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Solid Phase Extraction Disk Procedure to Determine 239Pu in Soils

ZHANG Ji-qiao;ZHAO Ya-ping;DING You-qian;ZHANG Sheng-dong;YANG Jin-ling   

  1. Department of Radiochemistry, China Institute of Atomic Energy,  Beijing 102413, China
  • Online:2016-11-20 Published:2016-11-21

固相萃取片法分析土壤样品中的239Pu

张积桥;赵雅平;丁有钱;张生栋;杨金玲   

  1. 中国原子能科学研究院 放射化学研究所,北京102413

Abstract:

239Pu in many soil samples should be analyzed to survey radioactive pollution level in nuclear facilities and its affinity environment efficiently. In order to input the opt conditions for column experiment, the experiments of the static adsorption coefficient of 239Pu to solid phase extraction disk with different contact time, concentration of HNO3 and different temperature were carried out. The chemical procedure for the rapid separation and determination of 239Pu in soils had been formulated, which using solid phase extraction disk (EmporeTM Anion Exchange-SR) as extraction material and liquid scintillation spectrometry counting as measurement. In the procedure, soil sample usage was 10 g, and were leached by 8 mol/L HNO3, the chemical recovery of the procedure was about 78.9%, and the minimum detectable concentration was 3.7 Bq/kg. It took less than 3 hours once and the presence of 137Cs, 90Sr-90Y and natural uranium, 241Am, 99Tc did not interfere with the procedure, owning high DF of them. The procedure can be used extensively in determination of 239Pu in soils.

Key words: soil, 239Pu, solid phase extraction disk, liquid scintillation spectrometry

摘要:

为了对核设施及周边环境的放射性污染水平进行有效监测,需要对土壤样品中的239Pu进行分析。本研究考察了静态吸附中介质酸度、接触时间以及温度对239Pu在固相萃取片上的吸附影响,确定最佳吸附条件;采用柱实验进行验证,以固相萃取片法为分离纯化手段,采用高酸上柱,低酸条件下还原解吸,以低本底液闪谱仪为放射性测量手段,建立快速分析土壤中239Pu的方法。该方法可测土壤样品量为10 g,使用8 mol/L HNO3浸取灰化后的模拟污染土壤样品,模拟土壤样品中239Pu的化学回收率为78.9%,比活度探测下限为3.7 Bq/kg,全流程分析时间小于3 h,对核素137Cs、90Sr-90Y、天然铀、241Am、99Tc去污效果良好,该方法可广泛应用于环境土壤样品的239Pu分析。

关键词: 土壤, 239Pu, 固相萃取片, 液闪谱仪