动力学光度法测定痕量镉的研究

本研究了氨水介质中，痕量镉阻抑过氧化氢氧化偶氮胂１褪色的新指示反应及其动力学条件，建立了动力学光度法测定痕量镉的新方法，方法检出限为２．７×１０＾－１２ｇＣｄ＾２＋／ｍｌ，测定范围为０－１．０μｇＣｄ＾２＋／２５ｍｌ。     

偶氮胂Ⅲ高灵敏光度法测定痕量铬的研究

研究了偶氮胂Ⅲ与Ｃｒ２Ｏ＾２－７的褪色反应,建立了一种新的光度法测定痕量Ｃｒ方法。发现其在硝酸介质中具有高灵敏的褪色反应,摩尔吸光系数达３．８×１０＾６,Ｃｒ量在０－０．８μｇ／２５ｍＬ范围内符合比耳定律。     

催化动力学光度法测定痕量铜的研究

本研究了铜（Ⅱ）催化抗坏血酸还原ＤＣＢ－偶氮胂的褪色反应，测定了反应级数和表观活化能，探讨了反应机理，建立了测定痕量铜（Ⅱ）的新方法。本法检出限为７．６×１０＾－１２ｇ／ｍｌ，线性范围为０￣６０ｎｇ／ｍＬ，用于测定面粉、血清、中药等几种样品中的痕量铜，结果满意。相对标准偏差为２．０％￣２．９％。     

铬(Ⅵ)-三溴偶氮胂-HNO3催化动力学光度法测定痕量铬的研究

研究了铬（Ⅵ）对硝酸氧化三溴偶氮胂（ＴＢＡＡ）褪色反应的催化作用及其动力学分析,建立了测定痕量铬的新方法。检出限可达ｎｇ级,线性范围０－２．５μｇＣｒ（Ⅵ）／５０ｍＬ,表观摩尔吸光系数５．４＊１０＾５Ｌ．ｍｏｌ＾－１．ｃｍ＾－１。方法简便,灵敏、快速、准确,已用于铸铁标样和人发样品中痕量铬的测定,结果满意。     

某些偶氮胂类试剂高灵敏光度法测定铬(Ⅵ)

研究了氮胂Ⅲ,二溴硝基偶氮胂和二溴羧基偶氮胂３种偶氮胂类试剂与Ｃｒ２Ｏ＾２－７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,摩尔吸光系数均达１×１０＾５Ｌ．ｍｏｌ＾－１．ｃｍ＾－１以上,是目前光度法测定Ｃｒ灵敏度最高的方法之一。可用于水中铬的测定。     

催化动力学光度法测定痕量钼（VI）

研究了在ＮＨ３－ＮＨ４Ｃｌ介质中，钼催化过氧化氢氧化偶氮胂Ⅲ的褪色反应及其动力学条件，建立了一种高灵度测定痕量钼的新方法，可测定０．０２～０．９０μｇ／２５ｍＬ范围内的钼，方法检出限为１．３×１０＾－１０ｇ／２５ｍＬ。     

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。     

钌(Ⅲ)-溴酸钾-番红花红(O)体系催化光度法测定痕量钌

催化光度法测定痕量钌的方法已有报道，作者发现钌（Ⅲ）对溴酸钾氧化番红花红（O）褪色反应有显著的催化作用，以此为指示反应建立了催化光度法测定痕量钌的方法。研究了反应的最佳条件，确定了方法的检出限和线性范围，并对动力学行为进行了研究。将该方法应用于贵金属精矿和氯化渣中痕量钌的测定，取得满意的结果。     

Ru(Ⅲ)-KIO4-偶氮氯膦pA褪色反应用于痕量钌了的催化光度测定

酸性介质中痕量Ｒｕ（Ⅲ）的存在对高碘酸钾氧化偶氯膦ｐＡ的褪色反应有明显的催化作用。此文研究了褪色反应的最佳条件,其Ｒｕ（Ⅲ）的检出限为５μｇ．Ｌ＾－１,钌在５～３２μｇ．Ｌ＾－１范围内符合比耳定律,由此建立了痕量钌的催化光度分析法,方法可直接在水相中进行,用于贵金属精矿中钌的测定,结果满意。     

对碘偶氮氯膦-高碘酸钾-钌(Ⅲ)的褪色反应用于痕量钌的催化分光光度法测定

在Ｈ２ＳＯ４ 介质中对碘偶氮氯膦与高碘酸钾的褪色反应只有在痕量钌（Ⅲ）的存在下才能定量进行。本文研究了该褪色反应的最佳条件及用于痕量钌的测定方法, 其检出限为０．０２ μｇ·１０ ｍ Ｌ－ １, 钌含量在０．０２～０．３０ μｇ·１０ ｍ Ｌ－ １范围内符合比尔定律。该方法用于贵金属精矿中钌含量的测定, 获得满意结果。     

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。     

Acid hydrolysis of carboxymethylcellulose of low degree of substitution

Cotton cellulose was swollen in a sodium hydroxide solution and carboxymethylated by a two-bath method for different periods of time for each process. The kinetics of acid hydrolysis and the crystallinity of the swollen and carboxymethylated samples were measured. The proportion of broken bonds, rate constants for hydrolysis, and permeability of cellulose to hydrolyzing agents were calculated. The susceptibility of glycosidic linkages to acid hydrolysis was improved by carboxymethylation more than by swelling in alkali. The increased accessibility of carboxymethylcellulose to acid was regarded as a consequence of increased intra-and intercrystalline swelling and of the glycosidic bonds' weakness caused by the electron-attracting carboxymethyl group on the C-6 position.     

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。     

Estimation of Kinetic Parameters of Thermal Oxidation of Ilmenite

The aim of the presented work was the investigation of thermal oxidation of ilmenite in static air atmosphere. The investigations were carried out by use of a derivatograph (MOM, Hungary). The changes of crystallographic structure of investigated samples were identified by X-ray diffractometry on Philips PW-1710 diffractometer. In temperature above 500°C appears structure of hematite Fe₂O₃. On the basis of the thermogravimetric measurements, the contracting area and contracting volume models were found as the best fitting experimental data. This revised version was published online in August 2006 with corrections to the Cover Date.     

Mechanism of action of base-catalyzed oxygenation of phenol derivatives

Cyclopropyl derivative of 2,6-di-tert-butylphenol is synthesized as a probe to investigate the mechanism of base-catalyzed autooxidation of phenol derivatives. Our study indicates that one electron reduction of molecular oxygen from phenolate gives phenoxyl radical 3, a key intermediate of autooxidation. The coupling of phenoxyl radical and superoxide radical gives peroxylate anion 4 and produces the final epoxy alcohol adduct 6.     

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^-。     

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.

     

化学计量中不确定度评定研究进展

测量不确定度是表征合理地赋予被测量之值的分散性的参数。本文针对化学计量不确定度评定基础模型仅适用于线性模型、概率分布为正态分布或缩放位移t分布等局限,介绍了近年来不确定度评定的研究热点:蒙特卡罗方法(Monte Carlo Method,MCM),不确定度评定的来源、评定概念、评估方法及其发展过程,扩大了测量不确定度评定与表示的适用范围。     

微量钙的测定方法研究进展

介绍了1995-2006年期间测定微量和痕量钙的方法,如电感耦合等离子体-原子发射光谱法、原子吸收光谱法以及离子色谱法等的工作原理和特点,并说明了其测定微量钙的应用领域。并对微量钙的测定技术进行了展望(引用文献55篇)。