停流流动注射—动力学方法多组份同时测定的研究：铁（Ⅱ）,钛（Ⅲ）和…

依据诱导反应原理，提出了同时测定多组份的动力学方法，并以停流流动注射分析研究了Ｆｅ（Ⅱ），Ｔｉ（Ⅲ）及Ｖ（Ⅳ）诱导的Ｃｒ（Ⅵ）－Ｉ＾－反应体系，建立了铁，钛和钒同时测定的条件。对铁，钛和钒测定的线性范围分别为０－２．２μｇ／ｍｌ，０－３．１μｇ／ｍｌ及０－１．８μｇ／ｍｌ，检测限分别为０．０１２，０．０２０和０．０１８μｇ／ｍｌ。     

固相反射光度法测定VB12中的痕量钴

研究了以活化硅胶作吸附剂，固相反射吸光光度法测定钴。试验表明，在ＰＨ＝４．０的乙酸钠－乙酸缓冲溶液中，０．０５ｇ活化硅胶对钴－ＰＡＮ〗１－（２－吡啶偶氮）－２－萘酚〖的吸附达最大值，形成的绿色络合物的最大反射吸收波长为６２５ｎｍ，Ｃｏ＾２＋含量在０～６．０μｇ／２５ｍｌ范围内，有良好的线性关系，检出限为８ｎｇ．ｍｌ＾－１，相对标准差为４．９７％。方法用于ＶＢ１２针剂中钴的测定，结果满意。     

氢化物发生电感耦合等离子体原子发射光谱法同时测定水和生物样品中…

研究了一种小型同心氢化物发生配置一个气液分离器后与多道ＩＣＰ－ＡＥＳ联用，同时测定水和生物样品中砷、铋、锑、硒的方法。检出限为砷０．４μｇ／Ｌ，铋０．５μｇ／Ｌ，锑１．４μｇ／Ｌ，硒０．５μｇ／Ｌ，相对标准偏差为砷２．７％，铋１．５％，锑２．７％，硒１．９％。用本法测定美国和国家标准物质中的氢化元素，结果满意。     

单扫描极谱法连续测定人发中的微量元素锌铁锰铜

本提出在０．１５ｍｏｌ／Ｌ乙二胺－７．５×１０＾－３ｍｏｌ／Ｌ三乙醇胺－２．５×１０＾－２ｍｏｌ／Ｌ硫氰酸钾底液中单扫描极谱法测定锌、铁、锰，续加硫酸（０．３ｍｏｌ／Ｌ）测定铜的方法，峰电位分别为－１．４２Ｖ，－１．６３Ｖ，－１．７１Ｖ，－０．４８Ｖ（ｖｓ．ＳＣＥ），线性范围：０．０５～１．４μｇ／ｍＬＭｎ，０．０４～１μｇ／ｍＬＣｕ，最低检出浓度．０３，０．０５，０．０２，０．０４μｇ／ｍＬＭ     

示波极谱法测定金属铅及铅锌矿浸出渣中微量锑

在ｐＨ２．４的邻苯二酚紫－Ｓｅ体系中，Ｓｂ产生一个灵敏的极谱波，其导数峰电位为－０．２８Ｖ，线性范围０．００８－０．４μｇ．ｍｌ＾－１，许多离子不干扰，不用分离和富集，可直接测定金属铅及铅锌矿浸出渣中微量锑。方法具有灵敏，快速，准确的特点。     

铜—2,3,4—三羟基—4‘—磺基—偶氮苯配合物吸附波的研究

在０．０６５ｍｏｌ．Ｌ＾－１柠檬酸钠－０．０４６ｍｏｌ．Ｌ＾１ＨＣｌ（ｐＨ６．６）介质中，２，３，４－三羟基－４’－磺基－偶氮苯和铜形成配合物，在单扫描示波极谱仪上于－０．２Ｖ处产生灵敏的吸附峰，测定铜的浓度范围为０．００５－０．３μｇ．ｍｌ＾－１，检出限为０．００２５μｇ．ｍｌ＾－１，本法已成功地用于人发及硫酸镍中铜的测定，并进行了电极反应机理研究。     

HCl－KSCN体系季胺盐（TOMA·Cl）萃取光度法测定痕量铜的研究

研究了以氯化三辛基甲基胺的二甲苯溶液为萃取剂，在ＨＣｌ－ＫＳＣＮ介质中痕量铜的萃取和分光光度测定。对萃取、分离定量的最适条件，选用适宜的反萃取剂以及铜的萃取体系等进行了详细研究。结果表明，桑德尔灵敏度为４．５×１０~（－４）μｇ／ｃｍ~２，相比Ｖ_ｗ／Ｖ_０＝４０，铜量在０．０２～１μｇ／ｍＬ范围遵守郎伯－比尔定律，成功地建立了一个新的测定微量铜的方法。     

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。     

二氯荧光素—氯化十六烷基吡啶荧光猝灭法测定微量碘

本文研究了用二氯荧光素（ＤＣＦ）－氯化十六烷基吡啶（ＣＰＣ）体系荧光猝灭法测定微量碘。在ｐＨ为２．８－３．１的Ｈ２ＳＯ４介质中，检出限为０．３０μｇ／２５ｍｌ线性范围为０．３０－２．００μｇ／２５ｍｌ，本法灵敏度高，选择性好，适用于微量碘的测定。     

萃取—缝管原子捕集原子吸收法测定水中碲（Ⅳ）和磅（Ⅵ）

研究了碲（Ⅳ）和碲（Ⅵ）在ＤＤＴＣ－ＣＣｌ４体系中的萃取和反萃取行为，并用缝管原子捕集技术结合火焰原子吸收法测定了水样中的碲（Ⅳ）和碲（Ⅵ），特征浓度为１．２ｇ／Ｌ／１％吸收，检出限０．２μｇ／Ｌ，相对标准偏差１．７％，富集倍中达１００％。     

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.     

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。     

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.     

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.     

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.     

NiY分子筛表面酸性影响其选择性吸附脱硫性能的机理研究

采用原位红外光谱技术,以噻吩、环己烯和苯为模型探针分子,分别考察单一烃分子在NiY分子筛上的吸附与反应行为以及噻吩与烯烃、芳烃间的竞争吸附和催化反应行为。单一探针分子吸附研究发现,NiY分子筛中与Ni物种相关的Lewis(L)酸位是噻吩的选择性吸附活性位;噻吩和环己烯在NiY分子筛中Brnsted(B)酸位上发生的质子化和低聚反应明显弱于HY分子筛。双探针分子竞争吸附研究发现,环己烯二聚体在NiY中强B酸位上的强化学吸附与噻吩存在显著的竞争吸附行为。另外,苯和噻吩在NiY上的竞争吸附现象在373K时明显减弱。由此,在选择性吸附脱硫过程中,减少吸附剂表面B酸中心可降低烯烃对噻吩的竞争吸附,另外适当提高吸附体系的温度可以有效避免芳烃对噻吩的竞争吸附。     

化学单元教学设计的探索

论述了单元教学是落实化学新课程三维目标的基本教学过程,同时对教学单元的含义、教学单元的选择与建构、化学单元教学设计及其意义进行了阐述。