Quality Assurance of Neutron Activation Analysis for the Determination of Atmospheric Particulate Matter Elements
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摘要: 仪器中子活化分析具有灵敏度高、无需样品预处理、可测元素种类多等优点,是大气颗粒物元素含量分析的常用方法之一,为污染源解析提供重要的数据基础。本文归纳整理了NAA实验室利用相对比较法和单比较器k0法分析大气颗粒物样品工作中各实验流程的质量保证过程,以及内、外部质量控制方法。Abstract: The instrumental neutron activation analysis has advantages including high sensitivity, no need for sample pretreatment, and a wide variety of measurable elements. It is one of the common methods for analyzing the element content of atmospheric particulate matter and can provide an important data basis for the analysis of pollution sources. This article summarizes the quality assurance process of each experimental process in the NAA laboratory using the relative comparison method and the single comparator k0 method to analyze atmospheric particulate matter samples, as well as internal and external quality control methods.
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表 1 大气颗粒物INAA分析的常用质量保证措施
Table 1. Quality assuarance for INAA of atmospheric particulate matter
实验室活动 误差来源 质量保证过程 样品制备 污染 在洁净间或层流清洁工作台处理APM样品,使用非金属
镊子进行操作,样品称量前在天平室环境中平衡至少24h。比较标准制备 同位素丰度差异,
比较标准使用不当比较标准中待测核素的丰度应与试样中的
保持一致;避免使用无证的比较标准。内部质量控制
物质制备质控物质使用不当 选用有证标准物质或单元素标准,在保存、
使用标准物质时,遵循标准物质使用说明。分析方案的选择 测量参数组合有误 测量前评估 高纯锗γ谱仪
性能控制性能不稳定,本底波动,高频干扰 利用刻度源进行性能参数验证,本底测
量,高压电源配件内部预防性清洁。测量 测量条件差异 保持测量架位 γ谱分析 峰拟合不当,干扰峰 对解谱软件进行性能检查,使用较小但无干扰的峰 校准 校准失效 制定校准方案,开展设备校准 表 2 大气颗粒物INAA分析质量监控计划
Table 2. Quality control plan for INAA of atmospheric particulate matter
监控方法 结果判定准则 监控频率 备注 标准样品分析 方法允许差 每次实验 内部质控 单比较器k0法与相对法比对 方法允许差 每次实验 内部质控 INAA与其他方法比对 方法允许差 1次/年 内部质控 人员比对 方法重复性 1次/半年 内部质控 实验室间比对/能力验证 方法允许差 1次/3年 外部质控 测量审核 组织方评价 1次/年 外部质控 -
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