金溶液中微量元素标准物质(GBW02797-GBW02800)的研制

IF 0.8 4区 工程技术 Q4 CHEMISTRY, ANALYTICAL Accreditation and Quality Assurance Pub Date : 2023-11-16 DOI:10.1007/s00769-023-01557-8
Jianying Zhang, Yanjie Cui, Tao Zhou, Jinzhuan Wang, Zanfang Zhu, Fangmei Liu, Guangyang Xiao, Jing Yu, Xinlei Wang, Boling Huang, Chun Li, Xingjiao Huang
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引用次数: 0

摘要

以ISO 17034和ISO指南35为基础,建立了测定2 mg/mL金溶液(0、1、5、10、20)ng/mL浓度水平)中23种微量元素的基质标准物质。以纯度为99.9995%的高纯金CRM GBW02793为原料,溶解后用多元素溶液掺杂制备候选rm。对于ICP-MS测量,研究和评估了基质匹配和内标校准。检出限(lod)为0.002 ~ 0.35 ng/mL。在96% ~ 108%范围内获得了满意的峰回收率,证明了测量的准确性。采用ICP-MS法进行均匀性和稳定性研究。统计分析表明,11个单元的元素分布良好,每个单元重复分析。此外,在室温下进行12个月的长期稳定性试验和在60℃和- 20℃下进行7天的短期稳定性试验均未发现明显的变化趋势。通过8个专家实验室的合作表征,每个浓度水平的RM分别为23个元素的质量分数进行了认证。采用CRM ERM-EB507进一步验证了表征中应用的所有测量方法。各实验室测量结果一致性较好,取与目标值一致的总体平均值作为认证值。此外,还综合考虑了不均匀性(ubb)、不稳定性(us)和赋值(uchar)的不确定性。所建立的均方根方法可确保纯金和黄金首饰中微量元素的分析结果可靠、可追溯。
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Development of Certified Reference Materials of Trace Elements in Gold Solution (GBW02797–GBW02800)

Based on ISO 17034 and ISO Guide 35, a new series of matrix reference materials for 23 trace elements in 2 mg/mL gold solutions with five concentration levels (0, 1, 5, 10 and 20) ng/mL were developed, respectively. High-purity gold CRM GBW02793 with purity of 99.9995 % used as raw material was dissolved and then doped with multi-element solutions to prepare the candidate RMs. For ICP-MS measurements, matrix-matched and internal standard calibrations were studied and evaluated. The limits of detection (LoDs) ranged from 0.002 to 0.35 ng/mL. The satisfactory spike recoveries from 96 % to 108 % were obtained, demonstrating the measurement trueness. The ICP-MS method was also applied in the homogeneity and stability study. The statistical analysis suggested that the elements were well distributed by measuring 11 units with duplicate analysis for each. Besides, no significant trends were observed in the long-term stability test at room temperature for 12 months or in the short-term stability test at 60 ℃ and − 20 ℃ for 7 days. Through collaborative characterization by eight expert laboratories, the RM at each concentration level was certified for the mass fractions of 23 elements, respectively. All applied measurement methods in the characterization were further validated by using CRM ERM-EB507. The measurement results from all laboratories showed great consistency, and the overall mean values which were consistent with the target values were used as the certified values. Additionally, uncertainties arising from inhomogeneity (ubb), instability (us) and value assignment (uchar) were comprehensively combined. The developed RMs would ensure reliable and traceable analytical results of trace elements in fine gold and gold jewelry.

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来源期刊
Accreditation and Quality Assurance
Accreditation and Quality Assurance 工程技术-分析化学
CiteScore
1.80
自引率
22.20%
发文量
39
审稿时长
6-12 weeks
期刊介绍: Accreditation and Quality Assurance has established itself as the leading information and discussion forum for all aspects relevant to quality, transparency and reliability of measurement results in chemical and biological sciences. The journal serves the information needs of researchers, practitioners and decision makers dealing with quality assurance and quality management, including the development and application of metrological principles and concepts such as traceability or measurement uncertainty in the following fields: environment, nutrition, consumer protection, geology, metallurgy, pharmacy, forensics, clinical chemistry and laboratory medicine, and microbiology.
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