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     

硫羟乳酸作为络合滴定掩蔽剂的研究

本文系统地研究了硫羟乳酸在络合滴定中的掩蔽性能。发现在ｐＨ３．０用ＥＤＴＡ滴定了Ｔｈ＾４＋时，可用它掩蔽Ｓｎ＾４＋，Ｔｌ＾３＋，Ｓｂ＾３＋，Ｂｉ＾３＋，Ｂｈ＾２＋和Ｃｕ＾２＋。在ｐＨ５．５滴定Ｙｂ＾３＋，Ｌａ＾３＋或Ｃｅ＾３＋时，可用它掩蔽Ｓｎ＾４＋，Ｔｌ＾３＋，Ｓｂ＾３＋，Ｂｉ＾３＋，Ｈｇ＾２＋，Ｃｕ＾２＋和Ｃｒ＾３＋，在ｐＨ１０．０滴定Ｍｇ＾２＋时，可用它掩蔽Ｓｎ＾４＋，Ｔｌ＾３＋，Ｓｂ＾３＋     

硫代苹果酸作为络合滴定掩蔽剂的研究

本系统地研究了硫代苹果在络合滴定中的掩蔽性能，发现它在ｐＨ１．５～１０可作为Ｓｎ＾４＋、Ｓｂ＾３＋、Ｔｂ＾３＋、Ｂｉ＾３＋、Ｃｕ＾２＋、Ｈｇ＾２＋和Ａｇ＾＋等的掩蔽剂（在ｐＨ２～３．５还可掩蔽Ｆｅ＾３＋）。掩蔽上述离子后，可在ｐＨ２．５～３用Ｔｈ＾４＋回滴ＥＤＴＡ，在ｐＨ５～６用ＥＤＴＡ滴定Ｚｎ＾２＋或Ｙｂ＾３＋等，或在ｐＨ１０用ＥＤＴＡ滴定Ｍｇ＾２＋、Ｃａ＾２＋、Ｍｇ＾２＋＋Ｃａ＾２＋和Ｍｎ＾     

测定钴的化学发光新体系

研究了新吖啶衍生物９，１０－二甲基吖啶氟磺酸盐的化学发光特性。建立了测定Ｃｏ６２＋的化学发光新体系。方法线性范围为１．０×１０＾－１０－１．０×１０＾－７ｇ／ｍＬ；检测限为５．０×１０＾－１１ｇ／ｍＬＣｏ＾２＋。测定５．０×１０＾－９ｇ／ｍＬＣｏ６２＋的相对标准偏差为６．０％。方法选择性好，用于自来水，江水，池塘水中痕量钴的测定，结果令人满意。     

高锰酸钾—抗坏血酸化学发光体系测定抗坏血酸

本文研究了高锰酸钾－抗坏血酸化学发光体系，建立了测定抗坏血酸的化学发光分析新方法，线性响应的浓度范围为５．０×１０＾－７ｍｏｌ／Ｌ～４．０×１０＾－５ｍｏｌ／Ｌ，检出限为３．０×１０＾－７ｍｏｌ／Ｌ，对２．５×１０＾－６ｍｏｌ／Ｌ抗坏血酸进行１０次平行测定，相对标准偏差为１．６％，考察了２２种物质的干扰情况。用于维生素Ｃ片剂及注射液中抗坏血酸含量测定，结果令人满意。     

2.5次微分循环示波计时电位法用于铑的示波性质的研究

将卷积技术应用于循环示波计时电位信号的处理，提出了２．５次微分循环示波计时电位法并将其用于对铑在ＨＣｌ－ＫＢｒ底液中的示波性质的研究。实验结果表明：在ＨＣｌ＋ＫＢｒ体系的示波图上，Ｒｈ＾３＋的特殊峰是由于铑 对氢的催化作用而产生的；在Ｙ＾２．５－Ｅ曲线上峰高与Ｒｈ＾３＋浓度在４×１０＾－７－７×１０＾－５ｍｏｌ／Ｌ范围内呈线性关系，检测下限为８×１０＾－５ｍｏｌ／Ｌ。     

溶出伏安法测定水中痕量钴

在０．０１ｍｏｌ／ＬＮＨ．Ｈ２Ｏ－ＮＨ４Ｃｌ和３．０×１０＾－５ｍｏｌ／Ｌ安息香缩氨基硫脲体系中，钴产生一灵敏的还原波，其峰电位是－０．９４Ｖ（ｖｓ．ＳＣＥ），峰电流与钴的浓度在２．０×１０－８－１．０×１０＾－６ｍｏｌ／Ｌ范围内成直线关系，检测限为５．０×１０＾－９ｍｏｌ／Ｌ，该法测定水中痕量钴结果令人满意。     

乳酸环丙沙星单扫描示波极谱法研究

研究了乳酸环丙沙星的极谱伏安行为，在ｐＨ＝８．３的０．０２ｍｏｌ／Ｌ，ＮＨ４Ｃｌ－ＮＨ３．Ｈ２Ｏ底液中，乳酸环丙沙星能产生１个灵敏的还原峰，峰电位为－１．６１Ｖ，其导数峰高与浓度在３．９×１０＾－８～１．８×１０＾－６ｍｏｌ／Ｌ和１．８×１０＾６～１．１×１０＾－５ｍｏｌ／Ｌ范围内呈现良好的线性关系，相关系数ｒ＝０．９９９７，检测下限为２．５×１０＾－８ｍｏｌ／Ｌ，用于乳酸环丙沙星注射液的测定，相     

哌仑西平的单扫描示波极谱法测定

本报道一种测定哌仑西平的单扫描示波极谱法，在０．１ｍｏｌ／ＬＮＨ４Ｃｌ－ＮＨ３．Ｈ２Ｏ（ｐＨ８．０±０．１）缓冲液中，哌仑西平有一极谱还原波，其峰电位为－１．５１Ｖ（ｖｓ．ＳＣＥ），其一阶导数峰高与哌仑西闰浓度在６．６×１０＾－７－４．６×１０＾－６ｍｏｌ／Ｌ（ｒ＝０．９９８１）和６．６×１０＾－６－１．６×１０＾－５ｍｏｌ／Ｌ（ｒ＝０．９９９１）范围内有线性关系，检测限为３．４×１０－７ｍｏｌ     

全固定化试剂流动注射化学发光测定铜

采用离子交换固定法把Ｌｕｍｉｎｏｌ（Ｌｕ），ＣＮ＾－固定在阴离子交换树脂上，串入流动注射系统中，当一定量洗脱剂被注入阴离子交换柱时，洗脱下来的Ｌｕ和ＣＮ＾－与分析物Ｃｕ＾２＋发生化学反应，产生化学发光，实现对Ｃｕ＾２＋的在线检测。本法检出限为１．３×１０＾－９ｇ／ｍＬ，线性范围为４．０×１０＾－９－６．０×１０＾－６ｇ／ｍＬ，ＲＳＤ为３．４％，单次测定在１ｍｉｎ内能完成。已用于井水中铜的测定，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.

     

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。