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分步消解法ICP-MS测量大米中砷及不确定度评价 被引量:1

Uncertainty Evaluation and Determination of Arsenic in Rice by ICP-MS with Stepwise Digestion Method
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摘要 为提高食品中重金属测定方法的准确性与可重复性、保障人民食品安全,采用石墨-微波分步消解法,使用电感耦合等离子质谱(ICP-MS)对大米中重金属砷含量进行检测,并根据试验过程对检测结果进行不确定度评定,分析测量过程中的样品称量、样品消解、标准溶液的配制、标准曲线的拟合和测量重复性等因素造成的不确定度,计算各不确定度分量,分析不确定度和扩展不确定度判断检测结果的可靠性。所测大米样品中的砷含量为0.110 mg/kg,扩展不确定度为0.011 mg/kg,k=2。通过对测量过程中不确定度的评定,试验发现该检测过程中的不确定度主要来源于样品消解和测量重复性,并与其他方法测试所得不确定度进行对比分析,结果较好。 It was to improve the accuracy and repeatability of the determination method of heavy metals in food and to ensure people’s food safety.The content of heavy metal arsenic in rice was detected by ICP-MS with graphite-microwave stepwise digestion method.The uncertainty of the detection results was evaluated according to the experimental process.The uncertainty caused by sample weighing,sample digestion,preparation of standard solution,fitting of standard curve,measurement repeatability and other factors in the measurement process was analyzed.The component of uncertainty was quantified,and the reliability of detection results was evaluated by the results of synthetic uncertainty and extended uncertainty.The content of arsenic in rice samples was 0.110 mg/kg.The extended uncertainty was 0.0112 mg/kg(k=2).On the basis of the evaluation of the uncertainty in the measurement process,it was found that the uncertainty in the measurement process mainly came from sample digestion and repeatability.The result was well by comparing and analyzing with the other methods.
作者 卢鑫 刘聪 陈燕敏 刘冰 侯金妹 LU Xin;LIU Cong;CHEN Yanmin;LIU Bing;HOU Jinmei(College of Chemistry and Chemical Engineering,Zhengzhou Normal University,Zhengzhou 450044;Anhui Zezhong Safety Technology Co.,Ltd.,Hefei 232000;Hefei Institute for Public Safety Research,Tsinghua University,Hefei 230601)
出处 《食品工业》 CAS 2024年第1期304-308,共5页 The Food Industry
基金 特大城市饮用水源地水体安全监测设备与风险预警系统研发及应用(安徽省重大科技专项)(202203a07020034)资助。
关键词 分步消解 大米 不确定度 stepwise digestion rice arsenic uncertainty
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