钴—H2O2—水杨基荧光酮反应体系的新催化动力学分析方法研究

在碱性介质中，痕量钴（Ⅱ）能显著催化Ｈ２Ｏ２氧化水杨基荧光酮的指示反应，本文据此建立了测定痕量钴的新催化动力学分析法，方法线性范围为０．１～２．８μｇ／Ｌ，检测限为０．０２μｇ／Ｌ。测得反应表现活化能为５９．０３ｋＪ／ｍｏｌ。测定了人发，茶叶，土壤和水等样品中钴的含量，结果满意。     

催化褪色光度法测定痕量钴的研究

研究了在ＰＨ１０．５的Ｎａ２Ｂ４Ｏ７－ＮａＯＨ介质中，痕量钴（Ⅱ）对过氧化氢氧化桑色素初色反应的催化作用，建立了催化动力学光度法测定痕量钴的新方法。方法的线性范围为０－１．２μ／ｍＬ检出限为４．４＊１０＾－１８ｇ／Ｌ。用于水和维生素Ｂ１２中钴的测定，结果满意。     

高灵敏催化光度法测定痕量钴

基于在氢氧化钠介质中，钴（Ⅱ）催化过氧化氢氧化５－溴水杨基荧光酮褪色的反应，建立了催化动力学光度法测定痕量钴的新方法，方法检出限为１．１×１０＾－１０ｇ／Ｌ，线性范围为２．５－８０ｎｇ，已成功地用于维生素Ｂ１２、人发及茶叶中痕量钴的测定。     

二溴硝基偶氮氯膦催化动力学光度法测定痕量钴的研究

研究了在ｐＨ７．０磷酸盐介质中，钴催化Ｈ２Ｏ２氧化二溴硝基偶氮氯膦色反应，建立了催化光度法测定痕量钴的新方法，其检出限为５×１０＾－７ｇ／Ｌ，在０．５－３２μｇ／Ｌ范围内，钴与ｌｇ呈良好的关系。     

邻联甲苯胺-过氧化氢催化光度法测定钴

１引言 在碱性介质中,痕量Ｃｏ（Ⅱ）见对Ｈ２Ｑ２氧化邻联甲苯胺（ｏ－Ｔｏｌｉｄｉｎｅ）的显色反应具有强烈的催化作用,探讨了利用该反应进行痕量Ｃｏ（Ⅱ）测定的影响因素,建立了测定痕量Ｃｏ（Ⅱ）的催化动力学光度法,该方法的灵敏度为１．７８ × １０－６ｇ／Ｌ,测定的线性范围为０．８～３．６ μｇ／Ｌ Ｃｏ２＋,应用于维生素Ｂ１２中痕量Ｃｏ（Ⅱ）的测定,结果满意。２实验部分２．１仪器与试剂 ７２１－１００型分光光度计;电热恒温水浴槽;Ｎｉｃｏｌｅｔ ＦＴ－ＩＲ ５ＤＸ红外光谱仪。钴（Ⅱ）标准溶液：１ｍｇ／Ｌ;…     

钴(Ⅱ)催化偶氮胭脂红B的褪色反应特性及应用

基于氢氧内介质中痕量钴对过氧化氢氧化偶氮胭脂红Ｂ的褪色反应的强烈催化作用,建立了催化光度法测定痕量钴的新方法。方法灵敏度为５．２４×１０＾－１２ｇ／ｍＬ,测定范围为０￣３５ｎｇ／１０ｍＬ,对质量浓度为３μｇ／Ｌ的Ｃｏ（Ⅱ）重复测定１１次的相对标准偏差为２．１６％。方法应用于维生素Ｂ１２和矿泉水中痕量钴的测定,结果满意。     

氧化藏红T褪色催化荧光法测定痕量钒

研究了在酸性介质中柠檬酸存在下，痕量钒（Ｖ）催化溴酸钾氧化藏红Ｔ的褪色反应及其动力学条件，建立了催化荧光测定痕量钒的新方法。催化反应在沸水浴中进行８ｍｉｎ，为假零级反应，反应的表观活化能力为９９．２１ｋＪ／ｍｏｌ，反应速度常数为０．１２／ｓ；该方法的检出限为２．２×１０＾－８ｇ／Ｌ；线性范围为０．２￣２．４μｇ／Ｌ研究了共存离子的影响，用于人发和煤灰中痕量钒的测定，结果令人满意。     

吖啶橙催化荧光法测定痕量钒

研究了在酸性介质中柠檬酸存在下,痕量钒（Ｖ）催化溴酸钾氧化吖啶橙退色及其动力学条件,建立了催化荧光法测定痕量钒（Ｖ）的新方法。钒（Ｖ）的线性范围为 ０．２～２．８ μｇ／Ｌ,检出限为 ５．８× １０－８ｇ／Ｌ。３０多种离子基本不干扰测定,将方法用于矿泉水,枸杞和人发样品中钒（Ｖ）的含量的测定,结果满意。此外,还对反应机理进行了初步探讨。     

下基罗丹明B—高磺酸钾动力学光度法测定锗

报道了以锗催化高碘酸钾氧化丁基罗丹明Ｂ为基础的动力学测定痕量铑的方法,详细研究了动力学条件,建立了动力学光度测定痕量铑的新方法。铑浓度在０－１８０μｇ／Ｌ范围内与ｌｏｇ呈线性关系,检出限为２．８４×１０＾－７ｇ／Ｌ,该反应对Ｒｈ或丁基罗丹明Ｂ为为一级反应,表观活化能为６４．０４ｋＪ／ｍｏｌ。本方法用于某些催化剂中铑的测定,其相对标准偏差为１．７６－３．４６％,回收率为９６．８－１０４．７％。     

高灵敏催化光度法测定痕量锰的研究

研究了在ＨＡｃ－ＮａＡｃ介质中，１，１０－邻菲口罗啉存在下，痕量Ｍｎ（Ⅱ）催化高碘酸钾氧化偶氮胂Ⅲ的褪色反应及动力学条件，建立了测定痕量锰的新方法。本法检出限为６．１５×１０－９ｇ／Ｌ，线性范围为０．２～３．２μｇ／Ｌ，已成功用于茶叶、花生、黄豆及中药材枸杞、灵芝中锰的测定。     

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。