液液萃取-GC%2fMS法测定水中硝基苯质量控制指标研究的论文.pdfVIP

萃取-GC/MS 法测定水中硝基苯质量控制指标研究1 [1] [1] [1] [2] 胡冠九 李娟 袁力 夏新 (1 国家环境保护地表水环境有机污染物监测分析重点实验室，江苏省环境监测中心 江苏 南京 210036 ； 2 中国环境监测总站 北京 100012 ) 摘要：本文采用液液萃取－气相色谱/质谱法，通过统计全 多家实验室的测定数据，对水中硝基苯测试的 平行样测定相对偏差、空白加标回收率、实际样品加标回收率、空白加标回收率平行样相对偏差以及样品 加标回收率平行样相对偏差5 个质控指标进行了研究，并给出了质控指标评价标准，提出在 率P 和γ均 为0.90 时，其平行样测定允许最大相对偏差应控制在11.0%；空白加标浓度为0.2-30 μg/L 时，回收率的 控制范围为 59%-113%；样品测定浓度为未检出、加标浓度在 0.25-50 μg/L 时，实际样品加标回收率控制 范围为56%-110%；空白加标、样品加标回收率平行样最大相对偏差应分别控制在10.0%和11.1%。在 率P 和γ均为0.95 时，其平行样测定允许最大相对偏差应控制在 13.5%；空白加标浓度为0.2-30 μg/L 时， 回收率的控制范围为 50%-122%；样品测定浓度为未检出、加标浓度在 0.25-50 μg/L 时，实际样品加标回 收率控制范围为49%-117%；空白加标、样品加标回收率平行样最大相对偏差应分别控制在12.6% 和14.6%。 关键词：硝基苯; 质控指标; 平行样相对偏差; 空白回收率; 样品回收率; 空白加标回收率平行样相对偏 差; 样品加标回收率平行样相对偏差 Research of quality control index for nitrobenzene in water determined by GC/MS followed by liquid-liquid extraction HU Guan-jiu [1] LI Juan [1] YUAN Li [1] XIA Xin [2] (1 Jiangsu Environmental Monitoring Center, Jiangsu, Nanjing, 2 10036; 2 China Environmental Monitoring Station, Beijing, 1000 12 ） Abstract: Five quality control index of nitrobenzene, including relative bias of duplicates, recovery of blank spike sample spike, relative bias of blank spike duplicates and relative bias of sample spike duplicates, were studied by evaluating data collected from many labs national-widely. The quality control index were produced . The results showed that when the probability of both P and were 0.90, the maximum relative bias of duplicates should be within 11.0%; the blank recovery should be within 59%-113% when the spiking concentration was 0.2-30μg/L; the sample recovery should be within 56%-110% when the nitrobenzene was not detected in all the samples and the spiking concentration was 0.25-50μg/L; the ma