1、247572112916742204y=2187.4325x+26.3125R2=0.9999表3 镉的标准曲线测试数据1172745407991058y=1053.6923x+7.9575表4 铅的标准曲线测试数据164182123166y=165.3872x-0.4085表5 铅的标准曲线测试数据75178349517686y=685.2172x+3.27403. 方法检出限、测定下限测试数据表 连续进行20次空白溶液重复性测试,计算砷、铬、镉、铅、镍的检出限和测定下限,测试结果如下表6所示:表6 砷、铬、镉、铅、镍的检出限、测定下限测试数据平行号砷铬镉铅镍离子计数测定结果-221.17.
2、92.215.97.00.62.8-3.321.48.10.21.1-1.923.46.4-0.14.1-2.323.18.72.66-3.015.411.1-0.21.4722.39.11.98-3.126.12.79-2.218.68.41.510-2.723.2-0.32.011-1.512.9-1.14.31222.09.013-2.120.93.31424.08.3-1.825.710.726.310.2-1.24.51724.87.218-2.615.83.919-1.721.710.60.42.12019.88.84.4离子计数平均值21标准偏差3.81.31.0测定下限(mg/
3、L)0.0220.00520.00370.0180.0048测定下限(mg/kg)0.260.180.90.24检出限(mg/kg)0.280.0650.0450.220.064. 方法精密度测试数据对样品进行12次的重复性测试,计算砷、铬、镉、铅、镍的精密度,如表7-11所示:表7 砷的精密度测试数据含量(mg/kg)5.14.8534.125.8068.550.605.44.9533.325.2550.555.2033.425.3569.651.404.5025.3070.151.754.4534.526.1069.251.055.334.726.2569.050.955.1033.025
4、.0550.634.626.2068.44.733.925.6568.950.904.6526.1568.050.255.069.151.004.9033.725.5550.50平均值(mg/kg)3425.706950.850.410.42变异系数CV(%)1.81.60.870.83表8 铬的精密度测试数据253.81120.325.002188.149.40239.61125.825.152190.549.45234.64.751116.324.902183.849.301129.025.202148.748.5245.95.001114.62175.449.10238.51131.32
5、177.249.15240.51110.324.802198.149.65239.21110.62178.449.20237.04.801128.42166.448.90248.91119.52177.5233.51127.72193.749.55244.21120.92172.749.05平均值(mg/kg )241.01121.02179.05.90.147.30.1613.30.312.42.90.650.630.61表9 镉的精密度测试数据114.25.05526.724.601030.148.50113.2521.324.351023.448.20113.8522.924.45102
6、4.448.25112.3523.924.501022.248.15112.5521.21025.748.30114.7523.71021.648.10112.0525.824.551021.5112.8523.51022.4111.4520.324.301022.5525.1527.024.651029.6111.8525.41025.611350.0052410240.113.00.880.090.440.29表10 铅的精密度测试数据16.75.1583.1164.915.780.0163.915.581.224.70164.849.9515.24.7082.549.7016.979.1
7、24.05165.650.2082.3163.815.182.625.10163.117.05.2580.4162.216.381.4165.7162.314.64.5581.824.85162.715.681.91640.81.20.360.374.81.461.450.73表11 镍的精密度测试数据70.8339.3670.748.7070.9338.4664.470.4338.0668.848.5572.6341.1661.448.0070.2337.424.40669.848.654.9340.1659.447.9072.3340.3664.272.5341.8666.848.4033
8、8.7661.370.3339.1665.071.2342.224.75668.771.6340.4663.7713406650.070.270.450.565. 实际样品加标测试数据 以土壤为例,进行三次实际样品以及不同加标量的加标测试,计算加标回收率,如表12-16所示:表12 砷的实际样品加标测试数据样品样品含量(4.7mg)50.1(mg)(101.5mg)加标测定结果( mg )9.6100.3202.49.70202.59.7100.2平均值( mg )加标量( mg )50.0100.0加标回收率(%)100.4101.0备注表13 铬的实际样品加标测试数据4.7(mg)48.7
9、(mg)(99.6mg)98.6200.198.7199.998.70200.00表14 镉的实际样品加标测试数据5.0(mg)47.3(mg)(94.7mg)94.5189.29.594.6189.192.094.4表15 铅的实际样品加标测试数据5.4(mg)49.1(mg)(98.3mg)198.599.0198.79.499.1198.398.94.0102.599.6表16 镍的实际样品加标测试数据46.7(mg)(93.1mg)9.893.6187.094.1187.194.0187.593.9187.26. 方法验证结论6.1 以GB/T2704-2008方法测得砷的检出限为0.
10、28mg/kg,测定下限为1.1mg/kg;校准曲线回归方程的相关系数高于0.999;方法的精密度测试变异系数分别为5.1%、0.6%、0.83;对实际样品的加标回收率在100%-101之间,满足实验室质量控制的要求,本次验证结果有效。6.2 以GB/T2704-2008方法测得铬的检出限为0.065mg/kg,测定下限为0.26mg/kg;方法的精密度测试变异系数分别为2.9%、0.63%、0.63%;对实际样品的加标回收率在100%-100.4之间,满足实验室质量控制的要求,本次验证结果有效。6.3 以GB/T2704-2008方法测得镉的检出限为0.045mg/kg,测定下限为0.08m
11、g/kg;方法的精密度测试变异系数分别为0.09%、0.44%、0.29%;对实际样品的加标回收率在92.0%-94.5之间,满足实验室质量控制的要求,本次验证结果有效。6.4 以GB/T2704-2008方法测得铅的检出限为0.22mg/kg,测定下限为0.9mg/kg;方法的精密度测试变异系数分别为4.8%、1.45%、0.75%;对实际样品的加标回收率在99.6%-102.5%之间,满足实验室质量控制的要求,本次验证结果有效。6.5 以GB/T2704-2008方法测得镍的检出限为0.06mg/kg,测定下限为0.24mg/kg;方法的精密度测试变异系数分别为1.4%、0.45%、0.56%;对实际样品的加标回收率在94.0%-94.4%之间,满足实验室质量控制的要求,本次验证结果有效。
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