国家地质实验测试中心
扫 描 看 全 文
李松, 饶竹, 郭晓辰, 等. 地下水中有机磷农药测量方法准确度的质量评价[J]. 分析测试学报, 2014,33(11):1237-1243.
Quality Evaluation on the Determination Method Accuracy of Organophosphorus Pesticides in Groundwater[J]. 2014,33(11):1237-1243.
采用5个浓度水平样品、通过7家实验室进行协同评定试验,验证了地下水中敌敌畏、甲拌磷、乐果、甲基对硫磷、马拉硫磷、毒死蜱、对硫磷等有机磷农药分析方法的稳定性与准确性。地下水中有机磷组分选用二氯甲烷与丙酮混合溶液(丙酮溶液的比例约为5%)进行液液萃取,利用气相色谱火焰光度检测器进行检测。每一浓度级别的水溶液样品分别进行3组全过程检测。由于个别实验室或数据可能与其他实验室或其他数据明显不一致从而影响统计处理,因此对这些数值进行了一致性和离群值检验,并应用柯克伦和格拉布斯法则对测量方法与结果的准确度进行了确定。结果表明,地下水中,7种有机磷农药在20~2 000 ng/L浓度范围内,经柯克伦法则与格拉布斯法则检验,参与统计的个别测量数据因离群被剔除后计算结果较好。协同验证试验中,有机磷各组分在5个浓度水平的基体加标平均回收率为91.1%~109%,相对标准偏差为2.2%~12.6%,各样品中替代物磷酸三苯酯的回收率为77.8%~119%,方法准确、可靠。
In this paper,the stability and accuracy of determination method for dichlorvos,phorate,dimethoate,methyl-parathion,malathion,chlorpyrifos and parathion in groundwater were verified by a balanced uniform-level experiment involving five concentration levels and seven laboratories collaboration.Seven organophosphorus pesticides were extracted from groundwater with dichloromethane solution containing about 5% acetone,and the quantitative analysis of organophosphorus pesticides was carried out by gas chromatography with flame photometric detector.The whole analysis processes in every research laboratory and every sample level gave three results for statistics.The presence of individual laboratories or values that appeared to be inconsistent with all other laboratories or values may change the estimates,therefore,decisions have to be made with respect to these values.The balanced uniform-level experiment can provide a deterministic way to prove the accuracies(trueness and precision) of determination method and result by Cochran-test and Grubbs-test methods.The scrutiny of statistical results of seven organophosphorus pesticides in groundwater for consistency and outliers showed that the determination method was stable within a level range of 20-2 000 ng/L after eliminating the outlier data.The average recoveries of determination method for these organophosphorus in different levels were in the range of 91.1%-109% with relative standard deviations of 2.2%-12.6%.The surrogate recoveries for triphenyl phosphate during the analysis process were 77.8%-119%.The detection method is accurate and reliable.
质量评价有机磷农药平衡均匀水平试验重复性限再现性限
quality evaluationorganophosphorus pesticidesbalanced uniform-level experimentrepeatability limitreproducibility limit
0
浏览量
1165
下载量
0
CSCD
关联资源
相关文章
相关作者
相关机构