超级微波消解–电感耦合等离子体质谱法测定豆奶粉中镍的不确定度评定及优化  

Evaluation and Optimization of Uncertainty in Determination of Nickel in Soy Milk Powder by Ultra-Wave Digestion-Inductively Coupled Plasma Mass Spectrometry

作　　者：薛敏敏 刘芳芳 朱礼 袁列江 吴海智 陈瑶 XUE Min-min;LIU Fang-fang;ZHU Li;YUAN Lie-jiang;WU Hai-zhi;CHEN Yao(Hunan Testing Institute of Product and Commodity Supervision,Changsha,Hunan 410007,China)

机构地区：[1]湖南省产商品质量检验研究院,湖南长沙410007

出　　处：《粮油食品科技》2023年第1期164-172,共9页Science and Technology of Cereals,Oils and Foods

基　　金：湖南省市场监督管理局科技计划项目(2022KJJH46)。

摘　　要：对超级微波消解-电感耦合等离子体质谱法测定豆奶粉中镍的不确定度进行评定与优化。以JJF1059.1—2012《测量不确定度评定与表示》与CNAS—GL006:2019《化学分析中不确定度的评估指南》为依据,建立不确定度评定的数学模型,分析不确定度的主要来源并评定不确定度分量,进而计算合成相对标准不确定度与扩展不确定度,最后分析不同来源对不确定度的影响,提出减小不确定度的可能优化方法。当包含概率为95%(即包含因子k=2)时,镍元素的扩展不确定度为0.222 mg/kg,即豆奶粉中镍含量的测定结果为(3.825±0.222)mg/kg。通过降低不确定度的优化方法,相对标准不确定度从0.0290下降至0.0238。标准工作溶液的配置与标准曲线的拟合是超级微波消解–电感耦合等离子体质谱法测定豆奶粉中镍的不确定度的主要来源,优化方法能够有效降低测定结果的不确定度。The uncertainty in determination of nickel in soy milk powder by ultra-wave digestioninductively coupled plasma mass spectrometry was evaluated and optimized.According to JJF1059.1—2012 Evaluation and expression of uncertainty in measurement and CNAS—GL006:2019 Guidance on quantifying uncertainty in chemical analysis,the mathematical model of uncertainty evaluation was built.The main sources of uncertainty were analyzed and their uncertainty components were evaluated.Then the relative standard uncertainty and the expanded uncertainty were computed.Finally,the influence of different sources was analyzed and the possible optimization methods for reducing the uncertainty were proposed.When the coverage probability was 95%(i.e.,the coverage factor was k=2),the expanded uncertainty of nickel is 0.222 mg/kg,which indicates the determination result of nickel in soy milk powder was(3.825±0.222)mg/kg.The relative uncertainty was reduced from 0.0290 to 0.0238 by the optimization methods.Configuration of standard working solution and fitting of standard curve were the main sources of the uncertainty in determination of nickel in soy milk powder by ultra-wave digestion-inductively coupled plasma mass spectrometry,and the optimization could reduce the determination uncertainty significantly.

关 键 词：不确定度 优化 电感耦合等离子体质谱法 豆奶粉 镍 

分 类 号：TS207.3[轻工技术与工程—食品科学]