方法验证报告土壤砷、铬、镉、铅和镍的测定

1、方法确认报告方法名称：土壤 碑、铭、镉、铅和银的测定 电感耦合等离子体发射光谱法 HJ 350-2007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 .基本情况说明1.1 仪器配备情况仪器设备编号：410设备名称：电感耦合等离子体发射光谱仪型 号： ICAP7200 Radial使用部门：检验科1.2 方法内容标准号：HJ 350-2007展览会用地土壤环境质量评价标准GB/T 27404-2008实验室质量控制规范食品理化检测检测方法确认技术要求验证项目：1)标线测定；2)测定低限测定；3)检出限测定；4)精密度测 定；5)样品加标测定。2 .标准曲线测试数据分别绘制神

2、、铭、镉、铅、锲标准曲线，观察线性效果，如下表所示：表1神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y=69.4654x-1.7805相关系数R2=1.0000表2铭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=2187.4325x+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(c

3、ps)/1172745407991058标线公式y=1053.6923x+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y=165.3872x-0.4085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=685.2172x+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行20次空白溶

4、液重复性测试，计算神、铭、镉、铅、锲的检出限和 测定下限，测试结果如下表6所示：表6神、铭、镉、铅、馍的检出限、测定下限测试数据平行号神铭镉铅银离子计数 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.

5、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测定卜限（mg/L）0.0220.00520.00370.0180.0048测定卜限（mg/kg）1.10.260.180.90.24检出Pm ( mg/kg)0.280.0650.0450.220.064 .方法精

6、密度测试数据对样品进行12次的重复性测试，计算神、铭、镉、铅、锲的精密度，如表7-11所示：表7神的精密度测试数据平行号离了计 数含量(mg/kg)离了计 数含量(mg/kg)离了计 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

7、.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铭的精密度测试数据平行号离了计 数含量(mg/kg)离了计 数含量(mg/kg)离了计 数含量(mg/kg)测定结 果(mg/kg)1253.85.201120.325.0021

8、88.149.402239.64.901125.825.152190.549.453234.64.751116.324.902183.849.304239.64.901129.025.202148.748.55245.95.001114.624.902175.449.106238.54.851131.325.252177.249.157240.54.901110.324.802198.149.658239.24.851110.624.802178.449.209237.04.801128.425.202166.448.9010248.95.101119.525.002177.549.15112

9、33.54.751127.725.202193.749.5512244.25.001120.925.002172.749.05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 (衿2.42.90.650.630.610.63表9镉的精密度测试数据平行号离了计 数含量(mg/kg)离了计 数含量(mg/kg)离了计 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.

10、00522.924.451024.448.254112.34.95523.924.501022.248.155112.54.95521.224.351025.748.306114.75.05523.724.451021.648.107112.04.95525.824.551021.548.108112.85.00523.524.451022.448.159111.44.90520.324.301022.548.1510112.54.95525.124.551021.548.1011112.84.95527.024.651029.648.5012111.84.95525.424.551025.6

11、48.30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 (衿0.880.090.410.440.290.29表10铅的精密度测试数据平行号离了计 数含量(mg/kg)离了计 数含量(mg/kg)离了计 数含量(mg/kg)测定结 果(mg/kg)116.75.1583.125.25164.950.00215.74.8580.024.30163.949.65315.54.8081.224.70164.849.95415.24.7082.525.05163.949.70516.95.2079.124.0516

12、5.650.20615.54.8082.325.00163.849.65715.14.7082.625.10163.149.45817.05.2580.424.45162.249.15916.35.0581.424.70165.750.201016.95.2582.525.05162.349.201114.64.5581.824.85162.749.301215.64.8581.924.90163.149.40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 (为5.04.81.461.450.730.75表11馍的精

13、密度测试数据平行号离了计 数含量(mg/kg)离了计 数含量(mg/kg)离了计 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

14、.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 (衿1.31.40.440.450.180.565 .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神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

15、 (mg)样品含量1101.5mg)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加林量(mg )5.050.0100.0加标回收率(%100.0100.4101.0备注/表13铭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加林量(mg )5.050.0100.0加标回收率(%100

16、.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加林量(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

17、)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馍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加林量(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方法测得种的检出限为 0.28mg/kg ,测定下限为1.1mg/kg; 校准曲线回归方程的

18、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方法测得铭的检出限为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 0.08mg/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