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微波消解-石墨炉原子吸收法测定大米粉中镉的不确定度评定

Uncertainty Evaluation of Cadmium in Rice Flour by Microwave Digestion-Graphite Furnace Atomic Absorption Spectrometry
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摘要 分析微波消解-石墨炉原子吸收法测定大米粉中镉含量的不确定度来源;依据JJF 1059.1—2019《测量不确定度评定与表示》和GB 5009.15—2023《食品安全国家标准食品中镉的测定》第一法建立测定大米粉中镉含量的数学模型,测定中不确定度产生的主要来源为重复性实验、原子吸收光谱仪校准、样品前处理、试样称量、标准储备液、标准溶液配制和校准曲线拟合引入的不确定度,其中校准曲线拟合、仪器校准、样品称量和标准溶液配制引入的不确定度相对较大,因此,在实验过程中应提高校准曲线相关系数,加强溶液配制操作的准确度,增加称样量,提高仪器的稳定性和灵敏度。该研究为提高大米粉中镉的检测的准确度提供了依据。 An uncertainty analysis of the determination of cadmium in rice flour by microwave digestion-graphite furnace atomic absorption method.Based on JJF 1059.1—2019“Evaluation and Representation of Measurement Uncertainty”and GB 5009.15—2023“Food Safety National Standard for the Determination of Cadmium in Foods”.Method 1,a mathematical model was established for the determination of cadmium content in rice flour.The main sources of uncertainty in the determination were the repeatability experiment,calibration of atomic absorption spectrometer,sample pretreatment,sample weighing,standard stock solution,standard solution preparation,and curve fitting.Among them,the uncertainties introduced by curve fitting,instrument calibration,sample weighing,and standard solution preparation were relatively large.Therefore,in the experimental process,the correlation coefficient of the calibration curve should be improved,the accuracy of solution preparation operations should be enhanced,the sample weight should be increased,and the stability and sensitivity of the instrument should be improved.This study provides a basis for improving the accuracy of cadmium detection in rice flour.
作者 吴静 王婧 程梦蓉 WU Jing;WANG Jing;CHENG Mengrong(Shaanxi Grain Quality and Security Center,710016 Xi'an,China)
出处 《粮食加工》 2025年第4期114-117,129,共5页 Grain Processing
关键词 不确定度 微波消解-石墨炉原子吸收 cadmium uncertainty microwave digestion-graphite furnace atomic absorption spectrometry
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