用HPLC法测定五氯硝基苯和多菌灵的复配制剂

采用ＨＰＨｙｐｅｒｓｉｌＣ１８色谱柱,甲醇和水梯度洗脱,用二极管矩阵检测（２５４ｎｍ）的ＨＰＬＣ法,１２ｍｉｎ内同时测定了五氯硝基苯－多菌灵可湿性粉剂中２种有效成分的含量。该法简便、快速、准确,标准偏差分别为０．１２％和０．１５％,相对标准偏差分别为０．４６％和１．４４％。     

染毒粮食中7种化学战剂的气相色谱分析方法

为了研究染毒粮食（大米、面粉）中７种化学战剂的检测方法,建立了相应的气相色谱分析方法。该法采用火焰光度检测器检测,ＢＰ－１０毛细管色谱柱分离,二氯甲烷萃取。模拟染毒大米、面粉中化学战剂测定相对误差为２．０％～１２．０％、８．１０％～２７．３％。相对标准偏差分别为０．９％～６．１０％、３．９５％～１６．８％。方法的最低检出浓度为０．０１～２μｇ／ｇ。所建方法操作简便,灵敏度高。     

固相萃取—紫外导数光谱法测定血中茚满二酮类抗凝血杀鼠剂

报道了血中敌鼠、氯敌鼠、杀鼠酮的题示测定方法。该法操作简便快速、回收率高，灵敏度较高，萃取使用国产高分子多孔微球ＧＤＸ３０１，价廉易得。三种杀鼠剂以１０ｍｇ／Ｌ量分别加于血中，回收率依次为１００．５％±２．９％、１０１．５％±１．３％及９９．３％±１．５％；血中三种杀鼠剂检出限分别为０．４、０．６及０．４ｍｇ／Ｌ。     

比值导数紫外吸收光谱法测定阿司匹林中的微量水杨酸

本文应用比值导数吸收光谱法于药物阿司匹林中微量水杨酸含量的测定,在０．０１￣０．１２％浓度范围内比值导数光谱峰高与水杨酸浓度成正比。线性相关系数为０．９９９４,检出限为０．００５％,样品测定回收率为９５．０％￣１０２．５％。将其用于阿司匹林原料中微量水杨酸杂质含量的测定,乙酰水杨酸含量在９０．０％￣９９．０％范围内,不干扰微量水杨酸的测定。     

2.5次微分溶出伏安法同时测定人脑中铜,铅,镉,锌

本文通过硝酸－硫酸混合酸消化脑样，在０．０３ｍｏｌ／ＬＨＣｌＯ４底液中，采用悬汞电极２．５次微分阳极溶出伏安法同时测定人脑中铜、铅、镉、锌四种微量元素。在选定的实验条件下，所述元素的浓度在５～１００ｎｇ／ｍＬ范围内与峰高成线性关系。用于人脑中铜、铅、镉和锌的分析，其相对标准偏差分别为６．５％、１０．５％、１２．７％和３．１％，其回收率为９８．０％、９４．０％、１０２．０％和１０４．０％。     

食品中甜蜜素的紫外分光光度法测定

采用紫外分光光度法测定食品中的甜蜜素。该法在０．２～１．０ｇ／Ｌ甜蜜素范围内符合比尔定律,回收率为９５．０％～１０２．７％,相对标准偏差（ＲＳＤ）为２．６６％～５．４０％,食品中共存的苯甲酸、山梨酸、糖精钠在０～１０．０ｇ／Ｌ范围内,色 ０～２．０ｇ／Ｌ范围内不影响测定。方法简捷,准确。     

乳液电导法对麻黄中麻黄碱和伪麻黄碱的分步检测

使用水－界面膜－油体系通过物质具有不同的酸离解常数及透膜常数以提高电导滴定方法的选择性,对麻黄草中的混合生物碱进行了分步测定,终点明确。盐酸麻黄碱回收率９９．８％±０．８％。麻黄草中麻黄碱含量０．４１％、伪麻黄碱０．１０％,其余生物碱０．０６％,生物碱总量０．５８％,与ＨＰＬＣ法结果总体一致。     

病人血样中痕量锗,锶的石墨炉原子吸收光谱法测定

本文运用石墨炉ＡＡＳ法加基体改进技术，测定了５０岁以上病人血清及环境水样中锗和锶的含量。用０．０１ｍｏｌ／ＬＨＮＯ３－０．１％ＴｒｉｔｏｎＸ－１００稀释血清，测定精度可与火焰法媲美。锗，锶的特征量分别为２８ｐｇ和１８ｐｇ；线性范围为０－２５０ｎｇ／ｍＬ和－３５．０ｎｇ／ｍＬ；相对标准偏差（ｎ＝１０）４．１０％和２．４９％；回收率分别为９２．２％－９９．０％和９２．０％１０２％。方法快速准确，结果满     

用碳糊修饰电极测定氨基酸的伏安法研究：Ⅰ.色氨酸和酪氨酸在聚酰 …

用含１０％聚酰胺的修饰碳糊电极研究了测定色氨酸和酪氨酸的伏安法,发现在０．２ｍｏｌ／Ｌ盐酸－醋酸钠底液中色氨酸和酪氨酸有良好的氧化峰响应。结合２．５次微分技术,两种氨基酸的检测浓度线性范围良好。色氨酸和酪氨酸的相对标准偏差分别为５．２％和７．０％,检测限分别为０．０２４μｍｏｌ／Ｌ和０．０３４μｍｏｌ／Ｌ。检测特性经统计秀较大的改善。文中对电极过程进行讨论。     

测定染发剂中苯二胺的气相色谱法

建立了气相色谱法同时测定染发剂中邻位、间位、对位苯二胺的方法。方法线性范围：邻苯二胺０．３～４０．０ｇ／Ｌ,对苯二胺０．２～５０．０ｇ／Ｌ,间苯二胺０．４～７０．０ｇ／Ｌ;平均回收率：苯二胺９４．７％,对苯二胺９２．２％,间苯二胺９０．１％。该法灵敏度高、操作简便、准确。     

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.     

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.     

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^-。     

Thermodynamics of the formation of oxosulfides of rare-earth elements

The enthalpies of solution of several oxosulfides of rare-earth elements and the high-temperature enthalpies of oxosulfides and oxosulfates of lanthanum and yttrium were measured using solution calorimetry and high-temperature microcalorimetry techniques. Standard enthalpies of formation and some thermodynamic properties of oxosulfides and oxosulfates were calculated. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2 pp. 294–297, February, 1997.     

探究“铁的锈蚀条件”实验创新设计

设计了铁的锈蚀实验,说明了铁钉的处理方法,增加了温度、酸、碱的影响条件,实现了铁跟蒸馏水及空气中氧气快速反应而生锈,使实验在5 min左右就能够得到准确的结果。