催化反应—导数示波极谱法测定痕量钨

在盐酸介质中，痕量钨对钛（Ⅲ）还原金莲花橙的缓慢反应有强烈催化作用，在ＮａＯＨ介质莲花橙Ｏ于－０．５０Ｖｖｓ．ＳＣＥ产生一灵敏的导数示波极谱波。据此，建立了一定检测限和测定范围分别为０．８ｎｇ／ｍＬ和１．６－８０ｍｇ／ｍＬＷ的催化反应－示波极谱新方法，用于钢和矿样中钨的测定，获得满意结果。     

催化动力学极谱法测定痕量钼

在稀Ｈ２ＳＯ４介质中，钼（Ⅵ）对硫酸联氨还原乙基橙的反应有强烈的催化作用。建立了催化动力学极谱法测定痕量钼的新体系，方法线性范围为２０－３００ｎｇ／ｍＬ，检出限为３．５４ｎｇ／ｍＬ。方法应用于尿中中钼的测定，结果满意。     

微分吸附计时电位法测定粮食中痕量钼

本文提出一种测定痕量钼的微分吸附计时电位法，利用悬汞电极作为工作电极，在０．１２ｍｏｌ／ＬＨＡｃ－０．０１ｍｏｌ／Ｌ，ＮａＡｃ－３．２×１０＾－６ｍｏｌ／Ｌ茜素红的最佳底液中，测定钼的线性范围为０．４ｎｇ／ｍＬ～７０ｎｇ／ｍＬ，吸附富集３ｍｉｎ检测下限可达０．１ｎｇ／ｍＬ。探讨了影响方法灵敏度的主要因素，初步研究了电极过程，利用该方法直接测定了粮食样品中钼的含量。     

催化动力学极谱法测定痕量钯的研究

研究了催化动力学极谱法测定痕量钯的方法，在盐酸介质中，钯催化次磷酸钠与钼酸铵反应生成磷钼蓝，用氨－氯化铵缓冲液调节溶液ｐＨ值为９．２６可抑制催化反应条件，并在单扫描示波极谱仪上于－１．２４Ｖ（ｖｓ．ＳＣＥ）产生一灵敏极谱波，导数波高与钯０．０５～１．０ｎｇ．ｍｌ＾－１呈线性关系，检出限为０．０３ｎｇ．ｍｌ＾－１，研究了极谱波性质及机理，证明其为吸附波，方法用于合成样及电镀废液中的钯测定，结果满意。     

钴(Ⅱ)-β-巯基丙酸-NaNO_2体系的极谱催化波研究

在ｐＨ３．８的Ｈ２ＳＯ４－ＮＨ４Ａｃ介质中，Ｃｏ（Ⅱ）－β－巯基丙酸（ＭＰＡ）－ＮａＮＯ２体系产生－灵敏的极谱催化波，峰电位在－０．８４Ｖ（ｖｓ．ＳＣＥ），钴浓度在０．０２～１００ｎｇ／ｍＬ范围内与峰电流呈线性关系。检出限为０．０１ｎｇ／ｍＬ。本文对极谱波的性质和机理进行了初步探讨。本法用于土壤中总钴和有效钴的测定，结果满意。     

钴（Ⅱ）—β—巯基丙酸—NaNO2体系的极谱化波研究

在ｐＨ３．８的Ｈ２ＳＯ４－ＮＨ４Ａｃ介质中，Ｃｏ（Ⅱ）－β－巯基丙酸（ＭＰＡ）－ＮａＮＯ２体系产生－灵敏的极谱催化波，峰电位在－０．８４Ｖ（ｖｓ．ＳＣＥ）钴浓度在０．０２～１００ｎｇ／ｍＬ范围内与峰电流呈线性关系，检出限为０．０１ｎｇ／ｍＬ。本文对极谱波的性质和机理进行了初步探讨，本法用于土壤中总钴和有效钴的测定，结果满意。     

铌（Ⅴ）—1—苯基—3—甲基—4—苯甲酰基—吡唑啉酮—5络合物吸附波的研究

在ｐＨ＝５．０的ＨＡｃＮａＡｃ介质中，Ｎｂ（Ⅴ）与１－苯基－３－甲基－４－苯甲酰基－吡唑啉酮－５（ＰＭＢＰ）生成络合物，于一０．９６Ｖ（ｖｓ．ＳＣＥ）出现一尖极谱波。在滴汞电极上用示波极谱仪或在悬汞电极上则吸附伏安曲线。峰电流与Ｎｂ（Ⅴ）浓度分别在０．００７５－０．８０μｇ／ｍＬ及０．００００７５－０．００７５μｇ／ｍＬ范围内呈线性关系。实验 ３     

铟（Ⅲ）－PMBP－Ferron极谱络合吸附波研究

在ＨＣｌ－ＮａＡｃ介质（ｐＨ２．５）中，可获得灵敏的Ｉｎ（Ⅲ）－ＰＭＢＰ－Ｆｅｒｒｏｎ极谱络合吸附波，峰电位在－０．６５Ｖ处（ｖｓ·ＳＣＥ），检出限为０．０４ｎｇ／ｍＬＩｎ。峰电流与铟浓度在０．０８～２００ｎｇ／ｍＬ范围内呈线性关系。本法测定工业废水中的痕量铟，结果满意。本文还研究了极谱波的性质和机理。     

二阶导数差示脉冲极法用于醋酸氟氢可的松的定量研究

用二阶导数差示脉冲极谱法对醛酸氟氢松进行了定量分析。在０．００１ｍｏｌ／Ｌ硫酸＋乙醇＋水（１＋２５＋２４）的底液中，醋酸氟氢可的松于－０．３４０Ｖ处出现一良好的二阶导数差示脉冲极谱，在５－１４０μｇ／ｍＬ范围内，醋酸氟氢可的松的浓度与其二阶导数差示脉冲极谱峰幅值呈线性关系，检测限为０．４ｎｇ／ｍＬ。本法操作简单、快速、灵敏、结果准确。     

铬蓝黑B指示催化动力学测定痕量钒的研究

本基于在酸性条件下，钒对溴酸钾氧化铬蓝黑Ｂ反应的催化作用，建立了测定痕量钒的催化动力学新体系。以极谱法测定的线性范围为０～１０ｎｇ／１０ｍＬ， 检测下限为１．４×１０＾－１２ｇ／ｍＬ；以光度法测定的线性范围为０～１０ｎｇ／６ｍＬ＜检测下限为１．１１×１０＾－１１ｇ／ｍＬ。应用于饮用水及人发中痕量钒的测定，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.     

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.     

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。     

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^-。     

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。