食品科学

• 成分分析 • 上一篇    下一篇

微波消解-电感耦合等离子体发射光谱法测定牡蛎中锌的不确定度评定

孙玲玲,宋金明*,于 颖,孙 萱,温廷宇,林 强   

  1. 中国科学院海洋研究所分析测试中心,山东 青岛 266071
  • 出版日期:2016-08-25 发布日期:2016-08-30
  • 通讯作者: 宋金明

Evaluation of Uncertainty for Zinc Determination in Oyster by Microwave Digestion-ICP-OES

SUN Lingling, SONG Jinming*, YU Ying, SUN Xuan, WEN Tingyu, LIN Qiang   

  1. Analytical Center of Institute of Oceanology, Chinese Academy of Sciences, Qingdao 266071, China
  • Online:2016-08-25 Published:2016-08-30
  • Contact: SONG Jinming

摘要:

对微波消解-电感耦合等离子体发射光谱法测定牡蛎中锌含量的不确定度来源进行了分析,依据JJF 1059—1999《测量不确定度评定与表示》,量化了各不确定度分量,计算合成不确定度,最终得出测定结果的扩展不确定度。结果表明,测定结果的不确定度主要包括校准曲线拟合、测量重复性、标准溶液配制、样品称量以及样品定容体积,其相对标准不确定度分量分别为0.016、0.004 7、0.001 4、0.002 2和0.000 8。通过对不确定度分量的分析,指出校准曲线拟合是影响测定结果不确定度的主要因素,测量重复性、标准溶液配制以及样品称量和定容过程对最终结果不确定度影响亦不可忽略。测定结果的合成标准不确定度为13.29 mg/kg,扩展不确定度为26.58 mg/kg(k = 2)。因此,牡蛎中锌含量的测定结果为(781.98±26.58)mg/kg(k = 2,P = 95%)。

关键词: 不确定度, 锌, 电感耦合等离子体发射光谱法, 微波消解, 牡蛎

Abstract:

The sources of uncertainty were analyzed for the determination of zinc in oyster by microwave digestioninductively
coupled plasma optical emission spectrometry (ICP-OES). According to JJF 1059—1999, the sub-uncertainty
was calculated and used to obtain combined uncertainty and expanded uncertainty of the measurement results. The results
showed that the uncertainty was mainly derived from fitting to the standard curve, and repeated experiments of samples,
preparation of the standard solution, and sample weighing and volume had a nonneligible effect on it with relative standard
uncertainty values of 0.016, 0.004 7, 0.001 4, 0.002 2 and 0.000 8, respectively. In this study, the combined standard
uncertainty of the measurement results was 13.29 mg/kg, and the expanded uncertainty was 26.58 mg/kg (k = 2). The final
result of zinc content in oyster was (781.98 ± 26.58) mg/kg (k = 2, P = 95%).

Key words: uncertainty, zinc, ICP-OES, microwave digestion, oyster

中图分类号: