高温水解–离子色谱法测定八氧化三铀中的氟和氯

建立了高温水解–离子色谱法测定八氧化三铀中氟和氯含量的方法。对影响高温水解的因素进行了试验研究,水解温度为1 050℃,水浴温度为(85±1)℃,氩气流量为600 mL/min,水解时间为1 h。选用Ion Pac AG11–HC(50 mm×4 mm)阴离子保护柱和Ion Pac AS11–HC(250 mm×4 mm)阴离子分析柱对样品进行分离,以氢氧化钾溶液等度淋洗。在0~5.00μg/mL范围内,氟和氯均有良好的线性,相关系数(r~2)分别为0.999 9,0.999 4;检出限分别为3,4μg/g。氟和氯测定结果的相对标准偏差分别为4.72%,3.23%(n=6),加标回收率分别为97%~101%,95%~99%。该法操作简便、快速,适用于八氧化三铀中氟和氯的检测。

Determination of Fluorine and Chlorine in Triurannium Octoxide by Pyrohydrolytic-ion Chromtography

A method for the determination offluorine and chlorine in triurannium octoxide(U3O8) by pyrohydrolytic-ion chromatography was established. The factors influencing hydrolysis at high temperature were examined and studied. Pyrohydrolytic temperature was 1050℃, water bath temperature was (85±1)℃,flow rate of argon was 600 mL/min, and hydrolysis time was 1 h. The chromatographic separation was performed on Ion Pac AG11-HC(50 mm×4 mm) guard column and Ion Pac AS11-HC(250 mm×4 mm) analytical column by using potassium hydroxide solution as eluent. In the range of 0-5.00μg/mL, the linearity was obtained forfluorine and chlorine, the linear correlation cofficients (r2) were 0.9999, 0.9994, and the detection limits were 3, 4μg/g, respectively. The relative standard deviations offluorine and chlorine detection results were 4.72%,3.23%(n=6),and the recoveries were 97%-101%, 95%-99%, respectively. The method is rapid and simple, and it is suitable for the determination offluorine and chlorine in triurannium octoxide.