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Feasibility study of a candidate reference material for ions in PM 2.5 : does commutability matter also for inorganic matrices?
Analytical and Bioanalytical Chemistry ( IF 4.3 ) Pub Date : 2018-07-04 , DOI: 10.1007/s00216-018-1220-6
G. Emma , J. Snell , J. Charoud-Got , A. Held , H. Emons

The existing Air Quality Directive 2008/50/EC establishes within the European Union (EU) member states limit values for fine air particulate matter (PM2.5) including the possibility to discount natural sources of pollution when assessing compliance with the legislation. In proving this, EU member states shall determine, amongst others, the rural background concentration of some anions (Cl, NO3 and SO42−) and cations (Na+, NH4+, K+, Ca2+ and Mg2+). To deliver reliable data and to comply with the data quality objectives of the legislation, environmental control laboratories should use certified reference materials (CRMs) to validate or verify the performance of their analytical methods. Since no CRMs for anions and cations in PM2.5 are presently available, we present the commutability issues encountered during the first attempt to develop such a material. We demonstrate that a dust, collected in a road tunnel and previously used for the production of two CRMs of a PM10-like material, does not behave as an authentic fine particulate matter collected according to EN12341:2014 when measured by an established method proposed by the European Committee for Standardization (CEN/TR 16269:2011). The water-soluble fractions of SO42−, NH4+, K+, Ca2+ and Mg2+ in a PM2.5-like candidate CRM produced from that road tunnel dust are only fully extracted after 3 h of sonication and not after 30 min, as stated in the method. Moreover, we found that the particle size of the test material influenced the extraction yield of K+, Ca2+ and Mg2+, suggesting that these ionic species were incorporated in the core of the particles and inaccessible to the extraction procedure. These particular features make the material unsuitable for the measurements of ions with the CEN method. The difference in the extraction time can be seen as a commutability issue and the candidate CRM should be considered as not commutable with routine samples. This demonstrates that commutability studies should not only be considered for clinical CRMs, but also for inorganic CRMs when they are intended to be used to quantify operationally defined analytes.

中文翻译:

PM 2.5中离子候选参比材料的可行性研究:可交换性对无机基质也很重要吗?

现有的《空气质量指令2008/50 / EC》在欧盟(EU)成员国内确定了细小空气颗粒物(PM 2.5)的限值,包括在评估法规遵从性时可以打折自然污染源的可能性。在此证明,EU成员国应确定,除其他外,一些阴离子的农村背景浓度(CL -,NO 3 -和SO 4 2-)和阳离子(Na +,NH 4 +,K +,钙2+和镁2+)。为了提供可靠的数据并遵守法规的数据质量目标,环境控制实验室应使用经认证的参考材料(CRM)来验证或验证其分析方法的性能。由于目前没有可用的PM 2.5中用于阴离子和阳离子的CRM,因此,我们介绍了在首次尝试开发这种材料时遇到的可交换性问题。我们证明,通过建议的既定方法进行测量时,在公路隧道中收集的灰尘以前曾用于生产类似于PM 10的材料的两个CRM,但这些灰尘并不表现为根据EN12341:2014收集的真实细颗粒物由欧洲标准化委员会(CEN / TR 16269:2011)。SO的水溶性部分如所述,从该公路隧道粉尘产生的PM 2.5样候选CRM中的4 2−,NH 4 +,K +,Ca 2+和Mg 2+仅在超声处理3小时后才被完全提取,而不是在30分钟后被完全提取。方法。此外,我们发现测试材料的粒径会影响K +,Ca 2+和Mg 2+的提取率。,表明这些离子种类被掺入了颗粒的核中,并且萃取过程难以接近。这些特殊功能使该材料不适合使用CEN方法进行离子测量。提取时间的差异可以看作是可交换性问题,应将候选CRM视为与常规样品不可交换。这表明,可交换性研究不仅应考虑用于临床CRM,还应考虑将无机CRM用于量化可操作定义的分析物时使用。
更新日期:2018-07-05
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