堆芯铝合金样品中63Ni的液闪测定技术
Determination of 63Ni in Aluminum Alloy Samples From Nuclear Reactor Core by Liquid Scintillation Method
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摘要: 为建立堆芯铝合金样品中63Ni活度测量的方法，对63Ni液闪测量的相关问题进行了研究。样品经前处理后用液闪进行测量，相应的前处理流程包括样品的溶解、阴离子交换分离、氢氧化物沉淀及萃取分离程序。通过条件实验对液闪测量过程的相关参数进行了比较研究，包括样品液酸度、样品液与闪烁液体积比及镍载体的加入量等。3110型液体闪烁能谱仪对不同活度63Ni标准系列的测量效率均在70%以上，样品液酸度选择为0.3mol/L，样品液与闪烁液体积比选择为1∶2，镍载体加入量选择为5mg。通过空白实验得出计数的标准偏差为0.077/s，相对标准偏差为15.3%（n=12），方法检出限为1.38Bq/g。该方法适用于反应堆退役样品的分析测量。Abstract: To establish a method of measuring the radioactivity of 63Ni in aluminum alloy samples from nuclear reactor core, various relevant problems were studied. Samples were pretreated before liquid scintillation counting (LSC) by dissolution, anion exchange separation, hydroxide precipitation, and solvent extraction procedures. LSC-related parameters, such as sample solution acidity, sample solution-to-cocktail volume ratio, and added nickel carrier amount, were investigated. The detection efficiency of Tri-Carb 3110 liquid scintillation spectrometer with respect to 63Ni for a series of 63Ni standards of different activities are all better than 70%. The recommended experimental conditions are listed below: sample acidity 0.3 mol/L, sample-to-cocktail volume ratio 1∶2, Ni carrier amount 5 mg. The standard deviation of 0.077/s and the relative standard deviation of 15.3%(n=12) are found for blanks. The detection limit is 1.38 Bq/g. The present method is suitable to analyze samples for decommissioning of nuclear reactors.
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Keywords:
- aluminum alloy /
- measure efficiency /
- standard deviation /
- detection limit
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