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Determination of trace elements in high-purity platinum by laser ablation inductively coupled plasma mass spectrometry using solution calibration

机译:溶液校准-激光烧蚀电感耦合等离子体质谱法测定高纯铂中的微量元素。

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摘要

Multi-element trace analysis by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) of high-purity metals, semiconductors and insulators (e.g., ceramics) is often limited by the lack of suitable standard reference materials (SRM) with the same matrix composition and also a lack of a significant number of certified trace element concentrations in the available SRMs. This paper describes a new and easy standard-free quantification strategy using solution-based calibration for the multi-element determination of trace impurities in high-purity platinum. For the mass spectrometric measurements, a quadrupole-based LA-ICP-MS instrument was coupled with an ultrasonic nebulizer (USN). Due to the lack of a high-purity blank platinum sample, quantification of the results of LA-ICP-MS measurements was carried out using the standard additions mode in solution-based calibration. In order to achieve matrix matching, the multi-element standard solutions (with different concentrations of analytes) were nebulized successively with a USN. Simultaneously the high-purity platinum target was ablated with a focused laser beam during solution calibration with the USN. The mass spectrometric method developed was validated using a platinum standard reference material (NIST SRM 681). The analytical results of the LA-ICP-MS of SRM 681 Platinum are in good agreement with the certified values. The relative standard deviation (RSD) of most elements (n=3) is between 2 and 10%. The proposed analysis method can be applied for other high-purity materials in a similar way, e.g., for trace and ultratrace analysis of high-purity metals, semiconductors and insulators such as high-purity ceramics.
机译:激光烧蚀电感耦合等离子体质谱法(LA-ICP-MS)对高纯度金属,半导体和绝缘体(例如陶瓷)进行的多元素痕量分析通常由于缺乏合适的标准参考材料(SRM)而受到限制。相同的基质组成,并且在可用的SRM中缺少大量的认证痕量元素浓度。本文介绍了一种基于溶液的校准方法,用于多元素测定高纯度铂中的痕量杂质,该方法简便易行,无需使用标准液即可进行定量。对于质谱测量,将基于四极杆的LA-ICP-MS仪器与超声雾化器(USN)耦合。由于缺乏高纯度的空白铂样品,因此在基于溶液的校准中使用标准添加模式对LA-ICP-MS测量结果进行了定量。为了实现基质匹配,用USN连续雾化多元素标准溶液(具有不同浓度的分析物)。同时,在用USN进行溶液校准期间,用聚焦的激光束烧蚀高纯度铂靶。使用铂标准参考材料(NIST SRM 681)验证了开发的质谱方法。 SRM 681铂金的LA-ICP-MS的分析结果与认证值完全一致。大多数元素(n = 3)的相对标准偏差(RSD)在2%至10%之间。所提出的分析方法可以类似的方式应用于其他高纯度材料,例如,用于高纯度金属,半导体和绝缘体(例如高纯度陶瓷)的痕量和超痕量分析。

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