阻抑-褪色光度法测定痕量硅

基于NH3 NH4 Cl缓冲溶液介质中 ,Si 对H2 O2 氧化十六烷基三甲基溴化铵 姜黄素离子缔合物的褪色反应的抑制作用 ,提出了测定痕量硅新的高灵敏的褪色光度法。该方法的表观摩尔吸光系数ε50 0=5 .70× 10 5L·mol-1·cm-1;线性范围为 0 .4～ 3.6 μg/L ;线性回归方程ΔA =2 .2 3× 10 -4 + 0 .0 2 0 17CSi (μg/L) ;相关系数r =0 .9999;测定下限为 2 0× 10 -8g/L。本法用于人发样和水样中痕量硅的测定 ,结果满意。     

阻抑动力学光度法测定痕量钛(Ⅳ)

在硫酸和聚乙烯醇溶液中 ,钛 ( )能抑制 Fe( )催化 H2 O2 氧化中性红褪色 ,研究了该反应的最佳条件和动力学参数 ,据此建立了一种测定痕量钛( )的新方法 ,方法检出限为 7.5× 1 0 -2 μg/m L ,测定范围为 0 .0 6～ 0 .60μg/m L,可用于人发中 Ti( )的测定。     

靛蓝胭脂红催化褪色光度法测定钴

研究了在弱碱性介质中 ,Co( )对 H2 O2 氧化靛蓝胭脂红的褪色反应催化作用 ,建立了催化动力学光度法测定痕量 Co( )的新方法。方法线性范围为 0～ 1 .0μg/2 5m L ,检出限为 9.92× 1 0 - 7g/L ,反应的表观活化能为 8.66k J/mol,用于水样中 Co( )的分析 ,结果满意     

催化过氧化氢氧化镍-依来铬红B络合物褪色光度法测定痕量汞

基于在PVA存在下 ,痕量汞催化过氧化氢氧化镍 依来铬红B络合物的褪色反应 ,建立了催化褪色光度法测定痕量汞的新方法。汞浓度在 0 .0 1～ 0 .0 6 μg/L范围内符合比尔定律 ;检出限为 1 .2× 1 0 -9g/L。用于人发和废水等样品中痕量汞的测定 ,获得满意的结果。     

溴酚红-过氧化氢催化光度法测定痕量锌

在稀氢氧化钠介质中,Zn2+催化过氧化氢氧化溴酚红的褪色反应,通过试验确定了测定条件,建立了一个催化动力学光度法测定痕量锌的方法。Zn2+的检出限为1.5×10-7g.L-1,线性范围为0~4.8×10-2mg.L-1,方法用于测定头发中痕量锌。     

煤矸石中痕量钴的催化光度法测定

研究了在 pH 10.0的 Na2B4O7－ NaOH介质中,痕量 Co(Ⅱ )催化 H2O2氧化桑色素的褪色反应,褪色程度与 Co(Ⅱ )量在一定范围内呈线性相关。基于此,建立了一种测定痕量 Co(Ⅱ )的光度法。结果表明方法的检出限为 7.6× 10－ 2 μ g/L, Co(Ⅱ )质量浓度在 0.0～ 50.0 μ g/L范围内符合比尔定律。结合 N530萃取剂萃取分离,测定了煤矸石中的痕量钴。     

催化褪色光度法测定痕量锰

1　引　　言测定痕量锰有高碘酸钾 天青 (检出限 2 4× 1 0 - 9ｇ ｍＬ)、过氧化氢 铬黑Ｔ(检出限 1 0× 1 0 - 9ｇ ｍＬ)、高碘酸钾 氨三乙酸 ＰＡＮ ＴｒｉｔｏｎＸ 1 0 0 (检出限 3 .6×1 0 - 9ｇ ｍＬ)和高碘酸钾 ＰＡＮ ＴｒｉｔｏｎＸ 1 0 0 (检出限 3 .2× 1 0 - 9ｇ ｍＬ)等催化光度法。实验表明 :在加热 1 0 0℃、1 0ｍｉｎ和聚丙烯酰胺 (ＰＡＭ)存在下 ,Ｍｎ2 + 能催化氯酸钾氧化铬天青Ｓ(ＣＡＳ)的褪色反应 ,ＰＡＭ对该体系有增稳作用 ,据此建立了氯酸钾氧化铬天青Ｓ催化褪色光度法测定痕量锰的新方法 (检出限 4 0× 1 0 - 1…     

阻抑褪色光度法测定微量硫代硫酸根

基于加热和pH =5 .0～ 6.0条件下 ,硫代硫酸根抑制H2 O2 氧化结晶紫 (CV)的褪色反应 ,建立了一种测定硫代硫酸根的方法。硫代硫酸根在 4.5× 1 0 -5～ 4.5× 1 0 -4g/L范围内服从比耳定律 ;检出限为 3 .2×1 0 -6g/L。本法用于定影废液中硫代硫酸钠含量的测定 ,结果满意。     

阻抑褪色光度法测定微量硫代硫酸根

基于加热和pH =5 .0～ 6 .0条件下 ,硫代硫酸根抑制H2 O2 氧化结晶紫 (CV)的褪色反应 ,建立了测定硫代硫酸根的方法。硫代硫酸根在 4 .5× 1 0 -5～ 4 .5× 1 0 -4g/L范围内服从比耳定律 ,检出限为 3.2× 1 0 -6g/L。本法用于定影废液中硫代硫酸钠含量的测定 ,结果满意     

催化光度法测定水中痕量亚硝酸根

利用在硫酸介质中亚硝酸根催化溴酸钾氧化吖啶橙的褪色反应 ,建立了测定痕量亚硝酸根的新方法。方法检出限为 7.6× 1 0 -8mol/ L,线性范围 0～1 .1 2× 1 0 -6mol/ L。本法可用于测定雨水和自来水中的痕量亚硝酸根     

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。     

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.     

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.     

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.     

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.

     

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。