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使用现有的恒电位仪、数字积分仪和数字电压表进行了镎浓度和价态的控制电位库仑滴定。利用部分电解氧化还原法测定了Ce(Ⅳ)/Ce(Ⅲ)和Np(Ⅵ)/Np(Ⅴ)电对的克式量电位,在1.00N H_2SO_4介质中,其数值分别为1.196和0.841伏。当镎的取样总量约为1.3毫克时,使用控制电位库仑法测定镎浓度得到了0.6%的精密度和较高的准确度(相对作为基准方法的恒电流库仑法有0.9%的偏差)。本方法测定镎的价态与反相分配色层法符合得很好。实验结果表明,大量铀存在时(铀:镎约为75)对镎的电解速度和镎价态测定没有显著影响。
Coulometric titration of valence and valence control potentials was performed using existing potentiostats, digital integrators and digital voltmeters. The gram-type potentials of Ce (Ⅳ) / Ce (Ⅲ) and Np (Ⅵ) / Np (Ⅴ) were determined by partial electrolysis-oxidation reduction method. The values were 1.196 and 0.841 V in 1.00N H 2 SO 4 medium respectively. . When the total sample size of 镎 was about 1.3 mg, the determination of 镎 concentration by the control potential coulometry yielded a precision of 0.6% and a high accuracy (a 0.9% deviation from the galvanostatic coulometric method as a reference method). Determination of the valence of this method and reverse phase distribution chromatography method in good agreement. Experimental results show that the presence of a large amount of uranium (uranium: 镎 about 75) on 镎 electrolysis speed and 镎 valence state determination had no significant effect.