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PURIFICATION OF CATECHOL AND ITS DERIVATIVES BY ZONE REFINER,AND THEIR APPLICATION TO THE CATARITIC ANALYSIS OF METALS

区域精炼机提纯儿茶酚及其衍生物及其在金属催化分析中的应用

基本信息

批准号：
07640816
负责人：
WATANABE Kunihiro
金额：
$ 1.47万
依托单位：
SCIENCE UNIVERSITY OF TOKYO
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (C)
财政年份：
1995
资助国家：
日本
起止时间：
1995 至 1996
项目状态：
已结题

项目摘要

The determination of manganese (II), which catalyzed a reaction between catechol or 2.3-dihydroxynaphthalene (DHN) and ethylenediamine (en), has been investigated in the presence of hydrogen peroxide. A change in the reactant was detected by fluorometric method. The mechanism of the reaction between DHN and en is discussed based on the change in the fluorescence spectra with the reaction time. The distribution of the DHN electron density was calculated by ZINDO in order to discusse the reactivity of DHN to the amine. The limit of detection of Mn (II) by proposed method was 3 ppt. The determination range of Mn (II) was from 10 to 140 ppt.On the other hand, the decrease of the absorbance at 330 nm, owing to the manganese (II) -catalyzed oxidation of DHN,was monitered. As a result, a catalytic method for the simple, sensitive and selective determination of Mn (II) was developed. In this reaction, en acted as an activator besides a masking agent. The Mn (II) could be determined in the concentration range of 20-1600 pg cm^<-3>.Stilbazo was investigated in order to develope a new indicator reagent. The mechanism of decomposition reaction of Stilbazo was estimated based on the radical reaction and on intermediate complex formation.The purifications of catechol and 2,3-dihydroxynaphthalene were studied by zone melting method. The effect of refiner was not recognized because the reagent was contaminated from glass tube.

锰 (II) 催化儿茶酚或 2,3-二羟基萘 (DHN) 与乙二胺 (en) 之间的反应，已在过氧化氢存在下研究了锰 (II) 的测定。通过荧光法检测反应物的变化。根据荧光光谱随反应时间的变化，讨论了DHN与en之间的反应机理。通过ZINDO计算DHN电子密度的分布，以讨论DHN对胺的反应活性。该方法对Mn(II)的检测限为3 ppt。 Mn (II) 的测定范围为 10 至 140 ppt。另一方面，监测到由于锰 (II) 催化的 DHN 氧化，导致 330 nm 处的吸光度降低。因此，开发了一种简单、灵敏、选择性测定 Mn (II) 的催化方法。在此反应中，除了掩蔽剂之外，E还充当活化剂。 Mn(II)可以在20-1600pg cm^-3的浓度范围内测定。对芪唑进行了研究以开发新的指示剂。基于自由基反应和中间配合物的形成，推测了芪的分解反应机理。采用区域熔融法研究了邻苯二酚和2,3-二羟基萘的纯化。由于试剂被玻璃管污染，精制剂的效果未得到认可。