流动注射在线萃取—石墨炉原子吸收光谱法测定地质样品痕量钯

应用流动注射在线萃取技术将ＰｄＣｌ＾２－６萃入２－巯基苯并噻唑－甲基异丁基酮直接进行石墨炉原子吸收测定。研究了流动注射在线萃取－石墨炉原子吸收光谱法测定地质样品中钯的实验条件、流路参数等。采样速率为２０样／ｈ,ＲＳＤ（ｎ＝１０）为４．８％,测定Ｐｄ的特征质量为２．６＊１０＾－１１。     

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。     

GFAAS法测定天然饮用矿泉水中的钼

本文介绍了石墨炉原子吸收光谱法测定天然饮用矿泉水中的钼。水样不需浓缩萃取直接测定。线性范围０．０２～１．６ｎｇ，检测限０．０１ｎｇ，相对标准偏差２．３％－４．５％，回收率９６％－１０３％。     

平台石墨炉原子吸收法测定高温镍基合金中砷

研究了基体改进剂，灰化，原子化温度和共存元素的干扰。采用钯作基体改进剂和匹配基体镍后，提高了灵敏度，增强了抗干扰能力。在波长１９７．２ｎｍ处，用平台石墨炉原子吸收法直接测定了高温镍基合金中砷。方法特征是为８８ｐｇ，检出限为０．２７μｇ．ｇ＾－１，相对标准偏差为３．１％－５．１％，回嵋率为８５％－１００％。     

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     

硫脲型树脂富集—石墨炉原子吸收光谱测定地质水中痕量金

本文研究了硫脲型树脂对金的吸附条件，提出了以水文地球化学探矿为目的现场富集，石墨炉原子吸收光谱测定地质水中痕量金的方法，实验表明：该树脂在［Ｈ＾＋］＞０．２ｍｏｌ／Ｌ的较宽酸度范围内，在最大流速情况下对天然水中痕量金进行富集，测得回收率达９８％以上，大部分共存离子不影响金的富集与测定，方法的检出限为０．０５ｎｇ／Ｌ。     

石墨炉原子吸收法测定聚苯乙烯泡沫塑料中的汞

本文提出的在聚苯乙烯泡沫塑料中测定汞的方法是将样品溶解在苯中，以Ｎａ２Ｓ２Ｏ３溶液反洗出汞，利用反洗液中Ｎａ２Ｓ２Ｏ３作基体改进剂，石墨炉原子吸收法测定汞，方法简便，快速，特征量为８０ｐｇ／０．００４４Ａ。本法分析样品与冷原子荧光法的结果一致，相对标准偏差≤８％，回收率９２％－１０２％。     

石墨炉原子吸收光谱法测定血铅的干扰校正

研究了用石墨炉原子吸收光谱法测定血铅的干扰校正方法。通过对测定过程中的干扰研究，建立了一种数学校正干扰的标准加入法基体匹配工作曲线。用本法分析健康儿童血铅及脐带血铅，线性范围为０￣９０ｎｇ／Ｌ，相关系数为０．９９９７，灵敏度为８．６ｐｇ／１％信号，检出限为４．８ｐｇ，与一般标准加入法工作曲线相比较，测定血铅线性斜率大，灵敏度高，准确性好。     

流动注射—氢化物—石墨炉原子吸收光谱法应用研究

本文采用自制的氢化物－石墨炉自动进样器及流动注射仪，直接测定了一些环境试样中的痕量锗，并研究了测定条件，该方法灵敏度高，线性范围宽，操作简单，速度快，耗样量少。特征质量：５．７ｐｇ／０．００４４Ａ；检出限：１．３ｐｇ，测定速度：３０个样／ｈ；回收率：９９．５％－１０４％。     

化学修饰石墨探针预富集—石墨炉原子吸收法测定Cr（Ⅵ）和Cr（Ⅲ）

本将化学修饰石墨探针选择性预分离富集和石墨炉探针原子化学测定的高灵敏度结合起来，建立了用ＴＯＰＯ修饰的石墨探针络合富集Ｃｒ（Ⅵ），Ｎａｆｉｏｎ修饰的石墨探针交换富集Ｃｒ（Ⅲ）的双饰石墨探针顺序分富集，石墨炉探针原子化法测定水体中Ｃｒ（Ⅵ）和Ｃｒ（Ⅲ）的方法。Ｃｒ（Ⅲ）的检出限为１．０３ｎｇ／ｍＬ，线性范围为０－５１ｎｇ／ｍＬ。Ｃｒ（Ⅵ）的检出限为０．３７ｎｇ／ｍＬ，线性范围为０－８１ｎｇ／ｍＬ。     

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。