填充毛细管液相色谱—毛细管气相色谱在线联用分析柴油全组成

采用填充毛细管液相色谱（ＰＣ－ＨＰＬＣ）与毛管气相色谱（ＣＧＣ）在线联用技术分析柴油全组分。半填充硅胶、半填充氨基的ＰＣ－ＨＰＬＣ柱（０．３２ｍｍ ｉ．ｄ）用于样品族分离（烷烃、单环芳烃、双环芳烃、三环芳烃和胶质）。经ＰＣ－ＨＰＬＣ分离后的各族组分（峰体积小于３０μＬ）被依次存放在多位储存接口内，然后分别转入ＧＣ作单个组分定量分析，可得出各族组分的相对含量及烷烃的碳数的正异构分布。该方法是分析柴油     

对土壤及玉米植株中均三氮苯类除草剂的残留分析

土壤或玉米植株样品用Ｖ（甲醇）∶Ｖ（乙腈）＝１∶１提取,提取液用石油醚净化后,浓缩液过Ｃ１８小柱净化,最后用Ｎｏｖａ－ＰａｋＣ１８柱进行ＨＰＬＣ分析。回收率：氰草津为８２．４％～９９．８％,莠去津为８５．６％～１０２．３％,西草净为８９．１％～１０８．４％。     

反相高效液相色谱分离测定铁—芳烃络合物光引发剂及光解动力学研究

本文以反相高效液相色谱法（ＲＰ－ＨＰＬＣ）研究了铁－芳烃络合物光引发剂及光解产物的分离条件和影响因素，推导出光解动力学方程式，方法灵敏度高，引发剂的检测限为１００ｎｇ／Ｌ，测定的标准偏差为０．３１％～０．４６％，相对标准偏差为０．８２％～２．１３％，在此条件下样品杂质不干扰测定。     

毛细管区带电泳在氧氟沙星含量分析中的应用

氧氟沙星（ＯＦ）是第三代喹诺酮类药物中效果最好的广谱抗菌素之一。由于它在ｐＨ２～１１范围内难溶于水与醇，给用ＨＰＬＣ法检测其含量带来一定困难。本文报告了用毛细管区带电泳（ＣＺＦ）分离检测该药的方法。由于使用ｐＨ调制样品引入技术，克服了其溶解性不好给ＨＰＬＣ法所带来的困难。其实验条件为：５０ｍｍｏｌ／Ｌ硼砂（ｐＨ１．５）为电泳缓冲液，２８０ｎｍ为紫外检测波长，２５ｋＶ为电泳电压。样品由高差进样方式引入分离毛细管（５．１２ｃｍ×５０μｍｉ．ｄ．，有效分离长度为３８．５ｃｍ）。用磺胺作内标，ＯＦ在４８～５３０ｍｇ／Ｌ及５８０～９７０ｍｇ／Ｌ范围内可进行定量分析。保留时间（ｔｒ）及相对紫外吸收（Ａ（样品）／Ａ（内标））的日内－ＲＳＤ值分别小于１．０％和２．４％（ｎ＝６）。     

土壤中残留的阿特拉津及其代谢产物的高效液相色谱和气－质谱联用分析

用一种简便、快速的前处理和高效液相色谱法（ＨＰＬＣ）对土壤样品中残留的阿特拉津及其主要代谢产物脱乙基阿特拉津、脱异丙基阿特拉津和２－羟基阿特拉津进行定量分析，样品添加回收率因土壤种类和化合物而异：７８～１２１％（阿特拉津、脱乙基阿特拉津、脱异丙基阿特拉津）和４０～７５％（２－羟基阿特拉津），最小格测浓度为０．００５ｍｇ／ｋｇ；应用气－质联用法（ＧＣ／ＭＳ）对前三种化合物和脱乙基－脱异丙基阿特拉津进行了定性分析，谱库检索匹配程度达到９０％以上。     

高效液相色谱（HPLC）测定芦丁纯度和含量

研究了一种用于芦丁含量测定与纯度检验的高效液相色谱法（ＨＰＬＣ），该法具有较高精度和良好专属性，适于例行分析，分离在Ｃ８柱上进行，流动相为ＴＨＦ（四氢呋喃）－磷酸缓冲液，检测波长为２８０ｎｍ，检测限为０．５μｇ／ｍＬ，可检出０．０５％的杂质用于某些实际样品分析，结果良好。     

反相高效液相色谱法同时测定发酵乳中的蛋白糖和氨基酸

介绍了同时测定发酵乳中蛋白糖和氨基酸的ＨＰＬＣ方法。样品经甲醇除去蛋白,异硫氰酸苯衍生,ＲＰ－ＨＰＬＣ法测定。蛋白糖回收率为９４．２％～９８．７％,精密度以相对标准偏差表示为２．１５％～３．７４％。     

高效液相色谱-间接光度检测法测定体液中西梭霉素

采用高效液相色谱－间接光度检测法（ＨＰＬＣ－ＩＰＤ）,在流动相中加入具有紫外检测响应的检测剂烟酰胺,用紫外检测器直接测定体液中无紫外吸收的西梭霉素含量。固定相为ＳｐｈｅｒｉｓｏｒｂＣ１８,流动相为甲醇－乙腈－水（２０∶１０∶７０）,内含磷酸０．０５ｍｏｌ／Ｌ、烟酰胺０．５ｍｍｏｌ／Ｌ、庚烷磺酸钠５ｍｍｏｌ／Ｌ。血清样品中西梭霉素平均回收率为９６．９２％±４．６３％,日内和日间变异系数分别为４．７５％和５．６５％。     

高效液相色谱法测定强化奶及食品中维生素D含量

介绍用反相高效液相色谱法（ＨＰＬＣ）测定食品中ＶＤ含量,样品经皂化、正己烷提取、正相ＨＰＬＣ净化,用反相ＨＰＬＣ定量分析。回收率为９４．８８％～９９．７０％,批内和批间ＣＶ分别为１．６２％和２．１２％。分析了奶粉、要素膳、肉松、儿保饮料等８种食品中ＶＤ含量,亦可用于各种食品中ＶＤ分析。     

柱切换高效液相色谱法在生物样品中的应用

评述了柱切换高效液相色谱法（ＣＳＨＰＬＣ）在生物样品分析中的应用进展．分别对柱切换装置，血样、尿样提取液中被测组分浓度的测定，在线浓缩样品技术以及ＣＳＨＰＬＣ的联用进行了介绍．     

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.     

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。