方法验证报告土壤砷、铬、镉、铅和镍的测定

方法确认报告方法名称："土壤砷、铬、镉、铅和镍的测定电感耦合等离子体发射光谱法"HJ350-2007验证人员：日期：审核人员：日期：报告编制人：日期：批准人：日期：1.根本情况说明1.1仪器配备情况仪器设备410设备名称：电感耦合等离子体发射光谱仪型号：ICAP7200Radial使用部门：检验科1.2方法容标准号：HJ350-2007展览会用地土壤环境质量评价标准GB/T27404-2008实验室质量控制规食品理化检测检测方法确认技术要求验证工程：1〕标线测定；2〕测定低限测定；3〕检出限测定；4〕精细度测定；5〕样品加标测定。2.标准曲线测试数据分别绘制砷、铬、镉、铅、镍标准曲线，观察线性效果，如下表所示：表1砷的标准曲线测试数据次数空白12345第一次标线梯度〔mg/L〕/0.10.250.50.751离子计数〔cps〕/515335068标线公式相关系数R2=1.0000表2铬的标准曲线测试数据次数空白12345第一次标线梯度〔mg/L〕/0.10.250.50.751离子计数〔cps〕/247572112916742204标线公式y=2187.4325*+26.3125相关系数R2=0.9999表3镉的标准曲线测试数据次数空白12345第一次标线梯度〔mg/L〕/0.10.250.50.751离子计数〔cps〕/1172745407991058标线公式y=1053.6923*+7.9575相关系数R2=0.9999表4铅的标准曲线测试数据次数空白12345第一次标线梯度〔mg/L〕/0.10.250.50.751离子计数〔cps〕/164182123166标线公式相关系数R2=1.0000表5铅的标准曲线测试数据次数空白12345第一次标线梯度〔mg/L〕/0.10.250.50.751离子计数〔cps〕/75178349517686标线公式y=685.2172*+3.2740相关系数R2=0.99993.方法检出限、测定下限测试数据表连续进展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1-221.17.902.22-215.97.00.62.83-3.321.48.10.21.14-1.923.46.4-0.14.15-2.323.18.7-0.12.66-3.015.411.1-0.21.47-2.322.39.1-0.11.98-3.126.17.92.71.49-2.218.68.40.11.510-2.723.27.0-0.32.011-1.512.97.9-1.14.312-2.722.09.01.52.013-2.120.99.10.13.314-1.524.08.3-1.82.015-1.825.710.7-1.51.916-1.926.310.2-1.24.517-2.124.87.203.318-2.615.88.4-0.13.919-1.721.710.60.42.120-2.119.88.8-0.14.4离子计数平均值-221903标准偏差0.53.81.31.01.1测定下限〔mg/L〕0.0220.00520.00370.0180.0048测定下限〔mg/kg〕1.10.260.180.90.24检出限〔mg/kg〕0.280.0650.0450.220.064.方法精细度测试数据对样品进展12次的重复性测试，计算砷、铬、镉、铅、镍的精细度，如表7-11所示：表7砷的精细度测试数据平行号离子计数含量〔mg/kg〕离子计数含量〔mg/kg〕离子计数含量〔mg/kg〕测定结果(mg/kg)15.14.8534.125.8068.550.6025.44.9533.325.2568.550.5534.55.2033.425.3569.651.4044.44.5033.325.3070.151.7554.44.4534.526.1069.251.0565.34.4534.726.2569.050.9575.15.1033.025.0568.550.685.34.9534.626.2068.450.5594.75.1033.925.6568.950.90105.14.6534.626.1568.050.25115.04.9534.125.8069.151.00125.34.9033.725.5568.450.50平均值(mg/kg)55.103425.706950.85标准偏差0.40.260.60.410.60.42变异系数CV(%)85.11.81.60.870.83表8铬的精细度测试数据平行号离子计数含量〔mg/kg〕离子计数含量〔mg/kg〕离子计数含量〔mg/kg〕测定结果(mg/kg)1253.85.201120.325.002188.149.402239.64.901125.825.152190.549.453234.64.751116.324.902183.849.304239.64.901129.025.202148.748.55245.95.001114.624.902175.449.106238.54.851131.325.252177.249.157240.54.901110.324.802198.149.658239.24.851110.624.802178.449.209237.04.801128.425.202166.448.9010248.95.101119.525.002177.549.1511233.54.751127.725.202193.749.5512244.25.001120.925.002172.749.05平均值〔mg/kg〕241.04.901121.025.052179.049.20标准偏差5.90.147.30.1613.30.31变异系数CV〔%〕2.42.90.650.630.610.63表9镉的精细度测试数据平行号离子计数含量〔mg/kg)离子计数含量〔mg/kg)离子计数含量〔mg/kg)测定结果(mg/kg)1114.25.05526.724.601030.148.502113.25.00521.324.351023.448.203113.85.00522.924.451024.448.254112.34.95523.924.501022.248.155112.54.95521.224.351025.748.306114.75.05523.724.451021.648.107112.04.95525.824.551021.548.108112.85.00523.524.451022.448.159111.44.90520.324.301022.548.1510112.54.95525.124.551021.548.1011112.84.95527.024.651029.648.5012111.84.95525.424.551025.648.30平均值〔mg/kg〕11350.0052424.50102448.20标准偏差1.00.0452.20.113.00.14变异系数CV〔%〕0.880.090.410.440.290.29表10铅的精细度测试数据平行号离子计数含量〔mg/kg)离子计数含量〔mg/kg)离子计数含量〔mg/kg)测定结果(mg/kg)116.75.1583.125.25164.950.00215.74.8580.024.30163.949.65315.54.8081.224.70164.849.95415.24.7082.525.05163.949.70516.95.2079.124.05165.650.20615.54.8082.325.00163.849.65715.14.7082.625.10163.149.45817.05.2580.424.45162.249.15916.35.0581.424.70165.750.201016.95.2582.525.05162.349.201114.64.5581.824.85162.749.301215.64.8581.924.90163.149.40平均值〔mg/kg〕164.958224.8016449.65标准偏差0.80.241.20.361.20.37变异系数CV〔%〕5.04.81.461.450.730.75表11镍的精细度测试数据平行号离子计数含量〔mg/kg)离子计数含量〔mg/kg)离子计数含量〔mg/kg)测定结果(mg/kg)170.84.95339.324.50670.748.70270.94.95338.424.45664.448.25370.44.90338.024.45668.848.55472.65.05341.124.65661.448.00570.24.90337.424.40669.848.65670.84.9340.124.60659.447.90772.35.05340.324.60664.248.20872.55.05341.824.70666.848.40972.35.05338.724.50661.348.001070.34.90339.124.50665.048.301171.24.95342.224.75668.748.551271.65.00340.424.60663.748.20平均值〔mg/kg〕714.9534024.5566548.30标准偏差0.90.071.50.111.20.27变异系数CV〔%〕1.31.40.440.450.180.565.实际样品加标测试数据以土壤为例，进展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平行号样品样品含量〔4.7mg〕样品含量50.1〔mg〕样品含量〔101.5mg〕加标测定结果〔mg〕19.6100.3202.429.70100.3202.539.7100.2202.5平均值〔mg〕9.70100.3202.5加标量〔mg〕5.050.0100.0加标回收率〔%〕100.0100.4101.0备注/表13铬的实际样品加标测试数据平行号样品样品含量4.7〔mg〕样品含量48.7〔mg〕样品含量〔99.6mg〕加标测定结果〔mg〕19.698.6200.129.7098.7199.939.798.7199.9平均值〔mg〕9.798.70200.00加标量〔mg〕5.050.0100.0加标回收率〔%〕100.0100.0100.4备注/表14镉的实际样品加标测试数据平行号样品样品含量5.0〔mg〕样品含量47.3〔mg〕样品含量〔94.7mg〕加标测定结果〔mg〕19.694.5189.229.594.6189.239.694.5189.1平均值〔mg〕9.694.5189.2加标量〔mg〕5.050.0100.0加标回收率〔%〕92.094.494.5备注/表15铅的实际样品加标测试数据平行号样品样品含量5.4〔mg〕样品含量49.1〔mg〕样品含量〔98.3mg〕加标测定结果〔mg〕19.698.6198.529.599.0198.739.499.1198.3平均值〔mg〕9.598.9198.5加标量〔mg〕4.050.0100.0加标回收率〔%〕102.599.6100.2备注/表16镍的实际样品加标测试数据平行号样品样品含量5.0〔mg〕样品含量46.7(mg〕样品含量〔93.1mg〕加标测定结果〔mg〕19.893.6187.029.894.1187.139.594.0187.5平均值〔mg〕9.793.9187.2加标量〔mg〕5.050.0100.0加标回收率〔%〕94.094.494.1备注/6.方法验证结论6.1以GB/T2704-2008方法测得砷的检出限为0.28mg/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；方法的精细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；校准曲线回归方程的相关系数高于0.999；方法的精细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0.08mg/kg；校准曲线回归方程的相关系数高于0.999；方法的精细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-