单柱离子色谱法测定痕量草酸根离子

本文采用单柱离子色谱系统测定了Ｃ２Ｏ＾２－４，以１．３ｍｍｏｌ／Ｌ葡萄糖酸钠／１．３ｍｍｏｌ／Ｌ硼砂为淋洗液测定Ｃ２Ｏ＾２－４，８常见阴离子Ｃｌ＾－，ＮＯ＾－３，ＨＰＯ＾２－４，ＳＯ＾２－４不干扰测定，Ｃ２Ｏ＾２－４的检出限为０．５７ｍｇ／Ｌ，相对标准偏差为１．０７％，工作曲线的线性范围为０．５７－５００ｍｇ／Ｌ，应用本方法测定了加Ｃ２Ｏ＾２－４的自来水样，Ｃ２Ｏ＾２－４的回收率为９９．５２％。     

硅钼杂多阴离子薄膜修饰电极线性扫描伏安法测定黑液中要溶性硅

本报导了以玻碳电极为基体的１∶１２硅钼杂多阴离子薄膜化学修，铈电极的制备及其电化学特性。并应用于导数伏安法测定。在４．０×１０＾－３ｍｏｌ／Ｌ９ＮＨ４）６Ｍｏ７Ｏ２４－６６．８×１０＾－２ｍｏｌ／ＬＮａ３Ｃｉｔ－０．４８ｍｏｌ／Ｌ ＮＨＯ３体系中，硅浓度在８．３×１０＾－７～１．７×１０＾－３ｍｏｌ／Ｌ。对可溶性硅（以ＳｉＯ２计）为２４５．０５ｍｇ／Ｌ的黑液，稀释１０倍后，取２．００ｍＬ平行测定     

二溴邻羧基偶氮氯膦光度测定铝合金中微量锶

本介绍在一定量钙、钡共存下测定锶的新方法。在０．４８ｍｏｌ／Ｌ Ｈ２ＳＯ４介质中，二溴邻羧基偶氮氯膦与锶形成２：１的蓝色络合物，最大吸收波长为６３０ｎｍ。摩尔吸光系数为３．２×１０＾４Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，锶量在０－１ｍｇ／Ｌ范围内符合比耳定律，经过二氧化锰共沉淀分离富集后，可测定各种复杂铝合金样品中痕量锶。     

抑制型离子色谱快速测定I^—,SCN^—,S2O^2—3

本用抑制型离子色谱，薄壳强碱性阴离子交换树脂为分离柱，柱温为３０±１℃，在常规淋洗液ＮａＨＣＯ３－Ｎａ２ＣＯ３中加入对－硝基苯酚作为有机改进剂，测定了Ｉ＾－、ＳＣＮ＾－、Ｓ２Ｏ＾２－３离子。它们有良好的线性关系，三种离子浓度在５．０～３０．０ｍｇ／Ｌ范围内其相关系数分别为：ｒＩ＾－０．９９９４、ｒｓｃｎ＾－０．９９０６、ｒｓ２ｏ＾２－３０．９９８５，检测限分别为：Ｉ＾－０．１７ｍｇ／Ｌ、ＳＣＮ＾     

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     

测定超氧化物歧化酶活性的一种新的极谱分析方法

报道一种测定超氧化物歧化酶活生的新极谱分析方法，在０．１２５ｍｏｌ／ＬＮＨ３．Ｈ２Ｏ－０．７５ＭＯＬ／ｌ ｎｈ４ｃＬ－２．５％，Ｎａ２ＳＯ３－０．５％，吐温－８０－的介质中，ＳＯＤ在－０．５２Ｖ处产生一氧极谱催化波。ＳＯＤ在１．０×１０＾３Ｕ／Ｌ－４．０×１０＾３Ｕ／Ｌ的活性含量范围内与催化电流呈线性关系，检出限为８．０×１０＾２Ｕ／Ｌ。     

平台石墨炉原子吸收法测定高温镍基合金中铋

本文用１ｍｇ／ｍＬ镍和０．２ｍｇ／ｍＬ钯作混合基体改进剂，提高了测定铋的灰化温度和抗干扰能力，且灵敏度几乎不变。可不经分离样品基体，直接用平台石墨炉原子吸收法测定高温镍基合金中铋。方法特征量为１８ｐｇ，检出限为０．０８１μｇ／ｇ。对含０．３－０．７μｇ／ｇ铋的镍基样品测定，相对标准偏差为３．０％－５．９％，回收率在８５％－１１９％之间。     

硫化物的快速分光光度法测定

提出了测定微量硫化物的快速亚甲蓝分光光度法，实验结果表明，在硫酸溶液中，Ｋ２Ｃｒ２Ｏ７＋对二甲氨基苯胺＋Ｓ＾－２迅速显色反应形成亚甲蓝，表现摩尔吸收系数为４．０６×１０＾４Ｌ．ｍｏｌ＾－１．ｃｍ＾－１；最大吸收波长为６６４ｎｍ；线性范围为０～０．８ｍｇ／Ｌ，实验了采用全差示光度法直接测定水中硫化物的条件，用于某江水中２１．６μｇ／Ｌ硫化物测定时，相对标准偏差为３．２％（ｎ＝６）；试样的标准加入回收     

硅胶管采样—液相色谱法测定空气中的氯氰菊酯

本文报道空气中氯氰菊酯的高效液相色谱测定方法，空气样品用硅胶管采样，经甲醇洗脱后用ＨｙｐｏｒｓｉｌＯＤＳ柱分离，紫外检测器检测，在本法的测定条件下，最低检测浓度为０．０４ｍｇ／ｍ＾３，当氯氰菊酯浓度范围为０～２５．０ｍｇ／Ｌ时，呈线性响应关系，相对标准偏差为２．４％～８．４％，本法的解吸效率为９６．８％～１００．３％，采样效率为１００％，氯氰菊酯在硅胶管中可稳定７ｄ。     

铋—2,3,4—三羟基—4‘—磺基—偶氮苯配合物吸附波的研究

在０．０６ｍｏｌ／Ｌ柠檬酸钠－０．００３ｍｏｌ／Ｌ ＨＣｌ（ｐＨ６．５）介质中，２，３，４－三羟基－４＇－磺基－偶氮苯和铋产生灵敏的单扫描极谱导数峰，铋含量在０～６．７×１０＾－６ｍｏｌ／Ｌ范围内与波高成线性关系，检测限２．４×１０＾－８ｍｏｌ／Ｌ。用提出的方法测定了锡中的铋，并对反应机理进行了研究。     

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。