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。     

氟化钙增敏石墨炉原子吸收法测定人发和血清样品中痕量钼的研究

石墨炉原子吸收法测定生物样品中痕量钼时，用氟化钙作基体改进剂，可使钼的原子吸光度提高５．７倍，其特征量原来的４．２× １０＾－１１ｇ／１％吸收降低到５．１×１０＾－１２ｇ／１％吸收，测定下限为０．５５ｎｇ·ｍＬ＾－１，线性范围为０～１０００ｎｇ· ｍＬ＾－１． 对人发和牛血清标样中痕量钼测定。结果满意。     

血清中锂的原子吸收法测定

对血清中锂的火焰原子吸收分光光度分析法（ＦＡＡＳ）进行了研究，发现血清在０．２４ｍｏｌ／ＬＨＮＯ３介质中，用３０００×１０－６Ａｌ３＋作为碱土金属干扰的抑制剂，用ＦＡＡＳ法测定血清理，其回收率和精密度都很好，分别为１０４．７％和２．８％．本法１％吸收的灵敏度为０．０３３μｇ／ｍＬ。采用本法对服用碳酸锂治疗苯中毒的患者血清中锂进行了测定，其含量在０．７５～４．６４μｇ／ｍＬ之间，结果令人满意。     

流动注射示差动力学化学发光法测定微量硅

根据硅钼杂多酸氧化Ｌｕｍｉｎｏｌ产生化学发光的性质，以及硅钼杂多酸与磷钼杂多酸形成速度的差异，采用停流技术，在硅磷共存时，不经分离，实现了对和钢样中硅的选择性测定。该法检出限为２．０×１０＾－８ｇ／ｍＬ，线性范围１．０×１０＾－７－１．０×１０＾－５ｇ／ｍＬ，相对标准偏差为２．８％。     

磷的光化学分析新方法研究

在０．２ｍｏｌ／ＬＨ２ＳＯ４－１０％乙醇介质中及紫外光照射条件下磷钼杂我酸光还原为磷钼蓝，据此建立了一个测定０．０５－２．０μｇ／ｍｌ的光化学分析新方法，并用于度样分析，探讨了光化学反应机理。     

GFAAS法测定天然饮用矿泉水中的钼

本文介绍了石墨炉原子吸收光谱法测定天然饮用矿泉水中的钼。水样不需浓缩萃取直接测定。线性范围０．０２～１．６ｎｇ，检测限０．０１ｎｇ，相对标准偏差２．３％－４．５％，回收率９６％－１０３％。     

硅钼黄—乙醇体系光化学还原硅钼蓝分光光度法测定硅

含０．８－２．０ｍｏｌ／Ｌ ＨＣｌ的硅钼黄－乙醇溶液体系在波长小于４６０ｎｍ的蓝紫光或紫外照射下，能够发生使硅钼黄定量还原为硅钼蓝的光化学反应。基于这一反应，研究建立了测试样品中硅含量的光化学还原硅钼蓝分光光度法。该法与化学还原硅钼蓝法相比，避免了因加入化学还原剂引起的干扰，重显性好，准确度高，操作简便，快速，测定结果的标准偏差≤０．０１２％，相对标准偏差≤１％。     

流动注射速差动力学化学发光分析Ⅱ微量磷的快速测定

本文根据磷钼杂多酸可直接氧化Ｌｕｍｉｎｏｌ产生化学发光的特性，建立了磷的流动注射化学发光分析方法。利用磷钼杂多酸、硅钼杂多酸、砷钼杂多酸形成速率的差异，在磷、硅、砷共存时，可不经任何分离，实现对水样和钢样中磷的快速测定。该法检出限为３．６×１０－５ｇ／Ｌ，线性范围２．０×１０－４～１．０×１０－２ｇ／Ｌ，相对标准偏差为１．８％（磷浓度１．０×１０－３ｇ／Ｌ；ｎ＝１１次）。采样频率４５样／ｈ。     

动力学—两次标准加入法同时测定钼和钨

本文提出了动力学－两次标准加入法双组份同时测定的新方法，讨论了测定的基本原理；用停流ＦＩＡ光度法研究了钼和钨共同催化的Ｈ２Ｏ２－Ｉ＾－动力学反应体系，并建立了钼和钨同时测定的条件，用本法测定了钢样和模拟样品中的钼、钨含量，结果满意，钼和钨的回收率分别为９７％－１０２．６％和９８．２％－１０３％；相对标准偏差分别为２．８％－３．２％和２．１％－３．５％。     

新催化光度法测定痕量钱

基于Ｍｏ对过氧化氢氧化铍试剂Ⅱ褪色反应的反催化效应及动力学条件，建立了测定钼的新催化光度法，Ｍｏ的线性范围为２－３６μｇ．Ｌ＾－１，检出下限达１．０μｇ．Ｌ＾－１。用于土壤，茶叶，花生和豆类食品中钼的测定，回收率为９６．７％－１０５％之间。     

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.     

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。     

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.

     

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.     

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.     

氯氧化镁生成热的研究

用氧化镁氯化镁水溶液制备了8水合氯氧化镁[nMg(OH)2·MgCl2·8H2O], 并测定了其在盐酸中的溶解热, 实验结果表明, 氯氧化镁溶解热与n值呈线性关系, 根据溶解热求出5Mg(OH)2·MgCl2·8H2O和3Mg(OH)2·MgCl2·8H2O的生成热分别为-7727.1和5888.1kJ·mol^1^-。     

Thermodynamics of the formation of oxosulfides of rare-earth elements

The enthalpies of solution of several oxosulfides of rare-earth elements and the high-temperature enthalpies of oxosulfides and oxosulfates of lanthanum and yttrium were measured using solution calorimetry and high-temperature microcalorimetry techniques. Standard enthalpies of formation and some thermodynamic properties of oxosulfides and oxosulfates were calculated. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2 pp. 294–297, February, 1997.     

探究“铁的锈蚀条件”实验创新设计

设计了铁的锈蚀实验,说明了铁钉的处理方法,增加了温度、酸、碱的影响条件,实现了铁跟蒸馏水及空气中氧气快速反应而生锈,使实验在5 min左右就能够得到准确的结果。