催化光度法测定超痕量亚硝酸根

迄今为止,有关动力学法测定亚硝酸根的报道甚少,笔者实验发现,在磷酸介质中,以溴酸钾氧化中性红,亚硝酸根具有高催化活性,据此,我们研究了适宜的催化反应条件,以及共存离子的影响,从而建立了测定超痕量亚硝酸根的新催化光度法,本法测定亚硝酸根     

催化动力学光度法测定新鲜果蔬中痕量亚硝酸根

基于在稀磷酸介质中亚硝酸根对溴酸钾氧化百里酚蓝褪色反应的催化效应 ,建立了一种测定痕量亚硝酸根的催化光度法。该方法测定亚硝酸根的线性范围为 0～ 6 .5 μg/ 2 5ml,灵敏度为 0 .6 7ng·ml- 1。用于新鲜果蔬样品中痕量亚硝酸根的测定 ,结果满意     

吖啶红荧光猝灭法测定痕量亚硝酸根

研究了在稀硫酸介质中亚硝酸根与吖啶红发生的亚硝化反应,建立了测定痕量亚硝酸根的荧光猝灭法。方法的测定范围为0.01～0.70μg·ml-1。方法用于环境水样中痕量亚硝酸根的测定,结果满意。     

二甲苯蓝FF-十六烷基三甲基溴化铵分光光度法测定痕量亚硝酸根

1 引言亚硝酸根是水质、食品和环境检测的重要指标之一.目前,测定亚硝酸根的方法已有不少,作者发现,在稀盐酸介质中,十六烷基三甲基溴化铵的存在可使二甲苯蓝FF与亚硝酸根的反应灵敏度提高,选择性增强,从而建立了测定亚硝酸根的新方法.     

催化光度法测定痕量亚硝酸根

寻找新指示物质,建立新催化动力学体系用于亚硝酸根测定能显著提高测定的灵敏度,特别是在水体及食物中痕量亚硝酸根的测定中,具有很重要的意义。本文利用亚硝酸根能灵敏地催化高碘酸钾氧化N-苯基邻氨基苯甲酸显色的反应,建立了测定痕量亚硝酸根的新方法,固定反应时间,并加入一定量的氢氧化钠溶液,以冷水流冷却,可使该催化反应中止。其反应机理为:     

催化荧光法测定痕量亚硝酸根和硝酸根

亚硝酸盐广泛存在于土壤、天然水、食品等物质中,其易于仲胺、酰胺等反应,生成强烈致癌的亚硝胺化合物,是水污染的指标之一.亚硝酸根的测定通常采用Griess比色法,近年来又报道了极谱法和动力学法.试验发现,在稀磷酸溶液中.亚硝酸根对溴酸钾氧比罗丹明6G的反应有很强的催化作用,据此建立了测定痕量亚硝酸根的催化荧光分析方法,硝酸根可用锌粉还原至亚硝酸根进行测定.本法用于雨水中痕量亚硝酸根和硝酸根的测定,得到了满意结果.     

溴酸钾氧化茜素绿催化光度法测定痕量亚硝酸根

基于酸性介质溴酸钾氧化茜紊绿反应,提出了测定痕量亚硝酸根新的催化光度法.本法的Sandell灵敏度为9.4×10~(-5)μg/cm~2亚硝酸态氮,测定亚硝酸根量的线性范围为0.01～0.12μg/ml,可用于水样中亚硝酸根测定。     

催化荧光光度法测定痕量亚硝酸根

1　引　　言亚硝酸根广泛存在于环境、水体、食品等物质中 ,它可与胺类及酰胺类化合物反应生成致癌物亚硝胺 ,因此 ,它是水质、环境、食品等检测的重要项目之一。催化动力学光度法测定亚硝酸根已有不少报道 ,而催化荧光法测定亚硝酸根的报道不多。吡红Ｂ是一种生物染色剂 ,在水溶液中发射红色荧光。作者发现 ,稀磷酸介质中 ,溴酸钾氧化吡红Ｂ使荧光猝灭 ,亚硝酸根对此氧化还原褪色反应具有灵敏催化作用 ,据此建立了测定亚硝酸根的催化荧光光度新方法。该法灵敏度较高 ,选择性好 ,简便快速 ,用于水及蔬菜中痕量亚硝酸根的测定 ,结果满意…     

四波长光度法测定微量亚硝酸根及其反应机理

利用吖啶黄与亚硝酸根的反应,根据四波长处吸光度的加和值与亚硝酸根浓度的线性关系,提出并建立了测定亚硝酸根含量的新方法。线性范围０．０４￣１．０ｍｇ／Ｌ,用于样品中亚硝酸根的测定均获得满意结果。并对反应机理进行了初步探讨。     

天青Ⅰ分光光度法测定冷却液中的亚硝酸根

研究了亚硝酸根与染料天青Ⅰ在盐酸介质中的显色反应。结果表明,反应产物的最大吸收波长为442nm,据此拟定了快速简便的分光光度测定冷却液中亚硝酸根的新方法。该方法亚硝酸根浓度在0～200ug/50mL范围内服从比尔定律,用于冷却液中亚硝酸根的测定,结果与KMnO_4容量分析法一致。     

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。     

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.     

氯氧化镁生成热的研究

用氧化镁氯化镁水溶液制备了8水合氯氧化镁[nMg(OH)2·MgCl2·8H2O], 并测定了其在盐酸中的溶解热, 实验结果表明, 氯氧化镁溶解热与n值呈线性关系, 根据溶解热求出5Mg(OH)2·MgCl2·8H2O和3Mg(OH)2·MgCl2·8H2O的生成热分别为-7727.1和5888.1kJ·mol^1^-。     

Acid hydrolysis of carboxymethylcellulose of low degree of substitution

Cotton cellulose was swollen in a sodium hydroxide solution and carboxymethylated by a two-bath method for different periods of time for each process. The kinetics of acid hydrolysis and the crystallinity of the swollen and carboxymethylated samples were measured. The proportion of broken bonds, rate constants for hydrolysis, and permeability of cellulose to hydrolyzing agents were calculated. The susceptibility of glycosidic linkages to acid hydrolysis was improved by carboxymethylation more than by swelling in alkali. The increased accessibility of carboxymethylcellulose to acid was regarded as a consequence of increased intra-and intercrystalline swelling and of the glycosidic bonds' weakness caused by the electron-attracting carboxymethyl group on the C-6 position.     

Estimation of Kinetic Parameters of Thermal Oxidation of Ilmenite

The aim of the presented work was the investigation of thermal oxidation of ilmenite in static air atmosphere. The investigations were carried out by use of a derivatograph (MOM, Hungary). The changes of crystallographic structure of investigated samples were identified by X-ray diffractometry on Philips PW-1710 diffractometer. In temperature above 500°C appears structure of hematite Fe₂O₃. On the basis of the thermogravimetric measurements, the contracting area and contracting volume models were found as the best fitting experimental data. This revised version was published online in August 2006 with corrections to the Cover Date.     

Mechanism of action of base-catalyzed oxygenation of phenol derivatives

Cyclopropyl derivative of 2,6-di-tert-butylphenol is synthesized as a probe to investigate the mechanism of base-catalyzed autooxidation of phenol derivatives. Our study indicates that one electron reduction of molecular oxygen from phenolate gives phenoxyl radical 3, a key intermediate of autooxidation. The coupling of phenoxyl radical and superoxide radical gives peroxylate anion 4 and produces the final epoxy alcohol adduct 6.     

化学计量中不确定度评定研究进展

测量不确定度是表征合理地赋予被测量之值的分散性的参数。本文针对化学计量不确定度评定基础模型仅适用于线性模型、概率分布为正态分布或缩放位移t分布等局限,介绍了近年来不确定度评定的研究热点:蒙特卡罗方法(Monte Carlo Method,MCM),不确定度评定的来源、评定概念、评估方法及其发展过程,扩大了测量不确定度评定与表示的适用范围。     

微量钙的测定方法研究进展

介绍了1995-2006年期间测定微量和痕量钙的方法,如电感耦合等离子体-原子发射光谱法、原子吸收光谱法以及离子色谱法等的工作原理和特点,并说明了其测定微量钙的应用领域。并对微量钙的测定技术进行了展望(引用文献55篇)。     

Stages of thermal decomposition of sodium oxo-salts of sulphur

Thermal behaviour of sodium oxo-salts of sulphur: Na₂SO₄, Na₂S₂O₇, Na₂S₂O₆, Na₂SO₃, Na₂S₂O₅, Na₂S₂O₄, Na₂S₂O₃, Na₂S₃O₆ and of sulphides Na₂S and Na₂S₂ was studied on heating up to 1000°C. The experiments were performed with anhydrous compounds obtained from commercial products by recrystallisation and dehydration. The stage mechanisms of decomposition of anionic sub-lattices of the salts have been proposed basing on the Górski’s morphological classification of simple species. The thermal stability and the stage decomposition mechanisms were correlated with the structure and the potential chemical properties of the salt anions. The thermal decomposition processes were studied by means of thermal analysis, and the decomposition products were identified by means of X-ray phase analysis.     

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.