Gd_xY_（1－x）P_5O_（14）：Ce，Tb的发光和能量传递Ⅱ．Ce→

研究了Ｇｄ＿ｘＹ＿（１－ｘ）Ｐ＿５Ｏ＿（１４）：Ｃｅ＿（０．０１），Ｔｂ＿（０．０２）体系中Ｇｄ的子晶格在Ｃｅ→Ｇｄ→Ｔｂ能量传递中的中介作用规律及ＧｄＰ＿５Ｏ＿（１４），ＧｄＰ＿５Ｏ＿（１４）：Ｃｅ，ＧｄＰ＿５Ｏ＿（１４）：Ｔｂ和Ｇｄ＿ｘＹ＿（１－ｘ）Ｐ＿５Ｏ＿（１４）：Ｃｅ，Ｔｂ的荧光光谱、激发光谱。结果表明，当ｘ＞０．７时，结构从单斜Ⅱ（Ｃ２／ｃ）的层状结构变为单斜Ｉ（Ｐ２＿１／ｃ）的带状结构，Ｃｅ￣（３＋）的发射光谱和Ｇｄ￣（３＋）的吸收光谱交迭增加等是Ｃｅ￣（３＋）→Ｇｄ￣（３＋）→Ｔｂ￣（３＋）能量传递几率增加的主要原因。     

两个环己烷螺含氮杂环化合物的合成和晶体结构

环己酮与硫代碳酰肼在不同介质中的反应，合成出两个不同的环己烷螺含氮杂环化合物。经Ｘ－射线结构分析确定它们分别为１，２，４，５－四氮螺［５，５］十一烷－３－硫酮，Ｃ＿７Ｈ＿（１４）Ｎ＿４Ｓ（Ⅰ）和１，２，４，－三氮螺［４，５］癸－１－烯－４－氨基－３－硫酮。Ｃ＿７Ｈ＿（１２）Ｎ＿４Ｓ＿ｘ（Ｓ＿ｘ＝０．８Ｓ＋０．２Ｏ）（Ⅱ）。晶体学参数分别为（Ⅰ）：Ｐ２＿１／ｃ，ａ＝１２．０２６（４），ｂ＝２６．８１７（６），ｃ＝１２．０４２（３），β＝１１５．９４（２）°，Ｚ＝４，Ｖ＝９３３．４（１０），Ｍ＿ｒ＝１８６．２８；（Ⅱ）：Ｐ２＿１／ｍ，ａ＝６．５９５（７），ｂ＝６．８１７（６），ｃ＝１０．５７２（６），β＝１０６．３（１）°，Ｖ＝４５６（１），Ｚ＝２，Ｍ＿ｒ＝１８１．０５。最终一致因子分别为Ｒ＝０．０５４，Ｒ＿ｗ＝０．０６５和Ｒ＝０．０８９，Ｒ＿ｗ＝０．０９６。两个化合物中，环己烷都为椅式构型，它与其螺联的６员氮杂环，５员氮杂环的最小二乘平面间的夹角分别为６８．９４和９０°。并对合成反应途径作了初步讨论。     

Na－Ca－Ba－RE氟碳酸盐系列矿物的两个新变种

Ｃａ氟碳钡铱矿富Ｓｒ变种和白云鄂博矿富Ｃａ变种分别产于俄罗斯科拉半岛希宾碱性岩体的碳酸盐和内蒙古白云鄂博钥铁稀土矿床碳酸盐脉石中。据电子探针分析得到的晶体化学式分别为：（Ｃ３＿（０．４６），Ｎａ＿（０．２８），□＿（０．１６））＿（０．９０）Ｂａ＿（１．０３）（Ｃｅ＿（０．８２），Ｓｒ＿（０．３８），Ｌａ＿（０．３５），Ｎｄ＿（０．３２），Ｐｒ＿（０．０９），Ｓｍ＿（０．０１））＿（１．９７）（ＣＯ＿３）＿４Ｆ和（Ｎａ＿（０．４４），Ｃａ＿（０．３２），□＿（０．２４））＿（１．００）Ｂａ＿（１．０７）（Ｃｅ＿（１．０３），Ｌａ＿（０．４６），Ｎｄ＿（０．２６），Ｐｒ＿（０．０８），Ｓｒ＿（０．０８），Ｓｍ＿（０．０２））＿（１．９３）（ＣＯ＿３）＿４Ｆ。由Ｘ射线方法测定的晶胞参数分别是：ａ＝０．５０９１，ｃ＝２．３０２ｎｍ和ａ＝０．５１１０，ｃ＝０．３３３ｎｍ。二者是Ｃａ氟碳钡铈矿（Ｃａ＿（０．５），□＿（０．５））ＢａＣｅ＿２（ＣＯ＿３）＿４Ｆ和白云鄂博矿ＮａＢａＣｅ＿２（ＣＯ＿３）＿４Ｆ类质同象系列的中间成员。基于白云鄂博矿晶体结构中离子半径的分析和键价的计算，表明Ｃａ＿￣（２＋）优先占据Ｎａ位，而Ｓ     

用高效液相色谱法测定热应激时大鼠肺及肝组织中细胞膜磷脂的变化

应用高效液相色谱法（ＨＰＬＣ）测定了正常大鼠肺及肝组织中细胞膜磷脂的含量及热应激时膜磷脂的含量变化。流动相为甲醇∶乙腈∶８５％磷酸（３∶１００∶１，Ｖ／Ｖ／Ｖ），色谱柱为μ－Ｐｏｒａｓｉｌ柱（３．９ｍｍｉ．ｄ．×３００ｍｍ）。通过测定膜磷脂的变化，可以为阐明机体的发病机理提供可靠的数据     

高效液相色谱法测定人血浆中甲磺酸培氟沙星浓度

建立了一种测定人血浆中甲磺酸培氟沙星的匠相液相色谱方法,用的是ＺｏｒｂａｘＯＤＳＣ＿（１８）柱和用三乙醇胺调节成ｐＨ为３．０的甲醇－０．０４ｍｏｌ／ＬＨ＿３ＰＯ＿４溶液（８０：２０,Ｖ／Ｖ）的流动相,检测在２７６ｎｍ处进行,流量为１ｍＬ／ｍｉｎ,线性范围是６．０１×１０￣（－８）～３．０１×１０￣（－５）ｍｏｌ／Ｌ（γ＝０．９９９８）,检测极限为６．０１×１０￣（－８）ｍｏｌ／Ｌ,平均回收率为９７．５７±３．０４％,日内与日间的ＣＶ分别为３．２９％和５．０８％。     

用高效液相色谱法测定热应激时大鼠肺及肝组织中细胞膜磷脂的变化

 应用高效液相色谱法（ＨＰＬＣ）测定了正常大鼠肺及肝组织中细胞膜磷脂的含量及热应激时膜磷脂的含量变化。流动相为甲醇∶乙腈∶８５％磷酸（３∶１００∶１，Ｖ／Ｖ／Ｖ），色谱柱为μ－Ｐｏｒａｓｉｌ柱（３．９ｍｍｉ．ｄ．×３００ｍｍ）。通过测定膜磷脂的变化，可以为阐明机体的发病机理提供可靠的数据。     

ICP－AES直接测定荧光级氧化铕中5个稀土杂质

本文采用ＪｏｂｉｎＹｖｏｎ３８Ⅱ光谱仪直接测定高纯氧化铕中Ｃｓ、Ｐｒ、Ｓｍ、Ｇａ、Ｄｙ５个稀土杂质，试验考查了氧化铕基体，共存元素，酸度等因素的影响。利用正文试验Ｌ＿（２５）（５）￣６确定了仪器最佳条件。当基体纯度为９９．９９％时；回收率在９４．０～１０８．０％之间。在实际应用中获得满意的结果。     

色谱法研究胃肠外营养中脂肪酸乳剂对大鼠多不饱和脂肪酸代谢的影响

运用色谱法测定了红细胞膜磷脂脂肪酸的组成。首先用双向薄层色谱分析法分离和提纯膜中的类脂,然后运用毛细管气相色谱法分析其中的组分。类脂中加入Ｇ_（１７：０）作内标,硫酸－甲醇液进行甲酯化处理后,上样测试。在３５０ｍｇ／Ｌ到８００ｍｇ／Ｌ的范围内线性关系良好,相关系数均大于０．９９。方法具有稳定性好、灵敏度高、重复性好、操作相对简便的特点,在研究胃肠外营养中脂肪酸乳剂对大鼠多不饱和脂肪酸代谢的影响中,取得了较好的效果。     

甲烷直接氧化制甲醇Ⅱ．催化膜反应器（CMR）

采用溶胶－凝胶（Ｓｏｌ－Ｇｅｌ）法制备了微孔结构均匀的“ＳｉＯ＿２／陶瓷”膜和“Ｍｏ－Ｃｏ－·Ｏ／ＳｉＯ＿２／陶瓷”催化功能膜，并用ＸＲＤ、ＳＥＭ和孔径测定等技术进行了表征。在常压、５００～７００℃的条件下，在催化膜反应器（ＣＭＲ）中考察了甲烷氧化制甲醇的反应。在相似的反应条件下（转化率为１．０％），用ＣＭＲ（甲醇选择性１１．２％）可获得较固定床反应器（甲醇选择性４．５％）高得多的甲醇选择性。     

荧光法测定水样中的硒(Ⅳ)、硒(Ⅵ)和有机硒

本文提出了水样中硒（Ⅳ）、硒（Ⅵ）和有机硒的荧光测定方法。基于酸性介质中２,３－二氨基萘与硒（Ⅳ）的选择性反应,直接测定硒（Ⅳ）;利用盐酸还原硒（Ⅵ）和ＨＮＯ３－ＨＣｌＯ４消化有机硒后,用差减法分别测出硒（Ⅵ）和有机硒。检出限０．０７μｇ／Ｌ,线性范围０～１０μｇ／Ｌ。硒（Ⅳ）、硒（Ⅵ）和有机硒的相对标准偏差与回收率分别为２．４％和９８．５％～１０１．５％、３．１％和９４．８％～１０３％、４．０％和９４．５％～９８．８％。     

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。