水质分析用多组分挥发性有机物质量控制标准样品研究
Development of the certified reference material of volatile organic compounds
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摘要: 本文研制了适合我国水质环境监测和科学研究需要的28种组分挥发性有机物质量控制标准样品.该样品采用分组称量方法制备,随机抽取15瓶样品对其进行均匀性研究,结果表明样品均匀性良好.在室温、4 ℃冷藏和-18 ℃冷冻的3种保存条件下,采用线性模型进行稳定性研究,标准样品在15个月的稳定性检验期间未发现不稳定变化趋势.检验结果表明,制备的28种挥发性有机物质量控制标准样品均匀性和稳定性良好.9家实验室将该标准样品稀释至纯水中1000倍后,采用吹扫捕集-气相色谱-质谱法进行联合定值,经统计分析处理评定出标准值和不确定度,特性量值在24.14—58.83 μg·L-1之间,不确定度在2.04—13.77 μg·L-1之间,可以满足挥发性有机物水质分析质量保证与质量控制的要求.Abstract: This paper describes a method of developing CRM of 28 volatile organic compounds(VOCs) mixture in methanol for environmental monitoring. A good homogeneity was obtained by the testing for the 28 VOCs from 15 units selected by a random stratified scheme covering the whole batch, and 3 sub-samples were analyzed in each unit. At room temperature, 4 ℃ refrigeration and -18 ℃ freezing storage conditions, the concentration of 28 VOCs did not change during monitoring period of 15 months. The CRM was certified by 9 laboratories after the samples were diluted 1000 times with pure water. Based on the results from different analytical techniques including Puge & Trap/Gas-Chromatography/Mass spectrometry and Head-Space/Gas-Chromatography/Mass spectrometry by the 9 collaborating laboratories, values for 28 VOCs were in the range of 24.14—58.83 μg·L-1, expanded uncertainty of each VOC is 2.04—13.77 μg·L-1. The CRMs are suitable for VOCs monitoring in water and method validation.
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