低锑砷合金中微量元素的测定

研究了火焰原子吸收光谱法测定低锑砷合金中微量元素含量的最佳测量条件,包括燃助比,燃烧器高度,灯电流,光谱通带以及基体元素对测定的影响,实验表明,在选定实验条件下,Cu,Ag元素欲望在0－4mg/L,Sb元素含量在0－80mg/L范围内均符合比尔定律,相关系数（r)为0．9979－0．9987,方法简便,快速,选择性好,该法用于低锑砷合金中微量元素Cu,Ag,Sb的测定,结果令人满意,方法的回收率为91－97％。相对标准偏差为1．1％－2．4％。     

CsCuHPVAsMoO杂多化合物对异丁烯选择性氧化反应的催化性能

 用组合法合成了CsCuHPVAsMoO系列杂多化合物催化剂，并采用FT－IR，H2－TPR，NH3－TPD和TG－DTA等方法对催化剂进行了表征．在自制固定床反应器中对异丁烯进行选择性氧化，考察了Cs，Cu和As含量、催化剂焙烧温度及反应条件对催化剂催化性能的影响．结果表明，Cs的引入有利于提高催化剂的选择性；Cu和As的引入在提高催化剂活性的同时，也提高了催化剂的选择性；当焙烧温度为340℃时，催化剂的活性和选择性最高．组成为Cs0．1Cu0．2HxPVAs0．2Mo10Oy的催化剂对异丁烯具有很强的选择性氧化能力，在最佳反应条件下，甲基丙烯酸、甲基丙烯醛和乙酸的收率分别可达52．84％，12．05％和18．21％．     

毛细管气相色谱法测定炼厂气中单体烃组分的含量

采用PLOT／Al2O3石英毛细管气相色谱柱和氢火焰离子化检测器，建立了炼厂气中单体烃组分含量测定的毛细管气相色谱法，当炼厂气中单体烃组分的含量大于或等于2．1％时，RSD≤0．95％，当炼厂气中单体烃组分的含量为0．5％－2．1％时，RSD为0．95％－10．0％，当炼厂气中单体烃组分的含量为0．2％－0．5％时，RSD为10．0％－25．0％，该方法对单体烃组分的测定结果与行业标准SH／T0230－92《液化石油气组成测定法》的测定结果基本一致。     

荧光猝灭法测定痕量六价铬

基于六价铬与碘化钾反应生产了单质碘，碘可以使2′，7′－二氯荧光素（DCF）发生荧光猝来，从而间接测定六价铬。六价铬浓度在0．20－2．50μg/25ml范围内，荧光强度差值与六价铬浓度呈线性关系，线性回归方程△F=12．12 0．19，相关系数r=0.9993，检出限为0．10μg/ml。方法简便，灵敏度较高，已用于合成样中六价铬的测定。回收率在100％－103％，结果满意。     

微波消解—原子荧光光谱法定量测定山梨糖醇液中的砷

应用微波消解技术和原子荧光光谱仪以氢化物发生原子荧光光谱法测定了山梨糖醇液中砷的研究。对微波消解条件以及氢化物发生条件进行了探讨。在选定的最佳条件下方法的检出限为0．22ng/mL,线性范围为0－80ng/mL。10次测定的相对标准偏差为0．49％－2．16％,回收率为94．8％－102．2％。该结果与国际推荐的湿法消解分析结果相对照,无显著性差异。     

龙津街婴儿辅食添加与微量元素含量的关系

为了解荔湾区龙津街婴儿辅食添加时间及结构对其体内微量元素含量有无影响，减少微量元素失衡对婴儿生长发育的影响，采用分层抽样方法对龙津街内进行“4－2－1”体检的398名3－12个月散居婴儿进行辅食添加情况了解，同时检测其头发中碘，锌，铁，钙，铜，锰的含量。用x^2求得两者关系P＜0．01，P＜0．05，表明辅食添加的时间正常与否，添加辅食结构是否合理对其头发中微量元素含量有密切关系。科学地进行辅食添加对平衡婴儿体内微量元素含量，促进其健康生长有重要意义。     

氧氟沙星在胶束体系中的荧光特性及应用

研究发现十二烷基硫酸钠胶束对氧氟沙星荧光有明显的增敏作用，据此建立了直接测定人体尿液中氧氟沙星的等波长差同步荧光光谱法（△λ=90nm）。经样品测定，其线性范围为0．12－3．6mg/L，检出限为0．12mg/L，回收率为92．2％－97．8％，相对标准偏差为1．2％－2．7％。     

六苄基六氮杂异伍兹烷的氧化反应性

研究了2，4，6，8，10，12－六苄基－2，4，6，8，10，12－六氮杂四环[5．5．0．0^5,9．0^3.11]十二烷在多种氧化条件下的氧化反应性，得到了一系列新的六氮杂异伍兹烷衍生物，并利用两步法以较高的收率得到期望的化合物六苯甲酰基六氮杂异伍兹烷。     

痕量铁的催化分光光度法研究

研究了在S2SO4介质中，以1，10－二氮菲为活化剂，铁（Ⅲ）催化过氧化氢氧化甲基橙的褪色反应的动力学条件。建立了测定痕量铁（Ⅲ）的动力学分析法。方法的灵敏度1．78×10－8g·L－1，线性范围0～1．2×10－5g·L-1。用于测定饮用水和湖水中的痕量钱，相对标准差在5％以内，平均回收率97％～106％。     

高效液相色谱法测定蜜蜂蜂体王浆酸

建立了蜂体中10－HDA的高效液相色谱分析方法。对10－HDA的提取方法进行了研究。在选择的最佳色谱条件下,线性范围为10～1000ng,r=0．9998,回收率96．5％～99．2％,检测限为0.53μg／g。     

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.     

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.

     

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。     

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.     

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。     

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.     

解决能源问题的新途径——光解水制氢的研究

面对日益枯竭的能源危机,氢能是一种洁净、最有前景的替代能源。目前在各种制氢的方法中光催化分解水制氢的研究最多,光解水过程中催化剂最关键,本文对利用太阳能光解水的途径、提高光催化反应效率以及光催化剂的开发研究进行了综述。     

黄酮化合物的合成研究进展

黄酮化合物是一类具有多种生物活性的天然产物,其经典的合成方法主要为查耳酮路线和β-丙二酮路线.近年来出现了许多新技术、新方法.本文介绍了2'-羟基查尔酮的氧化关环法、黄烷酮氧化法、改进的Baker-Venkataraman法及其他合成黄酮化合物的方法.