阻抑动力学分光光度法测定痕量碘

研究了在稀H3PO4介质中,痕量碘离子对NO-2催化溴酸钾氧化吖啶橙的阻抑作用,建立了测定痕量碘离子的阻抑动力学光度分析的新方法。测定碘离子的线性范围为0～0.40μg/mL,检出限为7.3×10-9g/mL。已用于食品中的微量碘的测定。     

阻抑动力学光度法测定乳品中的痕量碘

研究了在稀H2SO4介质中,痕量I-对KBrO3氧化酸性品红的阻抑作用及其动力学条件,建立了测定痕量I-的阻抑动力学光度分析的新方法.测定I-的线性范围为0～0.04 μg/mL,检出限为1.1×10-9 g/mL.已用于乳品中痕量碘的测定.     

阻抑动力学分光光度法测定微量碘

基于在稀磷酸介质中,痕量碘离子对亚硝酸根催化溴酸钾氧化甲基红的的阻抑作用,提出了测定痕量碘离子的阻抑动力学分光光度分析的方法.测定碘离子的线性范围在0.66 mg·L-1以内,检出限(3Sb/K)为7.5×10-6g·L-1.用于海带及食盐中微量碘的测定,测定结果的相对标准偏差(n=6)在1.4%～2.2%之间,测得方法的回收率为99.7%～100.1%.     

阻抑动力学光度法测定痕量尿素

研究了在酸性介质中,痕量尿素对NO2-催化KBrO3氧化维多利亚绿G的阻抑作用,通过测量617 nm处吸光度的变化,建立了测定痕量尿素的阻抑动力学光度分析的新方法。在最佳实验条件下,测定尿素的线性范围为0.0~0.14mg/L,检出限为5.0×10-6g/L。对2.0μg/25 mL进行10次平行测定的相对标准偏差为2.8%。并试验了共存离子对催化反应的影响,常见的离子均不干扰测定。方法可用于废水中痕量尿素的测定。     

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。     

催化动力学光度法间接测定水中痕量硫离子

在氨水介质中,硫离子可阻抑Fe(Ⅲ)催化过氧化氢氧化二甲酚橙褪色,并且催化体系和阻抑体系在570 nm处吸光度的差值与硫离子浓度呈线性关系,据此建立了阻抑动力学光度法间接测定痕量硫离子的新方法。方法的线性范围为0.0020~0.044mg/L,检出限为1.6×10-9g/mL,对0.040 mg/L硫离子进行10次平行测定的相对标准偏差为2.1%。方法用于废水中硫离子的测定,结果满意。     

阻抑乙基橙褪色动力学光度法测定痕量铁(Ⅲ)

在H2SO4介质中,痕量铁(Ⅲ)对KBrO3氧化乙基橙褪色反应有很强的阻抑作用,利用光度法检测阻抑反应过程中乙基橙浓度的变化,建立了铁(Ⅲ)-溴酸钾-乙基橙体系阻抑动力学光度法测定痕量铁(Ⅲ)的方法。在选定条件下,方法的线性范围为0.006～0.32μg/mL,检出限(3s/k)为0.0031μg/mL。     

阻抑动力学光度法测定食品中的痕量铜

研究了铜阻抑高碘酸钾氧化玫瑰桃红R的褪色反应 ,建立了阻抑动力学光度法测定痕量铜的新方法 ,找到了最佳试验条件。该法线性范围为 0～ 0 0 0 8μg/mL ,检出限为 0 3 9× 1 0 - 3μg/mL ,应用于食品中铜的测定 ,结果满意     

阻抑动力学光度法测定痕量铌(Ⅴ)

研究发现,在硫酸介质中,痕量铌(Ⅴ)能灵敏地阻抑溴酸钾氧化二甲基黄褪色。研究了该阻抑褪色反应的最佳条件及动力学参数,建立了一种测定痕量铌(Ⅴ)的新方法。该法测定线性范围为0~30 ng/10mL,检出限为4.21×10-11 g/ mL。方法用于矿石中铌的测定,结果满意。     

阻抑动力学光度法测定痕量铜

在pH 4.5的HAc-NaAc缓冲溶液中, 痕量铜对KBrO3氧化亮绿SF的褪色反应有明显的阻抑作用, 据此建立了测定痕量铜的新方法. 方法的线性范围为0.004～0.048 μg/mL, 检出限为8.63×10-4 μg/mL, 已用于人发中铜的测定.     

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.     

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.     

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^-。     

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.     

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.     

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.

     

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)。