电感耦合等离子体原子发射光谱法测定化肥中铊的不确定度评定  

Evaluation of uncertainty in the determination of thallium in fertilizer by inductively coupled plasma-atomic emission spectrometry

作　　者：姚洵 郑凯 单经宇 卢志琴 YAO Xun;ZHENG Kai;SHAN Jingyu;LU Zhiqin(Comprehensive Technology Center of Zhangjiagang Customs,Zhangjiagang,215600,China;Logistics Management Center of Zhangjiagang Customs,Zhangjiagang,215600,China;Zhangjiagang Inspection and Certification Co.,Ltd,Zhangjiagang,215600,China)

机构地区：[1]张家港海关综合技术中心,江苏张家港215600 [2]张家港海关后勤管理中心,江苏张家港215600 [3]张家港检验认证有限公司,江苏张家港215600

出　　处：《化学分析计量》2023年第12期104-108,共5页Chemical Analysis And Meterage

基　　金：南京海关科研项目(2023KJ31)。

摘　　要：采用电感耦合等离子体发射光谱法测定化肥中铊的含量,通过对测量过程进行分析,确定了不确定度的来源主要有电子天平、标准工作溶液配制、标准工作曲线拟合、样品消解液定容、消解回收率及测量重复性等引入的不确定度分量,其中样品处理消解回收率对不确定度的贡献最大。通过建立数学模型,对各不确定度分量进行评估量化,得到了测定结果的合成不确定度和扩展不确定度。结果显示,当置信概率为95%、包含因子为2时,样品中铊质量分数为0.316 mg/kg,其扩展不确定度为0.017 mg/kg。The content of thallium in fertilizer was determined by inductively coupled plasma atomic emission spectrometry.The measurement process was analyzed and the sources of uncertainty were detemined,which mainly included the uncertainty components introduced by the electronic balance,standard working solution preparation,standard working curve fitting,digestion solution constant volume,the digestion recovery rate and measurement repeatability.The digestion recovery rate contributed the most to the uncertainty.By establishing a mathematical model and evaluating and quantifying each uncertainty component,the combined uncertainty and expanded uncertainty of the determination results were obtained.The results showed that when the confidence probability was 95%and the coverage factor was 2,the thallium content in the sample was 0.316 mg/kg with the expanded uncertainty of 0.017 mg/kg.

关 键 词：电感耦合等离子体原子发射光谱法 化肥 铊 不确定度 

分 类 号：O657.3[理学—分析化学]