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

研究了在过氧化氢存在下，催化邻苯二酚或2，3-二羟基萘(DHN)与乙二胺(EN)反应的锰(II)的测定。用荧光法检测了反应物的变化。根据荧光光谱随反应时间的变化，对DHN与EN的反应机理进行了讨论。用ZINDO方法计算了dHN的电子密度分布，讨论了dHN与胺的反应活性。该方法的检出限为3ppt。锰(II)的测定范围为10~140ppm，同时观察到锰(II)对dHN的氧化，使其在330 nm处的吸光度降低。建立了一种简便、灵敏、选择性好的催化测定锰(II)的方法。在该反应中，EN除了起掩蔽剂的作用外，还起到了活化剂的作用。在20-1600pg·cm~(-1)~(-3)的浓度范围内，可测定痕量的Mn(II)。根据自由基反应和中间体络合物的形成，探讨了Stilbazo的分解反应机理，并用区域熔融法对邻苯二酚和2，3-二羟基萘的精制进行了研究。由于试剂受到玻璃管的污染，精炼剂的效果不被认可。

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.