同位素稀释质谱法测量贻贝中微量Ni,Cu,Pb

以天然丰度镍、铜、铅标液为稀释剂标定浓缩同位素￣（６２）Ｎ、￣（６５）Ｃｕ、￣（２０７）Ｐｂ溶液浓度，再以此浓缩同位素为稀释剂，用同位素稀释质谱法（ＩＤＭＳ）测量贻贝中Ｎｉ、Ｃｕ、Ｐｂ的含量。测量结果：贻贝中Ｎｉ，１．０１１±０．０１２×１０￣（－６）；Ｃｕ：７．６２±０．１４×１０￣（－６）；Ｐｂ：２．００８±０．０２４×１０￣（－６）。     

银基汞膜电极电位溶出法测定化妆品中的铋、铅、镉

研究了一种测定化妆品中铋,铅,镉的新方法。在乙二胺－盐酸底液中以银基汞膜电极为工作电极,饱和甘汞电极为参比电极,铂电极为对电极,用电位溶出法测定化妆品中的痕量Ｂｉ,Ｐｂ,Ｃｄ。结果表明,当Ｂｉ,Ｐｂ,Ｃｄ的浓度依次在０．２５￣１８００μｇ／Ｌ,０．１￣３６００μｇ／Ｌ,０．０５￣１２００μｇ／Ｌ范围内,与峰高呈良好的线性关系,样品回收率在９７％￣１０５％之间。本法有较高的精密度和准确度,适于在化妆     

X射线荧光光谱分析法测定多金属矿中的铅锌铜

采用粉末压制的样片进行Ｘ射线荧光光谱分析，测定多金属矿选矿流程中的Ｐｂ、Ｚｎ、Ｃｕ。选择康普顿散射线作Ｐｂ的内标，分析线附近的散射线作Ｚｎ、Ｃｕ的内标，用经验系数法校正基体效应。其分析范围是Ｐｂ：０．１９～７９．２９％，Ｚｎ：０．４５～５０．１１％，Ｃｕ：０．０２１～３１．１０％，分析结果与化学法相符。     

X射线荧光光谱分析测定多金属矿中的铅锌铜

采用粉末压制的样片进行Ｘ射线荧光光谱分析，测定多金属矿选矿流程中的Ｐｂ，Ｚｎ，Ｃｕ，选择康普顿散射线作了Ｐｂ的内标，分析线附近的散射线作ＺｎＣｕ的内标，用经验系数法校正基体效应，其分析范围是Ｐｂ：０．１９～７９．２９％，Ｚｎ：０．４５～５０．１１％，Ｃｕ：０．０２１～３１．１０％分析结果与化学法相符。     

乙基磺原酸钾—MIBK萃取原子吸收测定重晶石中铅,镉

本文较详细地研究了以乙基磺原酸钾作为金属分离的溶剂萃取试剂测定重晶石中铅，镉的条件，并确定了测定方法，铅和镉与乙基磺原酸钾反应生成白色络合物，该络合物在水相溶液中能定量地萃入甲基异丁基甲酮中。它们的回收率分别为９７％－１０３％和９６％－１０１％。铅和镉分别在０－６μｇ／ｍＬ和０－０．８μｇ／ｍＬ呈线性关系。本法可测定０．０００ｘ％－０．ｘ％Ｐｂ，０．０００ｘ％－０．０ｘ％Ｃｄ．     

电感耦合等离子体质谱法测定黄沙土壤中铅同位素比

用电感耦合等离子体质谱法（ＩＣＰ—ＭＳ）测定了５个黄沙原土样品中铅同位素比２０７Ｐｂ／２０６Ｐｂ、２０８Ｐｂ／２０６Ｐｂ，样品来自被认为是黄沙气溶胶源地区，为了使铅同位素测量中质量偏差和漂移减至最少，在样品中加入了铊标准溶液，测量２０５Ｔｌ／２０３Ｔｌ比，校正质量数差别选择的影响．同时，采用ＩＣＰ—ＭＳ和电感耦合等离子体原子发射光谱法（ＩＣＰ一ＡｌＳ）测定了随粒径变化样品中１２种元素浓度的变化．     

4-(2-吡啶偶氮)间苯二酚显色-分光光度法测定无机铅和烷基铅

１引言铅是公路两侧大气监测中重点控制的重金属元素。不同形态铅的毒性差异很大，其中三烷基铅的毒性最大。我国目前尚无大气中烷基铅的监测方法，用分光光度法进行铅形态分析也未见报道。本文报道了４－（２－吡啶偶氮）间苯二酚（ＰＡＲ）显色－分光光度法测定无机铅、二乙基铅和三乙基铅的方法，有较好的回收率和精密度，可用于测定大气飘尘中的烷基铅。二实验部分２．１仪器及试剂７２２型分光光度计，ｐＨＤ－１１型数字式酸度计。０．２４０ｍｍｏｌ／Ｌ二乙基铅（ＰｂＥｔ２）、三乙基铅（ＰｂＥｔ３）和０．４８０ｍｍｏｌ／Ｌ无机…     

儿童多动症与微量元素关系的探讨

为了探讨儿童多动症与微量元素的关系，测定了７２例多动症患儿头发中的六种元素Ｚｎ、Ｃｕ、Ｐｂ、Ｃｒ、Ｆｅ、Ｃａ含量，并将其与正常儿童进行比较，结果表明：多动症组Ｃｕ显著低于正常组，Ｐ〈０．０１，多动症组Ｚｎ显著低于正常组，Ｐ〈０．０５，多动症组Ｐｂ显著高于正常组，Ｐ〈０．０５。提示调整患儿体内微量元素平衡可作为治疗儿童多动症的辅助方法。     

X射线荧光光谱薄膜法测定多金属矿样中常量Pb,Zn,Cu,Fe,Mn

本文拟定了一个Ｘ射线荧光光谱薄膜测定常见铅、锌、铜、锰矿中０．２～ｘｘ％Ｐｂ、Ｚｎ、Ｃｕ、Ｆｅ、Ｍｎ的方法。实验考察了制片重现性和样品分解可靠性对本法结果的关键性影响，采用酸溶、钒作内标、Ｍｙｌａｒ膜制片测量。手续简便、方法精密度和准确性符合有色地质分析质量要求。     

TBP碳糊修饰电极三元络合物体系测定痕量铅（Ⅱ）

研制了磷酸三丁酯（ＴＢＰ）碳糊修饰电极，在含１－苯基－３－甲基－４－苯甲酰基－５－吡唑酮（ＰＭＢＰ）的ＨＣｌ－ＫＣｌ底液中，通过电位富集，将三元络合物Ｐｂ（ＰＭＢＰ）２（ＴＢＰ）２中的铅富集在电极上，用２．５次微分阳极溶出伏安法测定铅．铅浓度在１．０×１０－９～２．５×１０－７ｍｏｌ·Ｌ－１范围内与峰高呈良好的线性关系．该电极用于铜合金和废水中铅的测定，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。     

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。