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    Purex流程中二甲基羟胺与甲基肼的分析

    Analyzing Method of N, N-Dimethylhydroxylamine and Methylhydrazine in Purex Process

      摘要
    • 摘要: 研究了在测定1BP中的N，N-二甲基羟胺（DMHAN）和甲基肼（MMH）的浓度之前用TODGA将其中的Pu（Ⅲ）萃取出来；并基于所发现的在室温下pH为2.0～5.5时，Fe3+只与DMHAN反应而不与稀的MMH发生反应；以及在室温下pH为0～5.5时，稀的I2溶液只与MMH发生反应而不与稀的DMHAN反应；分别建立了用Fe3+/邻菲罗琳-分光光度法测定1BP萃余液中DMHAN的浓度，相对偏差小于1.0%，检测下限为3.00×10-6mol/L；用I2溶液褪色-分光光度法测定了其中的MMH的浓度，相对偏差小于1.0%，检测下限为3.00×10-5mol/L。并考察了反应时间、甲醇、甲醛和酸度等对结果的影响。该方法不仅适用于测定1BP中DMHAN和MMH的浓度，也适用于1BX、2BX和2BP中。

       

      Abstract: The extraction of Pu（Ⅲ） with TODGA from 1BP solution prior to the determination of N, N-dimethylhydroxylamine(DMHAN) and methylhydrazine(MMH) in it was studied and excellent removal was observed. It was found that Fe3+ could react with DMHAN but did not react with MMH in the pH range 2.0-5.5 at room temperature. It was also found that dilute I2 solution reacted only with MMH but not with dilute DMHAN in the pH range 0-5.5 at room temperature. Based on these findings the determination of DMHAN with Fe3+/1, 10-phenanthroline spectrophotometry, and the determination of MMH by iodine fading spectrophotometry were developed. Their detection limits were found to be 3.00×10-6 mol/L and 3.00×10-5mol/L, respectively. Their analytical errors were estimated lower than 1.0%. The influence of reaction time, acidity, and the existence of methanol or formaldehyde on the determination was examined. These methods could also be used to analyze DMHAN and MMH in 1BX, 2BX, and 2BP solutions.

       

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