罗丹明S-高碘酸钾体系催化光度法测定痕量铑

研究了铑(Ⅲ)催化高碘酸钾氧化罗丹明S的褪色反应,据此建立了测定微量铑的催化光度分析法,研究了该催化氧化还原褪色反应的最佳条件及动力学参数.结果表明:在以硫酸为介质及90±0.5℃的条件下,罗丹明S-高碘酸钾体系测定微量铑的方法具有较高的灵敏度,线性范围为10~140μg/LRh(Ⅲ),检出限为5.0×10-9g/mL,表观活化能为64.86 kJ/mol.方法灵敏,准确,应用于合成样品中微量铑的测定,结果令人满意.     

高碘酸钾氧化丁基罗丹明B催化动力学光度法测定微量芦丁

在氢氧化钠介质中 ,微量芦丁对高碘酸钾氧化丁基罗丹明B褪色反应有明显的催化作用 ,据此建立了测定芦丁含量的催化动力学光度法。讨论了动力学反应参数。该方法的线性范围为 0 .0 2～ 2 .0mg L ;检出限为 1.0× 10 - 2 mg L。方法简便 ,快速 ,灵敏度高 ,用于芦丁片剂中芦丁含量的测定 ,结果令人满意。     

阻抑动力学光度法测定芦丁的研究

在稀硫酸介质中,微量芦丁对高碘酸钾氧化玫瑰桃红R褪色反应有明显的阻抑作用,据此建立了测定微量芦丁的动力学光度新方法。选定了最佳条件并测定了反应动力学参数,方法的线性范围为0.02～0.4μg mL,检出限为5.0×10-9g mL。方法已用于槐米和芦丁片剂中芦丁的测定。     

动力学光度法测定芦丁的研究

在氢氧化钠介质中,微量芦丁对高碘酸钾氧化罗丹明6G褪色反应有明显的催化作用,据此建立了测定芦丁含量的动力学光度分析法。方法的线性范围为0.02～1.5μg/mL,检出限为1.0×10-8g/mL。测定了反应动力学参数。方法用于芦丁片剂中芦丁含量的测定,结果令人满意。     

丽春红2R-高碘酸钾催化动力学体系光度法测定痕量铁

在硫酸介质中,微量铁(Ⅲ)能显著催化高碘酸钾氧化丽春红2R(PR)的褪色反应。研究了该指示反应的最佳反应条件和动力学参数,建立了一个测定痕量铁的新的催化动力学分析方法。方法的线性范围为0.010～1.0μg/25mL,检出限为1.18×10-9g/mL。用本法测定了中草药及食品中铁的含量,结果满意。     

动力学光度法测定饮用水中微量碘

碘是人体必须的微量元素之一,是维持甲状腺功能的重要元素,也称为智慧元素。目前微量碘的测定大都采用碘／淀粉比色法,碘／有机溶剂比色法,碘（Ｉ－）／催化还原／动力学分光光度法,其他还有电化学分析方法及离子色谱［１］等方法测定碘。本文利用了碘对高碘酸钾氧化...     

催化褪色光度法测定痕量钛(Ⅳ)的研究

本文发现在硫酸介质中,钛(Ⅳ)催化高碘酸钾氧化中性红褪色的新指示反应,研究了反应的动力学条件,建立了催化褪色光度法测定痕量钛(Ⅳ)的新方法,灵敏度为2.8×10~(-11)Ti~(4+)/ml。     

催化分光光度法测定食品中痕量锰

文献报道了锰的催化动力学分析法^[1-5],但使用高碘酸钾-二甲苯兰FF体系,尚未见报道,本文的研究表明:高碘酸钾氧化二甲苯兰FF(Xylene Cyanole FF,简称XCIFF)使之褪色,有较佳的催化效应,溶液颜色由亮兰变为棕黄,同时使用邻菲罗啉作活化剂,反应灵敏度能进一步提高,方法的线性范围为1.85～11ngMn·mL^-1,利用此方法测定了某些食品中的痕量锰。     

阻抑动力学分光光度及荧光光度法测定微量碘

在稀磷酸介质中,微量碘离子对亚硝酸根催化溴酸钾氧化吡罗红B褪色及荧光猝灭的反应有显著阻抑作用,以此为指示反应提出了测定微量碘离子的阻抑动力学光度和阻抑动力学荧光分析新方法。测定碘离子的线性范围分别为4-200μg/L和3-40μg/L,检出限分别为2.8μg/L和1.6μg/L。用于食品中微量碘的测定,结果满意。     

动力学光度法测定痕量维生素K3的研究

在氢氧化钠介质中,微量维生素K3,对高碘酸钾氧化苯并红紫4B褪色反应有明显的催化作用,据此建立了测定维生素K3含量的动力学光度分析法.确定了反应动力学参数,方法的线性范围为0.02～1.1 μg/mL.检出限为1.0×10-8 g/mL.方法用于维生素K3片剂中维生素K3含量的测定,结果令人满意.     

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。     

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.     

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.

     

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。