铜（铅）—Ferron—氯化四苯胂络合物吸附波研究

在ＨＣｌ－六次甲基四胺介质中，铜（铅）－Ｆｅｒｒｏｎ－氯化四苯胂络合物产生灵敏的络合吸附波。峰电位分别为－０．４１Ｖ和－０．５７Ｖ。峰电流与铜、铜浓度分别在０．０００４－０．４μｇ／ｍＬ和０．００２－０．８μｇ／ｍＬ之间呈线性关系，检出限分别为０．０００２μｇ／ｍＬＣｕ和０．００１μｇ／ｍＬＰｂ。研究了极谱波的性质和电极反应机理。用拟定的方法连续测定水样和食品中的铜、铜，结果满意。     

铜（铅）－Ferron－氯化四苯胂络合物吸附波研究

在ＨＣｌ￣（－）六次甲基四胺介质（ｐＨ４．６２）中，铜（铅）－Ｆｅｒｒｏｎ氯化四苯胂络合物产生灵敏的络合吸附波。峰电位分别为－１．４１Ｖ和－０．５７Ｖ（Ｕｓ．ＳＣＥ）。峰电流与铜、铅浓度分别在０．０００４～０．４μｇ／ｍＬ和０．００２～０．８μｇ／ｍＬ之间呈线性关系，检出限分别为０．０００２μｇ／ｍＬＣｕ和０．００１μｇ／ｍＬＰｂ。研究了极谱波的性质和电极反应机理。用拟定的方法连续测定水样和食品中的铜、铅，结果满意。     

氯化三辛基甲基胺萃取原子吸收法测定微量锑的研究

本文在ＫＩ－Ｈ２ＳＯ４体系中，研究了锑的碘络阴离子的萃取行为，并结合火焰原子吸收法测定了微量锑，萃取体积比（Ｖ水／Ｖ有）为２０，线性范围为０－２μｇ／ｍｌ，锑的特征浓度为０．５μｇ／ｍｌ／１％吸收，检出限为０．１μｇ／ｍｌ。     

流动注射－化学发光分析测定矿石中痕量铌

利用铌对鲁米诺－Ｈ_２Ｏ_２－Ｋ_３Ｆｅ（ＣＮ）_６化学发光体系的抑制作用，建立了痕量Ｎｂ（Ｖ）的流动注射－化学发光测定法。方法的检出限是２．３ｎｇ／ｍＬＮｂ（Ｖ）。线性范围为０．０１～１μｇ／ｍＬＮｂ（Ｖ），测定的相对标准偏差为３．０％（０．０１μｇ／ｍＬＮｂ（Ｖ）（ｎ＝１１），方法已应用于矿石中Ｎｂ的测定。     

单扫描极谱法连续测定人发中的微量元素锌铁锰铜

本提出在０．１５ｍｏｌ／Ｌ乙二胺－７．５×１０＾－３ｍｏｌ／Ｌ三乙醇胺－２．５×１０＾－２ｍｏｌ／Ｌ硫氰酸钾底液中单扫描极谱法测定锌、铁、锰，续加硫酸（０．３ｍｏｌ／Ｌ）测定铜的方法，峰电位分别为－１．４２Ｖ，－１．６３Ｖ，－１．７１Ｖ，－０．４８Ｖ（ｖｓ．ＳＣＥ），线性范围：０．０５～１．４μｇ／ｍＬＭｎ，０．０４～１μｇ／ｍＬＣｕ，最低检出浓度．０３，０．０５，０．０２，０．０４μｇ／ｍＬＭ     

铜—2,3,4—三羟基—4‘—磺基—偶氮苯配合物吸附波的研究

在０．０６５ｍｏｌ．Ｌ＾－１柠檬酸钠－０．０４６ｍｏｌ．Ｌ＾１ＨＣｌ（ｐＨ６．６）介质中，２，３，４－三羟基－４’－磺基－偶氮苯和铜形成配合物，在单扫描示波极谱仪上于－０．２Ｖ处产生灵敏的吸附峰，测定铜的浓度范围为０．００５－０．３μｇ．ｍｌ＾－１，检出限为０．００２５μｇ．ｍｌ＾－１，本法已成功地用于人发及硫酸镍中铜的测定，并进行了电极反应机理研究。     

阻抑褪色光度法测定痕量汞

提出一种测定痕量汞的新的光度法。该法基于Ｈｇ（Ⅱ）对Ｈ２Ｏ２与离子缔合物ＡｇＣｌ·ＰＶＡ·Ａｇ~＋·Ｆｉｎ~－褪色反应的抑制效应,该离子缔合物对应于聚乙烯醇存在下Ｆａｊａｎｓ（法扬斯）法的终点,线性回归方程△Ａ＝０．０２＋ ４．０×１０~（－３）Ｃ_（Ｈｇ（Ⅲ））（μｇ／Ｌ）,相关系数ｒ＝０．９９９２,Ｈｇ（Ⅱ）浓度在４．０～２０．０μｇ／Ｌ范围内服从比耳定律,检出限０．０４μｇ／Ｌ。该法用于废水样中Ｈｇ（Ⅱ）的测定,结果与双硫腙法结果相符。     

1-(2-噻唑偶氮)-2-萘酚螯合物反相高效液相色谱法分离测定铜(Ⅱ)、铁(Ⅱ)和镍(Ⅱ)

以１－（２－噻唑偶氮）－２－萘酚（ＴＡＮ）作柱前显色剂，于ＯＤＳ柱上，用内含０．１ｍｏｌ／ＬＬｉＣｌ，５×１０－６ｍｏｌ／Ｌ ＴＡＮ和ＨＡｃ－ＮＨ４Ａｃ缓冲溶液（ｐＨ ５．５）的甲醇－水溶液（８０：２０，Ｖ／Ｖ）作流动相，流速为０．６ｍＬ／ｍｉｎ，并以紫外－可见检测器于５９０ｎｍ处进行检测，发展了一种ＲＰ－ＨＰＬＣ法同时分离测定铜（Ⅱ）、铁（Ⅱ）、镍（Ⅱ）的方法，方法灵敏度高，对于铜、铁、镍的检测限分别为１μｇ／Ｌ， ２ μｇ／Ｌ和 ０．４ μｇ／Ｌ。用于实际样品测定，结果满意。     

饮料食品中Ge－132和Ge~（4＋）含量测定研究

本文报告了在０．０１ｍｏｌ／ＬＣＴＡＢ体系中，以Ｆ－为掩蔽剂、苯芴酮显色、用分光光度法测定饮料食品中Ｇｅ－１３２含量，最低检测限０．０５４μｇ／ｍＬ；线性范围０．５４～２７．１４μｇ／ｍＬ；回收率９６．３％～１０１．５％，并确定了Ｇｅ－１３２摩尔吸收系数（ε）３．３９×１０４。用本法测定了康寿茶、矿泉水和博士奶中Ｇｅ－１３２含量，灵敏度高、重现性和准确度好。用盐酸化本体系，研究了二氧化锗（Ｇｅ~（４＋））的含量测定，其最低检测限０．０２１μｇ／ｍＬ；线性范围１．０～２１．０μｇ／ｍｌ；回收率９５．８％～１０２．８％，Ｇｅ－１３２不干扰。饮料食品中同时存在Ｇｅ－１３２和Ｇｅ（４＋）时，本体系可分别测定两者含量。     

极谱法快速同时测定锌电解液中微量铜、镉、钴

铜、镉、钻在了丁二酮肟－氯化铵－柠檬酸钠－ＨＡｃ－ＮａＡｃ体系中有灵敏的极谱波。其峰电位分别为－０．２４Ｖ、－ ０．７９Ｖ和－０．９３Ｖ,线性范围分别为４ × １０~（－６）～ ４ × １０~（－３）、５ × １０~（－６）～ ５×１０~（－３）、１×１０~（－７）～１×１０~（－４）ｇ／Ｌ,检测限分别为２×１０~（－６）、４ × １０~（－６）和５×１０~（－８）ｇ／Ｌ。方法无需预处理直接用于锌电解液中微量铜、镉、钴的测定,结果令人满意。     

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.     

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.     

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。     

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.     

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.

     

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。     

Investigation of Kinetics of Solid-Phase Synthesis of Lithium Orthosilicate

The kinetics of the interaction between lithium carbonate and silica with various degrees of dispersion was investigated by TG and DTA methods. It was found that the utilization of pyrogenic silica with a specific surface area of about 300 m²g^-1 instead of aerosil with one of 175 m²g^-1 leads to an increase of the reaction rate between lithium carbonate and silica, which depends on the formation and growth of lithium orthosilicate crystals in the first stage, and is conditioned by the diffusion of lithium and oxygen ions through the lithium orthosilicate layer formed at temperatures above 800 K. This supposition is supported by the kinetic analysis results obtained with the use of the different models. The optimal regime of heating is recommended. This revised version was published online in July 2006 with corrections to the Cover Date.     

小环化合物中饱和碳质子化学位移的计算

小环化合物由于其张力、构型、构象和各向异性效应等原因,环碳上质子化学位移缺乏规律性,难以预测,对此作者曾提出一种近似算法。本文根据303种小环化合物中饱和碳质子的化学位移实验数据,将适于计算这类质子化学位移的公式表述为:     

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。