方法驗(yàn)證報(bào)告土壤砷、鉻、鎘、鉛和鎳的測(cè)定

方法確認(rèn)報(bào)告方法名稱(chēng)："土壤砷、鉻、鎘、鉛和鎳的測(cè)定電感耦合等離子體發(fā)射光譜法"HJ350-2007驗(yàn)證人員：日期：審核人員：日期：報(bào)告編制人：日期：批準(zhǔn)人：日期：1.根本情況說(shuō)明1.1儀器配備情況儀器設(shè)備410設(shè)備名稱(chēng)：電感耦合等離子體發(fā)射光譜儀型號(hào)：ICAP7200Radial使用部門(mén)：檢驗(yàn)科1.2方法容標(biāo)準(zhǔn)號(hào)：HJ350-2007展覽會(huì)用地土壤環(huán)境質(zhì)量評(píng)價(jià)標(biāo)準(zhǔn)GB/T27404-2008實(shí)驗(yàn)室質(zhì)量控制規(guī)食品理化檢測(cè)檢測(cè)方法確認(rèn)技術(shù)要求驗(yàn)證工程：1〕標(biāo)線(xiàn)測(cè)定；2〕測(cè)定低限測(cè)定；3〕檢出限測(cè)定；4〕精細(xì)度測(cè)定；5〕樣品加標(biāo)測(cè)定。2.標(biāo)準(zhǔn)曲線(xiàn)測(cè)試數(shù)據(jù)分別繪制砷、鉻、鎘、鉛、鎳標(biāo)準(zhǔn)曲線(xiàn)，觀察線(xiàn)性效果，如下表所示：表1砷的標(biāo)準(zhǔn)曲線(xiàn)測(cè)試數(shù)據(jù)次數(shù)空白12345第一次標(biāo)線(xiàn)梯度〔mg/L〕/0.10.250.50.751離子計(jì)數(shù)〔cps〕/515335068標(biāo)線(xiàn)公式相關(guān)系數(shù)R2=1.0000表2鉻的標(biāo)準(zhǔn)曲線(xiàn)測(cè)試數(shù)據(jù)次數(shù)空白12345第一次標(biāo)線(xiàn)梯度〔mg/L〕/0.10.250.50.751離子計(jì)數(shù)〔cps〕/247572112916742204標(biāo)線(xiàn)公式y(tǒng)=2187.4325*+26.3125相關(guān)系數(shù)R2=0.9999表3鎘的標(biāo)準(zhǔn)曲線(xiàn)測(cè)試數(shù)據(jù)次數(shù)空白12345第一次標(biāo)線(xiàn)梯度〔mg/L〕/0.10.250.50.751離子計(jì)數(shù)〔cps〕/1172745407991058標(biāo)線(xiàn)公式y(tǒng)=1053.6923*+7.9575相關(guān)系數(shù)R2=0.9999表4鉛的標(biāo)準(zhǔn)曲線(xiàn)測(cè)試數(shù)據(jù)次數(shù)空白12345第一次標(biāo)線(xiàn)梯度〔mg/L〕/0.10.250.50.751離子計(jì)數(shù)〔cps〕/164182123166標(biāo)線(xiàn)公式相關(guān)系數(shù)R2=1.0000表5鉛的標(biāo)準(zhǔn)曲線(xiàn)測(cè)試數(shù)據(jù)次數(shù)空白12345第一次標(biāo)線(xiàn)梯度〔mg/L〕/0.10.250.50.751離子計(jì)數(shù)〔cps〕/75178349517686標(biāo)線(xiàn)公式y(tǒng)=685.2172*+3.2740相關(guān)系數(shù)R2=0.99993.方法檢出限、測(cè)定下限測(cè)試數(shù)據(jù)表連續(xù)進(jìn)展20次空白溶液重復(fù)性測(cè)試，計(jì)算砷、鉻、鎘、鉛、鎳的檢出限和測(cè)定下限，測(cè)試結(jié)果如下表6所示：表6砷、鉻、鎘、鉛、鎳的檢出限、測(cè)定下限測(cè)試數(shù)據(jù)平行號(hào)砷鉻鎘鉛鎳離子計(jì)數(shù)測(cè)定結(jié)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離子計(jì)數(shù)平均值-221903標(biāo)準(zhǔn)偏差0.53.81.31.01.1測(cè)定下限〔mg/L〕0.0220.00520.00370.0180.0048測(cè)定下限〔mg/kg〕1.10.260.180.90.24檢出限〔mg/kg〕0.280.0650.0450.220.064.方法精細(xì)度測(cè)試數(shù)據(jù)對(duì)樣品進(jìn)展12次的重復(fù)性測(cè)試，計(jì)算砷、鉻、鎘、鉛、鎳的精細(xì)度，如表7-11所示：表7砷的精細(xì)度測(cè)試數(shù)據(jù)平行號(hào)離子計(jì)數(shù)含量〔mg/kg〕離子計(jì)數(shù)含量〔mg/kg〕離子計(jì)數(shù)含量〔mg/kg〕測(cè)定結(jié)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標(biāo)準(zhǔn)偏差0.40.260.60.410.60.42變異系數(shù)CV(%)85.11.81.60.870.83表8鉻的精細(xì)度測(cè)試數(shù)據(jù)平行號(hào)離子計(jì)數(shù)含量〔mg/kg〕離子計(jì)數(shù)含量〔mg/kg〕離子計(jì)數(shù)含量〔mg/kg〕測(cè)定結(jié)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標(biāo)準(zhǔn)偏差5.90.147.30.1613.30.31變異系數(shù)CV〔%〕2.42.90.650.630.610.63表9鎘的精細(xì)度測(cè)試數(shù)據(jù)平行號(hào)離子計(jì)數(shù)含量〔mg/kg)離子計(jì)數(shù)含量〔mg/kg)離子計(jì)數(shù)含量〔mg/kg)測(cè)定結(jié)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標(biāo)準(zhǔn)偏差1.00.0452.20.113.00.14變異系數(shù)CV〔%〕0.880.090.410.440.290.29表10鉛的精細(xì)度測(cè)試數(shù)據(jù)平行號(hào)離子計(jì)數(shù)含量〔mg/kg)離子計(jì)數(shù)含量〔mg/kg)離子計(jì)數(shù)含量〔mg/kg)測(cè)定結(jié)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標(biāo)準(zhǔn)偏差0.80.241.20.361.20.37變異系數(shù)CV〔%〕5.04.81.461.450.730.75表11鎳的精細(xì)度測(cè)試數(shù)據(jù)平行號(hào)離子計(jì)數(shù)含量〔mg/kg)離子計(jì)數(shù)含量〔mg/kg)離子計(jì)數(shù)含量〔mg/kg)測(cè)定結(jié)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標(biāo)準(zhǔn)偏差0.90.071.50.111.20.27變異系數(shù)CV〔%〕1.31.40.440.450.180.565.實(shí)際樣品加標(biāo)測(cè)試數(shù)據(jù)以土壤為例，進(jìn)展三次實(shí)際樣品以及不同加標(biāo)量的加標(biāo)測(cè)試，計(jì)算加標(biāo)回收率，如表12-16所示：表12砷的實(shí)際樣品加標(biāo)測(cè)試數(shù)據(jù)平行號(hào)樣品樣品含量〔4.7mg〕樣品含量50.1〔mg〕樣品含量〔101.5mg〕加標(biāo)測(cè)定結(jié)果〔mg〕19.6100.3202.429.70100.3202.539.7100.2202.5平均值〔mg〕9.70100.3202.5加標(biāo)量〔mg〕5.050.0100.0加標(biāo)回收率〔%〕100.0100.4101.0備注/表13鉻的實(shí)際樣品加標(biāo)測(cè)試數(shù)據(jù)平行號(hào)樣品樣品含量4.7〔mg〕樣品含量48.7〔mg〕樣品含量〔99.6mg〕加標(biāo)測(cè)定結(jié)果〔mg〕19.698.6200.129.7098.7199.939.798.7199.9平均值〔mg〕9.798.70200.00加標(biāo)量〔mg〕5.050.0100.0加標(biāo)回收率〔%〕100.0100.0100.4備注/表14鎘的實(shí)際樣品加標(biāo)測(cè)試數(shù)據(jù)平行號(hào)樣品樣品含量5.0〔mg〕樣品含量47.3〔mg〕樣品含量〔94.7mg〕加標(biāo)測(cè)定結(jié)果〔mg〕19.694.5189.229.594.6189.239.694.5189.1平均值〔mg〕9.694.5189.2加標(biāo)量〔mg〕5.050.0100.0加標(biāo)回收率〔%〕92.094.494.5備注/表15鉛的實(shí)際樣品加標(biāo)測(cè)試數(shù)據(jù)平行號(hào)樣品樣品含量5.4〔mg〕樣品含量49.1〔mg〕樣品含量〔98.3mg〕加標(biāo)測(cè)定結(jié)果〔mg〕19.698.6198.529.599.0198.739.499.1198.3平均值〔mg〕9.598.9198.5加標(biāo)量〔mg〕4.050.0100.0加標(biāo)回收率〔%〕102.599.6100.2備注/表16鎳的實(shí)際樣品加標(biāo)測(cè)試數(shù)據(jù)平行號(hào)樣品樣品含量5.0〔mg〕樣品含量46.7(mg〕樣品含量〔93.1mg〕加標(biāo)測(cè)定結(jié)果〔mg〕19.893.6187.029.894.1187.139.594.0187.5平均值〔mg〕9.793.9187.2加標(biāo)量〔mg〕5.050.0100.0加標(biāo)回收率〔%〕94.094.494.1備注/6.方法驗(yàn)證結(jié)論6.1以GB/T2704-2008方法測(cè)得砷的檢出限為0.28mg/kg，測(cè)定下限為1.1mg/kg；校準(zhǔn)曲線(xiàn)回歸方程的相關(guān)系數(shù)高于0.999；方法的精細(xì)度測(cè)試變異系數(shù)分別為5.1%、0.6%、0.83；對(duì)實(shí)際樣品的加標(biāo)回收率在100%-101之間，滿(mǎn)足實(shí)驗(yàn)室質(zhì)量控制的要求，本次驗(yàn)證結(jié)果有效。6.2以GB/T2704-2008方法測(cè)得鉻的檢出限為0.065mg/kg，測(cè)定下限為0.26mg/kg；校準(zhǔn)曲線(xiàn)回歸方程的相關(guān)系數(shù)高于0.999；方法的精細(xì)度測(cè)試變異系數(shù)分別為2.9%、0.63%、0.63%；對(duì)實(shí)際樣品的加標(biāo)回收率在100%-100.4之間，滿(mǎn)足實(shí)驗(yàn)室質(zhì)量控制的要求，本次驗(yàn)證結(jié)果有效。6.3以GB/T2704-2008方法測(cè)得鎘的檢出限為0.045mg/kg，測(cè)定下限為0.08mg/kg；校準(zhǔn)曲線(xiàn)回歸方程的相關(guān)系數(shù)高于0.999；方法的精細(xì)度測(cè)試變異系數(shù)分別為0.09%、0.44%、0.29%；對(duì)實(shí)際樣品的加標(biāo)回收率在92.0%-94.5之間，滿(mǎn)足實(shí)驗(yàn)室質(zhì)量控制的要求，本次驗(yàn)證結(jié)果有效。6.4以GB/T2704-