EN71-3方法确认

Linearity(线性)(ForICP-OES)（AN-0160）1Scope(目的)ThepurposeofthisvalidationistoestimatethelinearityofSolubleelementsforEN71-3(ISO8124/ASTMF963-2003)withICP-OES.本实验目的是来确认用ICP测定可迁移元素的线性。2Procedure(过程)2.1Prepareaseriesofstandardsolutionsasbelow:0.1mg/L,0.2mg/L,0.4mg/L,1.0mg/L,2.0mg/LforAs,Hg,Sb,Se0.5mg/L,1.0mg/L,2.0mg/L,5.0mg/L,10.0mg/LforBa,Pb,Cd,Cr配制一系列的标准溶液如下：砷，汞，锑，硒为0.1mg/L,0.2mg/L,0.4mg/L,1.0mg/L,2.0mg/L钡，铅，铬，镉为0.5mg/L,1.0mg/L,2.0mg/L,5.0mg/L,10.0mg/L2.2AnalyzethesolutionsassampleswithICP-OES.用ICP来分析上述溶液。2.3Calculatethecorrelationcoefficient(R)withminimumrequirementofR0.995.检验其标准曲线的相关系数（R）达到最低要求：R0.995。3Results(结果)ThelinearityofAs,Hg,Sb,Se,Ba,Pb,Cd,Crin0.07NHCLAs,Hg,Sb,Se,Ba,Pb,Cd,Cr在0.07NHCL中的线性范围ConcentrationofAsstandardworkingsolutions(ppm)Intensity(c/s)ConcentrationofBastandardworkingsolutions(ppm)Intensity(c/s)0.1163.8320.5621730.2304.49211203780.4611.61224333111470.58558303322960.14101155306ConcentrationofCdstandardworkingsolutions(ppm)Intensity(c/s)ConcentrationofCrstandardworkingsolutions(ppm)Intensity(c/s)0.538905.70.535531.2175553.9170354.221528072141176537499553478591072301010650584ConcentrationofPbstandardworkingsolutions(ppm)Intensity(c/s)ConcentrationofHgstandardworkingsolutions(ppm)Intensity(c/s)0.52264.640.1454.52114415.190.2887.70528858.630.41738.74521858.914421.651043296.328757.17ConcentrationofSbstandardworkingsolutions(ppm)Intensity(c/s)ConcentrationofSestandardworkingsolutions(ppm)Intensity(c/s)0.1255.790.1154.0190.2462.1930.2281.5010.4879.1910.4564.16912138.6511407.6624254.2322868.31ThegraphofAsconcentration(0.1ppmto2ppm)againstIntensityR=0.99990.01000.02000.03000.04000.000.511.522.5Concentration(ppm)Intensity(c/s)ThegraphofBaconcentration(0.5ppmto10ppm)againstIntensityR=0.99990.0300000.0600000.0900000.01200000.0024681012Concentration(ppm)Intensity(c/s)ThegraphofCdconcentration(0.5ppmto10ppm)againstIntensityR=0.99970.0200000.0400000.0600000.0800000.0024681012Concentration(ppm)Intensity(c/s)ThegraphofCrconcentration(0.5ppmto10ppm)againstIntensityR=0.99940.0200000.0400000.0600000.0800000.0024681012Concentration(ppm)Intensity(c/s)ThegraphofPbconcentration(0.5ppmto10.0ppm)againstIntensityR=1.00000.012000.024000.036000.0024681012Concentration(ppm)Intensity(c/s)ThegraphofHgconcentration(0.1ppmto2.0ppm)againstIntensityR=1.00000.02500.05000.07500.010000.000.511.522.5Concentration(ppm)Intensity(c/s)ThegraphofSbconcentration(0.1ppmto2.0ppm)againstIntensityR=1.00000.01200.02400.03600.000.511.522.5Concentration(ppm)Intensity(c/s)ThegraphofSeconcentration(0.1ppmto2.0ppm)againstIntensityR=0.99990.0800.01600.02400.03200.000.511.522.5Concentration(ppm)Intensity(c/s)4Conclusion(结论).ThecalibrationcurveislinearwithR0.995forBa,Pb,Cd,Crfrom0.5ppmto5ppm;As,Hg,Sb,Sefrom0.1ppmto2.0ppm.最终确认在0.07N盐酸中的砷，汞，锑，硒其线性范围0.1ppm到5ppm，钡，铅，铬，镉其线性范围0.05ppm到10ppm均达到R0.995。注：根据CPSD-AN-00003-MTHD要求，现行使用砷，汞，锑，硒0.2ppm,0.4ppm,1.0ppm和钡，铅，铬，镉1.0ppm,2.0ppm,5.0ppm作为校准工作曲线。Instrumentdetectionlimit(仪器检出限)1Scope(目的)Thepurposeofthisvalidationistodeterminetheinstrumentdetectionlimit(IDL)ofsolubleelementsforEN71-3(ISO8124/ASTMF963-2003)withICP-OES.做仪器检出限的目的是来确认仪器对可迁移元素元素的检出限.2Procedure(过程)2.1PlacethereagentblanktotheICP将试剂空白打入ICP中。2.2Takeaseriesofsevenreplicatemeasurementsforsolubleelements重复读7次试剂空白，记录可迁移元素的强度。2.3AnalyzethesevenreplicatesandcalculatetheIDLas1.645×standarddeviation.分析这七次重复测量值并计算理论仪器检出限（等于1.645×标准偏差）。2.4VerifythecalculatedIDLuntilthesignaltonoiseratioreaches3:1.校验仪器检出限直到信背比为3：1。3Results(结果)TheIDLofSolubleelementsin0.07NHCl可溶出元素在0.07N盐酸中的仪器检出限TrialMeasuredAs(mg/L)MeasuredBa(mg/L)MeasuredCd(mg/L)MeasuredCr(mg/L)MeasuredHg(mg/L)MeasuredPb(mg/L)MeasuredSb(mg/L)MeasuredSe(mg/L)1-0.00190.0000-0.0001-0.0004-0.00130.00000.00600.005220.00130.0000-0.0002-0.0003-0.0013-0.00190.00030.00393-0.0022-0.0001-0.0001-0.0002-0.0002-0.00070.0020-0.00194-0.0024-0.0001-0.0002-0.0003-0.0011-0.00150.00440.00555-0.00200.0000-0.0002-0.0002-0.0008-0.00080.00170.00076-0.0021-0.0002-0.0001-0.0002-0.0005-0.0010-0.0001-0.00787-0.00930.0000-0.0001-0.0003-0.0009-0.00140.0035-0.0058StandardDerivation0.00320.00010.00010.00010.0004140.00060.00220.005358InstrumentalDetectionLimit(1.645×SD)0.00530.00010.00010.00010.00070.00110.00360.008813VerifiedIDL0.03000.00080.00080.00080.01000.02000.05000.0400VerifiedIDLofAs,Hg,Sb,Se,Ba,Pb,Cd,Crin0.07NHCLAs,Hg,Sb,Se,Ba,Pb,Cd,C在0.07NHCL中的校验仪器检出限TrailCountBlankPb0.0200mg/LSignaltoNoiseRatio130.7716127.2624.14222.1958127.2625.73327.7183127.2624.59424.0611127.2625.29524.0826127.2625.28626.1864127.2624.86724.7588127.2625.14VerifiedIDLofPb0.0200mg/LTrailCountBlankAs0.0300mg/LSignaltoNoiseRatio113.724064.03264.67218.239664.03263.51313.248164.03264.83412.973264.03264.94513.523864.03264.73613.441264.03264.76715.066264.03264.25VerifiedIDLofAs0.0300mg/LTrailCountBlankBa0.0008mg/LSignaltoNoiseRatio147.6875152.8713.21239.5933152.8713.86330.4613152.8715.02434.1127152.8714.48544.3013152.8713.45622.7092152.8716.73743.0437152.8713.55VerifiedIDLofBa0.0008mg/LTrailCountBlankCd0.0008mg/LSignaltoNoiseRatio129.384791.42113.11218.010891.42115.0832