在国产近红外光谱仪实验样机上用偏最小二乘法定量分析大麦成分

采用偏最小二乘法和国产近红外光谱分析仪实验样机，对大麦中的蛋白质和淀粉含量进行了定量测定．测定结果为：对蛋白质和淀粉预测的相关系数分别为０．９６１、０．９４９，相对标准偏差分别为２．７％、２．９％，相对误差分别小于５．７％、６．８％．     

烷基醇聚氧乙烯醚中二噁烷的测定

采用顶空气相色谱法测定了烷基醇聚氧乙烯醚中的二口恶烷。研究了顶空条件，标准曲线的相关系数为０．９９８９，检出限为２０μｇ／Ｌ，回收率为９１．６％～９７．６％，相对标准偏差小于２．５％。     

反相合并带流动注射分析法测定维生素C的含量

采用流动注射反相合并带技术，在乙酸介质中，维生素Ｃ与过量的Ｉ３反应，剩余的Ｉ３在３５０ｎｍ处由检测器检出，信号强度△Ａ与维生素Ｃ含量在０～５．０×１０＾－５ｍｏｌ．Ｌ＾－１范围内呈良好的线性关系，相关系数ｒ＝０．９９９５，相对标准偏差ＲＳＤ＝０．４％（ｎ＝１１），采样频率为７０次次／ｈ。     

烷基醇聚氧乙烯醚中二噁烷的测定

 采用顶空气相色谱法测定了烷基醇聚氧乙烯醚中的二口恶烷。研究了顶空条件，标准曲线的相关系数为０．９９８９，检出限为２０μｇ／Ｌ，回收率为９１．６％～９７．６％，相对标准偏差小于２．５％。     

HPLC法快速测定峰皇浆及制品中添加的维生素B6

本文研究了快速、简便测定蜂皇浆及制品中添加的低含量维生素Ｂ_６的ＨＰＬＣ法。称取适量样品，用１０％偏磷酸提取、净化，清液供ＨＰＬＣ分析用。ＷＡＴＥＲＳ荧光检测器，激发波长２９０ｎｍ，发射波长３９０ｎｍ，ＶＢ_６含量在０～１２０ｎｇ之间工作曲线相关系数大于０．９９９，样品中ＶＢ_６含量为０．１％～５％时，方法回收率为９２．１７％～９８．４２％，相对标准偏差（ｎ＝６）小于３．７％。     

碘的凝胶色谱测定方法

建立了碘折凝胶色谱测定方法。色谱条件为：Ｓｈｉｍ－ｐａｃｋ ＤＩＯＬ－１５０柱；流动相甲醇０．０１ｍｏｌ／Ｌ Ｈ３ＰＯ４（１０：９０）流速为１．２ｍＬ／ｍｉｎ；柱温为３５℃，检测波长为２２４ｎｍ；线性范围是０．０１０－１．０ｍｇ／Ｌ，相关系数为０．９９９３，检测限为０．００１ｍｇ／Ｌ，相对标准偏差为１．２％－４．６％；回收率为９１％－９８％。所建立的方法已用于食盐，尿，系带等样品的测试，均取得较好     

碳糊电极测定甲硝唑的研究

报道了用碳糊电极测定甲硝唑的方法。在ｐＨ３．２的ＬｉＣｌ－ＨＣｌ电解溶液中，用二次导数阴极溶出伏安法测定甲硝唑。在碳糊电极上开路富集甲硝唑６０ｓ，然后记录其在－０．５８Ｖ的二次导数阴极溶出峰。溶出峰电流ｉｐ与甲硝唑浓度在３．０×１０－７～３．０×１０－６ｍｏｌ／Ｌ和３．０×１０－６～１．０×１０－４ｍｏｌ／Ｌ范围内呈良好的线性关系，相关系数分别为０．９９８６和０．９９９７，检出限为１．７×１０－７ｍｏｌ／Ｌ，相对标准偏差为６．０％（ｎ＝１０）。本方法直接用于甲硝唑片剂的测定，并用多种方法对甲硝唑在碳糊电极表面的反应机理进行了探讨。     

高效液相色谱中同系物保留植收敛现象的研究

在讨论影响溶质保留行为因素的基础上，建立了描述同系物保留值收敛现象的一般模型，对１２种同系物（共３８组数据）在６种不同组成的二元流动相和８种固定相中的保留值进行了回归分析，相关系数ｒ≥０．９７４，标准偏差ＳＤ≤０．０５。绘制了这些同系物的三维保留图形及投影图，并据此对同系物收敛现象及其物理意义进行了讨论，建立了计算收敛点坐标的简便方法。     

EMG模型中参数τ的一种关系式

利用一个关系式δ＝ａ＋ｂ／Ｆ＋ｃτ将标准偏差σ、时间衰减常数τ和流动相流速Ｆ很好地关联起来,取得了很好的结果,相关系数达到０．９９以上。     

一种自动微量滴定新方法

本文依据传统滴定分析原理，利用流动注射装置提出一种新的自动微量滴定方法，它不仅具有流动注射滴定分析法简便快速，试剂和试样消耗少，仪器装置简单等优点，而且测定信号怀被测组分的浓度直接成线性关系，结果的准确度和精度优于一般流动注射滴定方法。通过用盐酸滴定氢氧化钠进行验证，相关系数为０．９９９９，相对标准偏差（ＲＳＤ）为０．４％。     

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。