头孢噻肟钠降解产物在银微电极上示差脉冲阴极溶出伏安法的测定

基于包噻肟钠（ＣＴＸ）在０．１０ｍｏｌ／Ｌ ＮａＯＨ溶液中水浴降解产物含有巯基（－ＳＨ），在ＰＨ４．５ＮａＡｃ－ＨＡｃ介质中，于奶微电极上产生－灵敏的吸附伏安还原峰，峰电位Ｅｐ＝－０．５５Ｖ（ｖｓ．ＳＣＥ）。示差脉冲溶出峰电流与ＣＴＸ浓度在１．０＊１０＾－７－１．０＊１０＾－５ｍｏｌ／Ｌ范围内呈线性关系，方法可应用于模拟样品ＣＴＸ的检测，令人满意。     

差分脉冲吸附溶出法测定痕量铜

本文报道一种差分脉冲吸附溶出测定痕量铜的方法，在３．０×１０＾－５ｍｏｌ／Ｌ双硫腙－０．５ｍｏｌ／Ｌ，ＮａＯＨ－０．０１ｍｏｌ／Ｌ，ＥＤＴＡ底液中，在汞膜电极上于－０．５Ｖ，吸附富集铜－双硫腙配合物３ｍｉｎ，然后记录其在一０．８７Ｖ的差分脉冲阴极溶出峰，溶出峰高与铜浓度在０．５～１０ｎｇ／ｍＬ范围内有线性关系（ｒ＝０．９９８），检测限为０．３ｎｇ／ｍＬ。应用本方法测定地质化探化试样，电镀废水中的痕     

铜（Ⅱ）锌（Ⅱ）—氟哌酸体系电化学行为及示波极谱法研究

铜（Ⅱ）和锌（Ⅱ）分别在０．１ｍｏｌ／ＬＫＨ２ＰＯ４－Ｎａ２ＨＰＯ４缓冲溶液（ｐＨ６．５）和０．２５ｍｏｌ／ＬＮＨ４Ｃｌ溶液中，与氟哌酸形成良好的络合吸附波，峰电位分别为－０．２６Ｖ和－１．２８Ｖ（ｖｓ．ＳＣＥ），络合比分别为１：３和１：２，峰电流与铜（Ⅱ）和锌（Ⅱ）的浓度均在４．０×１０＾－７～５．０×１０＾－６ｎｏｌ／Ｌ范围内呈线性关系，检测限分别为７．０×１０＾－８和５．０×１０＾－８ｍｏｌ     

Mo（Ⅵ）－PAN与Mo（Ⅵ）－PAR体系的极谱性质对比研究

本文比较了Ｍｏ（Ⅵ）－１－（２－吡啶基偶氮）－２－萘酚（ＰＡＮ）与Ｍｏ（Ⅵ）－４（２－吡啶基偶氮）间苯二酚（ＰＡＲ）的极谱性质，讨论它们在作为吸附波试剂时的优缺点，以求得在选择络合剂时的感性和理性认识．本文还报道了Ｍｏ（Ⅵ）－ＰＡＮ－ＫＢｒＯ３吸附催化波体系，最佳实验条件，０．１ｍｏｌ／ＬＨＡｃ－－ＮａＡｃ，ｐＨ＝４．６，０．０１ｍｏｌ／ＬＫＢｒＯ３，２．５×１０－５ｍｏｌ／ＬＰＡＮ．峰电位为－０．７１Ｖ（ｖｓ．ＳＣＥ），检出限１×１０－９ｍｏｌ／Ｌ，线性范围０～６×１０－７ｍｏｌ／Ｌ     

铜（Ⅱ）锌（Ⅱ）－氟哌酸体系电化学行为及示波极谱法研究

铜（Ⅱ）和锌（Ⅱ）分别在０．１ｍｏｌ／ＬＫＨ＿２ＰＯ＿４－Ｎａ＿２ＨＰＯ＿４缓冲溶液（ｐＨ６．５）和０．２５ｍｏｌ／ＬＮＨ＿４Ｃｌ溶液中，与氟哌酸形成良好的络合吸附波，峰电位分别为－０．２６Ｖ和－１．２８Ｖ（ｖｓ；ＳＣＥ）；络合比分别为１：３和１：２；峰电流与铜（Ⅱ）和锌（Ⅱ）的浓度均在４．０×１０￣（－７）～５．０×１０￣（－６）ｍｏｌ／Ｌ范围内呈线性关系，检测限分别为７．０×１０￣（－８）和５．０×１０￣（－８）ｍｏｌ／Ｌ。用线性扫描和循环伏安法等手段研究体系的行为，表明均具吸附性，而铜（Ⅱ）－氟哌酸体系属络合物中铜（Ⅱ）的两电子还原的可逆过程。     

亚硝酸根—巯基乙酸—钴（Ⅱ）络合物的极谱吸附波研究

提出了一个测定痕量亚硝酸根的极谱吸附波新体系．在含有巯基乙酸（ＴＧＡ）和钻．（Ⅱ）的 ｐＨ ４．４的 Ｈ２ＳＯ４－ＮａＡｃ介质中，得到一灵敏的亚硝酸根络合物单扫极谱吸附波，峰电位为－０．７５ Ｖ（ｖｓ．ＳＣＥ）．峰电位与亚硝酸根浓度在１．１× １０－３－８．７×１０－６ｍｏｌ／Ｌ范围内呈线性关系．检出限为 ５． ５×１０－９ ｍｏｌ／Ｌ．本法简便快速，选择性好，用于水样和食品中痕量ＮＯ-２的测定，结果满意。     

3,3‘—四亚甲基—双—（1—苯基—5—吡啶酮—4—羟酸酯）极谱行为研究

ＴＰＰＣ在０．０８ｍｏｌ／ＬＣＨ３ＣＯＯＮａ和０．４ｍｏｌ／ＬＣＨ３ＣＯＯＨ（ＮａＡｃ－ＨＡｃ下同）底液条件下，在电位－１．５７Ｖ附近产生一尖锐的导数波，峰高在３．７×１０＾－６－５．６×１０＾－５ｍｏｌ／Ｌ范围内呈线性关系，同时，讨论了极谱波的性质及电极反应机理。     

碳纤维汞膜微电极1.5次微分伏安法测定胆固醇的研究

将胆固醇吸附在碳纤维汞膜微电极表面，阳极溶出时，可产生一个灵敏的１．５次微分溶出峰，其峰电位为－０．０６Ｖ（ｖｓ，ＳＣＥ，下同），峰电流和样品浓度在１．０×１０－５～１．０×１０－７ｍｏｌ／Ｌ范围内有良好的线性关系。检出限可达１．０×１０－８ｍｏｌ／Ｌ。本文讨论了测定条件，建立了测定胆固醇的新方法，并对实际样品进行了分析。     

砷的氢催化波研究及硫中微量砷的测定

砷在１．５×１０＾－４ｍｏｌ／Ｌ Ｃｏ－０．１ｍｏｌ／Ｌ ＫＣＮＳ－１％抗坏血酸－０．７ｍｏｌ／Ｌ Ｎａ２ＳＯ４－４×１０＾－３ｍｏｌ／Ｌ ＮａＢｒ介质中产生一灵敏催化波，峰电位为－１．１Ｖ。采用微分脉冲极谱法研究了各项实验条件，建立了直接测定硫中微量砷的方法。该法简便快速，结果满意。     

催化动力学光度法测定痕量苯酚

研究了在硫酸介质中苯酚对Ｉ＾－１催化Ｃｅ＾４＋－Ａｓ（Ⅲ）反应的抑制作用及其动力学条件。建立了用催化动力这光度法测定痕量苯酚的新方法，结果表明，在０．００１ｍｏｌ／ＬＣｅ（ＳＯ４）２，０．００１２５ｍｏｌ／Ｌ，Ａｓ２Ｏ３，０．０１ｍｇ／Ｌ，ＫＩ，０．０１２５ｍｏｌ／Ｌ，Ｈ２ＳＯ４和０．１３％（ｗ／ｖ）ＮａＣｌ溶液中测定苯酚，其表面摩尔吸光系数为２．１×１０＾５Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，线性范围     

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.

     

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。     

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。     

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.     

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.     

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。