自动固相萃取仪在尿中钚分析方法中的应用

摘要

In order to monitor the intakes of plutonium by workers and estimate the internal exposure doses efficiently ,a recommended technique by the international com-mission on radiological protection (ICRP) was measurement of activity in excreta ,such as urine .The separation and purification method were provided for plutonium in urine by an automatic solid phase extraction apparatus .After the optimization of the experi-mental method ,the whole experiment could be processed automatically .The experi-ments were operated in the following conditions :nitric acid concentration of 7~8 mol/L , adsorption rate of 0.5 mL/min ,desorption rate of 0.3 mL/min ,desorption solution of 10 mL with 0.36 mol/L HCl-0.01 mol/L HF .The whole recovery rate and relative standard deviation were 75.70% and 7.98% ,respectively .It showed that the separa-tion efficiency and the stability of samples were improved dramatically in the pre-treatment process of plutonium in urine by using automatic solid phase extraction apparatus .%为了对钚操作者内照射剂量进行有效监测和估算,国际辐射防护委员会(ICRP)推荐测量工作人员的排泄物,比如对尿液中钚进行分析.本研究采用自行研制的自动固相萃取仪分离纯化尿中的钚,并优化实验方案,实现自动化操作.分离纯化的优化实验条件为:料液硝酸浓度为7~8 mol/L、吸附速度为0.5 mL/min、解吸速度为0.3 mL/min和解吸液为10 mL 0.36 mol/L HCl-0.01 mol/L HF溶液.采用优化条件处理后,全程平均回收率为75.70%,相对标准偏差为7.98%.结果表明,在尿中钚分析的前处理中,采用自动固相萃取仪进行分离纯化,能够显著提高分离效率,提高样品前处理的稳定性.