HP－50＋大口径毛细管气相色谱法测定水果中多种有机氯农药残留量

以ＨＰ－５０＋大口径毛细管柱为分离柱，ＧＣ－ＥＣＤ测定水果中１４种有机氯农残。方法的检测限为０．１×１０￣（－９）～２．０×１０￣（－９），回收率范围在８８．６％～１０５．８％，变异系数２．６％～１０．５％。样品前处理采用微量化学法。     

电致化学发光法测定天然水中痕量银（Ⅰ）

对四正丁基碘化胺（ＴＢＡＩ）－银（Ⅰ）－硫脲体系的电致化学发光进行了研究。当在Ｐｔ－Ｐｔ－Ａｇ／ＡｇＣｌ三电极上施加＋１．５Ｖ的正矩形脉冲时，前述体系可观察到电致化学发光现象。银（Ⅰ）对此发光过程有明显的催化作用。银（Ⅰ）的浓度在１．０×１０－８～３．０×１０－６ｍｏｌ／Ｌ范围内与发光强度呈良好的线性关系，检出限为８．０×１０－９ｍｏｌ／Ｌ。相对标准偏差为４％。该法用于测定天然水中的痕量银。结果满意。     

花生中黄曲霉毒素B1、B2、G1、G2的多功能净化柱-高效薄层色谱分析

建立了一种测定食品中黄曲霉毒素（ ＡＦＴ） Ｂ１ 、Ｂ２ 、Ｇ１ 、Ｇ２ 的多功能净化柱（ ＭＦＣ） 净化, 单相展开的薄层色谱法。 以乙腈－ 水（ 体积比９ ∶１） 提取样品中ＡＦＴ, 经ＭＦＣ 净化浓缩后, 采用ＨＳＧ６０ 薄层板, 以丙酮－ 氯仿（ 体积比９ ∶１） 展开, 薄层扫描仪荧光检测扫描定量。该法用于花生样品的检测,４ 种毒素的分离良好; 线性范围：０ ．０５ ～１ ．０ ｎｇ, 相关系数≥０ ．９９９ １; 检出限均达到０ ．５ ×１０ － ９ ; 相对标准偏差为４ ．６７ ％ ～１０ ．２１ ％ ; 样品加标０．５ ×１０ － ９ ～１０ ×１０ － ９ , 平均回收率为８６ ．５ ％ ～９９ ．０％ 。     

毕兹多克隆抗体的制备和分析应用

用琥珀酸酐－碳二亚胺法和氯磺化法合成了毕兹（Ｂｚ）的两种人工抗原Ｂｚ＿ＨＳ＿ｐｒｏｔｅｉｎ和Ｂｚ＿ＳＯ２＿ｐｒｏｔｅｉｎ。由Ｂｚ＿ＳＯ２＿ＢＳＡ（牛血清白蛋白）诱导出的抗血清能够用来测定１０－９ｍｏｌ·Ｌ－１的Ｂｚ，工作曲线的线性范围在３×１０－５～３×１０－９ｍｏｌ·Ｌ－１，相对标准偏差为１３６％（ｎ＝６），回收率在９０％～１１５％。     

分光光度法测定氯化稀土和轻稀土氧化物中的镨,钕,钐

本文提出在１０％盐酸介质，用紫外－可见分光光度法测定氯化稀土、轻稀土氧化物中的镨、钕、钐，测定波长分别为４４４ｎｍ、５７５ｎｍ、４０１ｎｍ，钐对镨的干扰和镨对钕的干扰均可用校正系数加以消除。方法回收率为９７．５％～１０２．９％，检出下限分别为５０×１０￣（－６）ｇ／ｍＬ，１０×１０￣（－６）ｇ／ｍＬ，１００×１０￣（－６）ｇ／ｍＬ。     

高效液相色谱法测定伸筋丹中士的宁含量

采用高效液相色谱法（ＨＰＬＣ）测定了中成药伸筋丹中士的宁含量。色谱条件：氰基柱并加同种类预柱；流动相：甲醇－水－乙酸－三乙胺（９８００：１５５：３０：１５）；ｐＨ６．７；流速：１．０ｍＬ／ｍｉｎ；紫外检测，波长２５４ｎｍ；在４～２０ｍｇ／Ｌ浓度范围内，士的宁的峰面积Ａ与浓度Ｃ间的回归方程为：Ａ＝－７．０１×１０~３＋９．０８×１０~５Ｃ（ｒ＝０．９９９９）；外标法定量，方法精密度ＲＳＤ＝１．９１％（ｎ＝６）。     

高效液相色谱法测定抗氧剂264和对甲酚

用反相高效液相色谱法分离和测定了抗氧剂２６４和对甲酚，其线性范围分别是１．２×１０－９～２．８×１０－８ｍｏｌ和１．８×１０－９～２．４×１０－６ｍｏｌ，相对标准偏差分别为１．７％和０．９８％。     

一种基于形成杂多核络合物的荧光增敏效应的研究：Ⅲ.锰（Ⅱ）,钴（…

本研究了Ｍｎ＾２＋和Ｃｏ＾２＋对７－（８－羟基－３，６－二磺基萘偶氮）－８－羟基喹啉－５－磺酸－硼砂反应体系的混合荧光增敏作用。实验条件下，荧光增敏强度满足线性加和关系的范围是：Ｍｎ＾２＋浓度０￣２．９×１０＾－７ｍｏｌ／Ｌ；Ｃｏ＾２＋浓度０￣８．８～１０＾－７ｍｏｌ／Ｌ；总浓度不超过１．０×１０＾－６ｍｏｌ／Ｌ。检出限量为Ｍｎ＾２＋４．５×１０＾－９ｍｏｌ／Ｌ和Ｃｏ＾２＋１．４×１０＾－８ｍｏ     

高灵敏反相流动注射化学发光法测定抗坏血酸

基于抗坏血酸对Ｆｅ２＋－Ｌｕｍｉｎｏｌ－Ｏ２体系化学发光的抑制效应，利用反相流动注射技术，建立了一个测定抗坏血酸的高灵敏化学发光新方法。该法检出限达２×１０－１０ｇ／ｍＬ；抗坏血酸浓度在 １×１０－９～１× １０－６ｇ／ｍＬ范围内与体系化学发光强度减小量呈良好线性相关；相对标准偏差为１．９％（Ｃ＝５×１０－８ｇ／ｍＬ，ｎ＝１１）。     

乙醛存在下氨基糖苷类抗生素的吸附伏安法研究

用悬汞电极，于Ｂｒｉｔｔｏｎ－Ｒｏｂｉｎｓｏｎ－ＣＨ３ＣＨＯ（ｐＨ９．５～１０．５）体系中研究了妥布霉素、丁胺卡那霉素等五种氨基糖苷类抗生素的吸附伏安行为，并讨论了其电极过程。认为该类抗生素结构上共有的伯、仲氨基与乙醛的衍生化反应产物，在一定电位下易吸附于电极表面。其不可逆还原峰的峰电位为－１．４５Ｖ（ｖｓ．ＳＣＥ）。在选定条件下，浓度在２．０×１０（－９）～２．５×１０（－７）ｇ／ｍＬ范围内均与还原峰峰电流呈良好的线性关系，检测限低至１．０×１０（－９）ｇ／ｍＬ。方法无需预处理即可用于软膏、尿样的测定，回收率在９０．３％～１１４％之间。     

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。