耐辐照玻璃成分分析标准物质的研制

采用高温熔融方法制备了玻璃成分分析标准物质.对标准物质的制备技术、均匀性检验、稳定性考察及定值不确定度进行了分析.研制的耐辐照成分分析标准物质具有良好的均匀性和稳定性,各组分不确定度均小于5％.     

氢化可的松纯度标准物质的研制

介绍纯度标准物质氢化可的松的研制方法.采用高效液相色谱法对该标准物质进行了定值及均匀性、稳定性检验.该标准物质定值结果为99.5%,扩展不确定度为0.2%,其均匀性和稳定性检验结果表明,该标准物质符合国家一级标准物质的技术要求.     

超高强度钢（35CrNi3Mo）化学成分标准物质研制

采用与超高强度钢,台炼过程相同的工艺制备了35CrNi3Mo化学成分标准物质。对标准物质的制备技术、均匀性检验、稳定性考察进行了分析。研制的35CrNi3Mo化学成分标准物质具有良好的均匀性和稳定性。采用8家实验室进行协作定值,对定值结果的不确定度进行评定,各组分定值结果的相对扩展不确定度小于13％。     

激光玻璃成分分析标准物质的研制

采用高温熔融方法制备了激光玻璃成分分析标准物质。对该标准物质的均匀性、稳电性进行了检验。结果表明,研制的标准物质具有良好的均匀性和稳定性。采用6家实验室进行协作定值,各组分：芑值结果的相对扩展不确定度均小于5％（k=2）。     

碳化硼成分分析标准物质的研制

介绍碳化硼成分分析标准物质的制备方法。以硼酸和蔗糖为原材料,酯化反应得到硼酸酯沉淀,经过烧结制备碳化硼粉体。用低温前驱体裂解法制备碳化硼成分分析标准物质,并进行了均匀性检验、稳定性考察,采用8家实验室协作定值,对定值结果的不确定度进行了评定。结果表明,研制的碳化硼成分分析标准物质具有良好的均匀性和稳定性,量值准确可靠,定值结果的相对扩展不确定度为0.003 1%~0.13%(k=2)。     

液相色谱仪检定用甲醇中胆固醇标准物质的研制

采用重量–容量法制备了液相色谱检定用200μg/m L的甲醇中胆固醇标准物质,分别用F检验和回归曲线法对研制的标准物质进行了均匀性和稳定性检验,对定值结果的不确定度进行了评定。结果表明,研制的甲醇中胆固醇标准物质具有良好的均匀性和稳定性,定值结果的相对扩展不确定度为2%(k=2)。该标准物质可用于液相色谱仪示差折光检测器、蒸发光散射检测器的检定。     

甲基对硫磷溶液标准物质的研制

采用重量–容量法研制了1.00 ng/μL甲基对硫磷农药标准物质,对研制的甲醇中甲基对硫磷溶液标准物质量值进行了均匀性和稳定性检验,对定值结果的不确定度进行了评定。结果表明,该标准物质均匀性良好,在一年内量值没有显著性变化,具有良好的稳定性,定值结果的相对扩展不确定度为3%(k=2)。该标准物质可用于农药残留测量结果的准确性评价。     

硬质聚氯乙烯氧指数标准物质的研制

研制硬质聚氯乙烯(硬质PVC)氧指数标准物质。对制备技术、均匀性检验、稳定性考察及定值不确定度进行了分析。研制的硬质PVC标准物质具有良好的均匀性和稳定性,定值数据呈正态分布,各实验室数据等精度。硬质PVC标准物质氧指数标准值为43．6％,扩展不确定度为0．7％。     

聚甲基丙烯酸甲酯氧指数标准物质的研制

介绍聚甲基丙烯酸甲酯氧指数标准物质的研制过程：对标准物质的制备技术、均匀性检验、稳定性考察及定值和不确定度进行了逐项分析。采用本体聚合的聚甲基丙烯酸甲酯板材直接加工制备标准物质,标准物质具有良好的均匀性和稳定性,定值准确可靠,标准值为17．9％,扩展不确定度为0．28％。     

GC–MS校准用异辛烷中八氟萘标准溶液的研制

采用重量–容量法研制了气相色谱–质谱(GC–MS)校准用100.1 pg/μL异辛烷中八氟萘溶液标准物质,分别用F检验和回归曲线法对研制的溶液标准物质进行了均匀性和稳定性检验,对定值结果的不确定度进行了评定。结果表明,研制的异辛烷中八氟萘溶液标准物质具有良好的均匀性和稳定性,定值结果的相对扩展不确定度为3%(k=2)。该标准物质可用于GC–MS联用仪的EI源及负CI源的信噪比校准。     

利用手持技术改进测定乙醇分子结构实验

利用压强传感器代替排水集气法,改进测定乙醇分子结构实验的仪器装置,并探索最佳反应条件。另外,设计两个空白实验,结合压强变化曲线对实验误差进行相关讨论。     

光谱仪测试范围的扩展

由于石化行业的生产需要，其材质的使用具有多样性和广泛性，经常会出现顾客委托的测试样品的一个或几个元素跨越光谱仪现有测试程序测量范围的情况。本法通过对光谱仪测试原理的认识，根据光谱仪的测试能力及标样的采集，实现了一个或几个元素测量范围的扩展，并对其测量的影响因素进行了研究。     

Influence of viscosity of medium on processes of oxygen quenching of excited states of mesoporphyrin

The oxygen quenching rate constants for singlet and triplet excited states of the dimethyl ester of mesoporphyrin IX increase with decreasing viscosity of the medium and reach a maximum at a viscosity of approximately 0.4 mPa·sec, after which the rate constants begin to decrease. The drop in rate constant with increasing fluidity of the medium may be related to a nonequilibrium character of the elementary act in the interaction of the reactants in the solvent cage. In viscous media such as isopropyl alcohol, isobutyl alcohol, and isoamyl alcohol, the reaction radius is greater than the sum of the radii of the reacting particles. The long-range character of these processes is due to the relatively weak dependence of the quenching probability on distance.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 161–167, March–April, 1989.     

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.

     

Neutral diterpenoids of oleoresins of five species of conifers of Transcarpathia

The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodynkh Soedinenii, No. 6, pp. 812–816, November–December, 1988.     

物质分配系数的测定实验改进

实验教学目的是从解决实际问题出发,以实验技术训练和实验设计思想培养为目标。介绍了将单一的物质分配系数测定实验改进为综合实验,提高了实验效果及实验资源利用率。     

Calculation of enthalpies of hydrogenation of hydrocarbons

Sets of hydrogen molecule equivalents have been developed which permit the calculation of hydrogenation of different types of carbon-carbon bonds from ab initio total energies (3-21G and 6-31G* basis sets, and, to a more limited extent, for MP2/6-31G* data) of reactants and products. The calculated enthalpies of hydrogenation are in good agreement with experiment for unstrained molecules, with average errors on the order of 2 kcal/mol. The 6-31G* equivalents allow the enthalpies for strained molecules to be calculated accurately, but the 3-21G equivalents do not. The equivalents for both basis sets have been tested by calculating the enthalpies of hydrogenation of carbon-carbon bonds in nitrogen- and oxygen-containing organic molecules, free radicals, and classical carbocations. The results are in good agreement with experiment in most cases.     

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。