反相离子对色谱法测定硫代硫酸根和碘离子的研究

首次利用Ｓ２Ｏ２－３和Ｉ－与Ｈｇ－ＥＤＴＡ二元络合物通过柱前衍生形成ＥＤＴＡ－Ｈｇ－Ｓ２Ｏ３和ＥＤＴＡ－Ｈｇ－Ｉ两种三元络合物的方法,实现了对Ｓ２Ｏ２－３和Ｉ－的间接反相离子对色谱分离和紫外检测。在ＺｏｒｂａｘＯＤＳ柱上,用甲醇∶水＝２３∶７７作流动相,内含对离子ＴＢＡ＋３．０ｍｍｏｌ／Ｌ,ＥＤＴＡ１．０ｍｍｏｌ／Ｌ,ＮａＮＯ３２．０ｍｍｏｌ／Ｌ和缓冲剂ＫＨ２ＰＯ４－Ｎａ２ＨＰＯ４（ｐＨ７．０）,紫外２５４ｎｍ检测。Ｓ２Ｏ２－３和Ｉ－的最小检出限分别为６１．１ｎｇ和３７．６ｎｇ。方法简便,选择性好。     

大口径毛细管气相色谱法测定腈纶布料中残留的二甲基甲酰胺

提出了测定腈纶布料中残留的二甲基甲基甲酰胺的大口径毛细管气相色谱分析方法。检测范围为０￣５０ｍｇ／Ｌ,检测限为２μｇ／Ｌ,回收率为９０．０－９７．５％,ＲＳＤ〈４．６％。     

胶束毛细管电泳法测定牡丹皮及芍药中牡丹酚和芍药甙

用胶束毛细管电泳地（ＭＥＣＣ）测定牡丹皮、白芍、赤芍及其不同炮制品的牡丹酚、芍药甙的含量,以３０ｍｍｏｌ／Ｌ磷酸盐缓冲溶液（ＮａＨ２ＰＯ４－Ｎａ２ＨＰＯ４）中含２０ｍｍｏｌ／Ｌ十二烷基硫酸钠（ＳＤＳ）的表面活性剂电解质,ＰＨ＝６．８５,于２５４ｎｍ紫外检测,实验结果线性关系良好。塔数达到４．６×１０＾４。     

单糖的高效毛细管区带电泳定量分析

生物体中常见的９种单糖经α－萘胺衍生化后，用５０ｍｍｏｌ／Ｌ硼砂作为电泳介质，实现了高效毛细管电泳分离，并以β－吲哚乙酸为内标，研究了９种单糖毛细管电泳的定量方法，结果表明浓度在０．２～４．０ｍｍｏｌ／Ｌ范围内呈良好的线性。６次进样的标准偏差小于±３％。     

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％。     

毛细管区带电泳法测定甲氧苄胺嘧啶和磺胺甲基异恶唑的离解常数 …

报道了利用３０ｍｍｏｌ／ＬＨＡｃ－ＮａＡｃ为缓冲液测定复方新诺明中甲氧苄胺嘧啶和磺胺甲基异恶唑的离解常数及含量的毛细管区带电泳方法。该方法具有简便、快速、准确等特点。测定ＴＭＰ和ＳＭＺ的ＰＫａ分别为６．６０和５．９０。其平均回收率分别为１０１．５％和９９．６％最低检出限为０．４８ｍｇ／Ｌ和０．０２８ｍｇ／Ｌ,ＲＳＤ为１．２６％和１．１２％。     

高效毛细管电泳—电化学法检测烟酰胺腺嘌呤二核苷酸

报道了一种测定烟酰胺腺嘌呤二核苷酸的毛细管电泳电化学检测方法。采用３０ｃｍ×２５μｍ的石英毛细管分离ＮＡＤＨ与脲酸，以微型碳糊电极测定经分离后的ＮＡＤＨ的含量。在ｐＨ７．５的磷酸盐缓冲溶液中，标准工作曲线的范围为１．０－１００μｍｏｌ／Ｌ；最代检测浓度为０．６０μｍｏｌ／Ｌ。     

高效液相色谱法测定小鼠脑组织单胺递质及其相关化合物

采用苯基柱等度洗脱分离,自然荧光检测法,直接测定小鼠脑组织匀浆中单胺递质及其相关化合物。优化出了最佳色谱条件,流动相为２０ｍｍｏｌ／Ｌ柠檬酸三钠（ｐＨ４．５０）－甲醇（９５：５,Ｖ／Ｖ）;柱温为３５℃。该方法能同时检测８种化合物。最低检测限为１．０－２．５μｇ／Ｌ,回收率均在９３５以上;线性范围为１．０μｇ／Ｌ－１．０ｍｇ／Ｌ。     

用气相色谱-原子发射光谱法检测VX、Bz及其降解产物

应用气相色谱－原子发射光谱（ＧＣ－ＡＥＤ）同时检测Ｓ－（２－二异丙基氨乙基）甲基硫直膦酸乙酯（ＶＸ）、二苯羟乙酸－３－喹咛环酯（ＢＺ）战剂及其降解产物等５种化合物,得取了Ｃ、Ｈ、Ｓ、Ｎ、Ｏ、Ｐ６种元素色谱图,通过选择合适的检测元素,其检出限ＶＸ为１５．６ｍｇ／Ｌ,Ｂｚ为１６．７９ｍｇ／Ｌ,二异基氨基乙太醇为３．０２ｍｇ／Ｌ,３－羟基喹咛为２８．４０ｍｇ／Ｌ,二苯羟乙酸甲酯为３１．７８ｍｇ／Ｌ,定量     

5,10,15,20—四（3—溴—4—磺酸苯基）卟啉高效液相色谱法测定河水中微量…

研究了新合成的显色剂５，１０，１５，２０－四（３－溴－４－磺酸苯基）卟啉与Ｃｏ（Ⅱ）、Ｚｎ（Ⅱ）、Ｃｕ（Ⅱ）形成配合物离子的反应，在ＺＯＲＢＡＸ ＯＤＳ柱上，用含２０ｍｍｏｌ／Ｌ乙酸－乙酸钠（ｐＨ６．０）和１０ｍｍｏｌ／Ｌ四乙基碘化铵的乙腈－水（２７：７３，Ｖ／Ｖ）流动相洗脱，在４２０ｎｍ波长下检测。Ｃｏ（Ⅱ）、Ｚｎ（Ⅱ）、Ｃｕ（Ⅱ）螯合物在９ｍｉｎ内获得完全分离，检测限分别为０．２ｎｇ，０．０５     

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。