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通往无机化学分析物质量测量用 SI 可溯源一级传递标准的道路。

On the way to SI traceable primary transfer standards for amount of substance measurements in inorganic chemical analysis.

机构信息

Bundesanstalt für Materialforschung und -prüfung (BAM), Unter den Eichen 87, 12205, Berlin, Germany.

出版信息

Anal Bioanal Chem. 2023 Jul;415(16):3057-3071. doi: 10.1007/s00216-023-04660-4. Epub 2023 Apr 1.

Abstract

During its 25 years of existence, the Inorganic Analysis Working Group of the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM IAWG) has achieved much in establishing comparability of measurement results. Impressive work has been done on comparison exercises related to real-world problems in fields such as ecology, food, or health. In more recent attempts, measurements and comparisons were focused on calibration solutions which are the basis of most inorganic chemical measurements. This contribution deals with the question of how to achieve full and transparent SI traceability for the values carried by such solutions. Within this framework, the use of classical primary methods (CPMs) is compared to the use of a primary difference method (PDM). PDM is a method with a dual character, namely a metrological method with a primary character, based on the bundling of many measurement methods for individual impurities, which lead to materials with certified content of the main component. As in classical methods, where small corrections for interferences are accepted, in PDM, many small corrections are bundled. In contrast to classical methods, the PDM is universally applicable to all elements in principle. Both approaches can be used to certify the purity (expressed as mass fraction of the main element) of a high-purity material. This is where the metrological need of National Metrology Institutes (NMIs) for analytical methods meet the challenges of analytical methods. In terms of methods, glow discharge mass spectrometry (GMDS) with sufficient uncertainties for sufficiently small impurity contents is particularly noteworthy for the certification of primary transfer standards (PTS), and isotope dilution mass spectrometry (IDMS), which particularly benefits from PTS (back-spikes) with small uncertainties, is particularly noteworthy for the application. The corresponding relative uncertainty which can be achieved using the PDM is very low (< 10). Acting as PTS, they represent the link between the material aspect of the primary calibration solutions and the immaterial world of the International System of Units (SI). The underlying concepts are discussed, the current status of implementation is summarised, and a roadmap of the necessary future activities in inorganic analytical chemistry is sketched. It has to be noted that smaller measurement uncertainties of the purity of high-purity materials not only have a positive effect on chemical measurements, but also trigger new developments and findings in other disciplines such as thermometry or materials science. Primary Transfer Standards (PTSs) are the link between the immaterial world of the International System of Units (SI) and the material aspects of the primary calibration solutions.

摘要

在其 25 年的存在期间,咨询委员会的量值溯源:化学和生物学中的物质(CCQM IAWG)无机分析工作组在建立测量结果的可比性方面取得了很大成就。在与生态学、食品或健康等领域的实际问题相关的比较研究方面开展了令人印象深刻的工作。在最近的尝试中,测量和比较集中在校准溶液上,这些溶液是大多数无机化学测量的基础。本贡献探讨了如何为这些溶液所携带的值实现完全和透明的 SI 可溯源性的问题。在此框架内,将经典基准方法(CPMs)与使用基准差值方法(PDM)进行了比较。PDM 是一种具有双重特征的方法,即基于将许多测量方法用于单个杂质的组合的具有基准性质的计量学方法,这导致了具有认证主成分含量的材料。与接受小干扰校正的经典方法一样,在 PDM 中,许多小校正被捆绑在一起。与经典方法不同,PDM 原则上可普遍适用于所有元素。这两种方法都可用于认证高纯材料的纯度(表示为主元素的质量分数)。这就是国家计量研究院(NMIs)对分析方法的计量需求与分析方法的挑战相吻合的地方。就方法而言,对于足够小的杂质含量,具有足够小不确定性的辉光放电质谱法(GMDS)对于主要传递标准(PTS)的认证特别重要,而同位素稀释质谱法(IDMS)特别受益于具有小不确定性的 PTS(后峰),其应用也特别重要。使用 PDM 可以实现的相应相对不确定度非常低(<10)。作为 PTS,它们代表了初级校准溶液的物质方面与国际单位制(SI)的非物质世界之间的联系。讨论了基础概念,总结了当前实施情况,并勾勒出无机分析化学未来必要活动的路线图。需要注意的是,高纯材料纯度的测量不确定度较小不仅对化学测量有积极影响,而且还会在其他学科(如测温学或材料科学)中引发新的发展和发现。主要传递标准(PTS)是国际单位制(SI)的非物质世界与初级校准溶液的物质方面之间的联系。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/20e0/10287771/d32beecb1bd9/216_2023_4660_Fig1_HTML.jpg

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