．摩尔吸光系数为 １．２ ×１０ ５Ｌ·ｍｏｌ－１·ｃｍ－１。据此建立了一种新的测定Ｃｒ（Ⅵ）的光度法。     

非催化动力学光度法测定铬的研究

研究了在ＨＣｌ介质中，Ｃｒ（Ⅵ）氧化碘离子显色反应的动力学条件，建立了测定Ｃｒ（Ⅵ）的非催化动力学分析法。方法的灵敏度７．２７×１０－７ｇ·Ｌ－１，检测限５．３３×１０－６ｇ·Ｌ－１，测定范围２×１０－５～３×１０－４ｇ·Ｌ－１。用于测定标钢中的铬，测定值与标准值基本一致     

新试剂3，5－二溴－4－偶氮变色酸苯基荧光酮的合成及其应用研究

本文提供了新显色剂３，５－二溴－４－偶氮变色酸苯基荧光酮的合成方法，研究了试剂与铜（Ⅵ）的分光光度性质及反应条件，在盐酸介质中及表面活性剂ＣＴＭＡＢ存在下，试剂与钼（Ⅵ）形成红色胶束配合物，在５４２ｎｍ处有最大吸收，表观摩尔吸光系数为１．６８×１０￣５Ｌ·ｍｏｌ￣－１·Ｌ￣－１，铜（Ⅵ）含量在０～１０μｇ／２５ｍＬ范围内符合比尔定律，大多数常见金属元素的存在不干扰铜的测定，拟定方法用于铜样中微量钼的测定，结果满意。     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

Determination of heats of detonation and influence of components of composite explosives on heats of detonation of high explosives

The heats of detonation of 20 simple high explosives and explosive mixtures were determined by means of an adiabatic detonation calorimeter designed by the authors. The results indicated that the performance of the instrument was reliable and the experimental data were very accurate. For explosive mixtures, there was a linear accumulative relationship between the heats of detonation of the explosive mixture and its components. Accordingly, the heats of detonation of explosive mixtures could be calculated directly from the heats of detonation of simple explosives and the characteristic heats of other components. The experiments showed that the gold or brass shell of the cylindrical charge could be substituted by a thick-walled porcelain shell, which had the advantage of cheapness.

     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。     

Synthesis of phenolic components of Grains of Paradise

Two vanilloids, (5E)-8-(4-hydroxy-3-methoxyphenyl)oct-5-en-4-one (1) and 4-[3-hydroxydecyl]-2-methoxyphenol (2), isolated from the dried seeds of Grains of Paradise (Aframomum melegueta), were synthesized; the latter compound was made as the S-enantiomer and the material derived from the seeds was found to be a 1:1.7 mixture of the R and S isomers. The synthetic route used should allow the preparation of analogs having extended alkyl chains and consequently different lipophilicity, and 3, a homolog of 2, was also prepared.     

恶臭嗅辨实验室建设探讨

针对恶臭测试的环境影响问题,提出了解决的实例方案,并对方案的要点及优缺点进行讨论,此方案在实际操作中具有较好的效果。     

Summary of development of the theory of stability of colloids and thin films

In this review, the research of the author in the field of colloidal systems is summarized. The factors influencing colloidal stability are systematized and analyzed. Examples are presented to illustrate the practical utilization of the theory of stability of colloids and thin films.This review was prepared on the basis of the works of the author, which were awarded the State Premium for 1991 in the field of science and technology, chemistry section.Institute of Physical Chemistry, Russian Academy of Sciences, 117915 Moscow. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 8, pp. 1708–1717, August, 1992.     

Study of hydration of two cements of different strengths

Main hydration products of two cement pastes, i.e. CSH-gel, portlandite (P) (and specific surface S) were studied by static heating, and by SEM, TEM and XRD, as a function of cement strength (C-33 and C-43) hydration time (th) and subsequent hydration in water vapour.Total change in mass on hydration and air drying, M_o, increased with strength of cement paste and with hydration time. Content of water escaping at 110 to 220°C, defined as water bound with low energy, mainly interlayer and hydrate water, was independent on cement strength but its content increased with (th). Content of chemically bound (zeolitic) water in CSH-gel, escaping at 220-400°C, was slightly dependent on strength and increased with (th). It was possibly derived from the dehydroxylation of CSH-gel and AFm phase. Portlandite water, escaping at 400-500°C, was independent on cement strength and was higher on longer hydration. Large P crystals were formed in the weaker cement paste C-33. Smaller crystals were formed in C-43 but they increased with (th). Carbonate formated on contact with air (calcite, vaterite and aragonite), decomposed in cement at 600-700^oC. It was high in pastes C-33(1 month) and C-43(1 month), i.e. 5.7 and 3.3%, respectively; it was less than 1% after 6 hydration months (low sensitivity to carbonation) in agreement with the XRD study showing carbonates in the air dry paste (1month), and its absence on prolonged hydration (6 months) and on acetone treatment. Water vapour treatment of (6 months) pastes or wetting-drying increased this sensitivity.Nanosized P-crystals, detected by TEM, could contribute to the cement strength; carbonate was observed on the rims of gel clusters.This revised version was published online in November 2005 with corrections to the Cover Date.     

解决能源问题的新途径——光解水制氢的研究

面对日益枯竭的能源危机,氢能是一种洁净、最有前景的替代能源。目前在各种制氢的方法中光催化分解水制氢的研究最多,光解水过程中催化剂最关键,本文对利用太阳能光解水的途径、提高光催化反应效率以及光催化剂的开发研究进行了综述。     

黄酮化合物的合成研究进展

黄酮化合物是一类具有多种生物活性的天然产物,其经典的合成方法主要为查耳酮路线和β-丙二酮路线.近年来出现了许多新技术、新方法.本文介绍了2'-羟基查尔酮的氧化关环法、黄烷酮氧化法、改进的Baker-Venkataraman法及其他合成黄酮化合物的方法.