方法驗(yàn)證報(bào)告 項(xiàng)目陰離子表面活性劑 方法連續(xù)流動(dòng)注射亞甲基藍(lán)分光光度法 參加單位無錫市環(huán)境監(jiān)測中心站 參加人員及職稱施新鋒（助理工程師） 交報(bào)告日期2004.7.15 蓋章項(xiàng)目負(fù)責(zé)單位負(fù)責(zé)人及職稱交報(bào)告日期 蓋章一、儀器狀況（本驗(yàn)證主要儀器）儀器名稱規(guī)格型號(hào)性能狀況備注美國LACHAT流動(dòng)注射儀QuiKChem8000FIA優(yōu)良二、試樣說明試樣名稱試樣來源固定和保存方法標(biāo)準(zhǔn)溶液和考試樣品采用國家標(biāo)準(zhǔn)樣品實(shí)際水樣為本單位監(jiān)測的地表水和廢水加入氯仿保存三、全程序空白和加標(biāo)測試表1空白值測定測定次數(shù)12345678910測定結(jié)果(mg/l)0.05350.0500.05610.03850.04190.04510.05610.05120.01850.067空白均值(mg/l)0.04779標(biāo)準(zhǔn)差Sb0.013最低濃度XL=3×Sb039（采用0.1mg/l測定檢出限）表2檢出限測定最低濃度測定次數(shù)1234567測定結(jié)果(mg/l)0.1130.09950.1030.09750.09660.08900.0945標(biāo)準(zhǔn)差SWb0.0075檢出限D(zhuǎn)L=3.14×SWb0.024mg/l表3校準(zhǔn)曲線測定編號(hào)標(biāo)曲濃度(mg/l)峰面積(V.S)12.004.5021.001.8830.5000.7440.2000.24950.1000.065660.00-0.0159回歸方程у=-0.0334x2+0.583x+0.0483相關(guān)系數(shù)Γ=0.99977表4方法上限測定D測定次數(shù)123456測定值(mg/l)標(biāo)準(zhǔn)差SpP上限說明：該公式有誤。D-加標(biāo)量為方法檢出限的3～5倍t0.05(f)-概率為0.05自由度為f的單側(cè)臨界值（2.447）f-自由度Sp-加標(biāo)回收值的標(biāo)準(zhǔn)差四、精密度測定表5精密度測定測定結(jié)果(mg/l)試樣平行號(hào)0.1C0.5C0.9C備注10.1810.9551.68C=2.00mg/l20.1880.9261.7230.2011.041.7440.1780.9091.8250.1820.8931.5460.9531.87均平值(mg/l)0.1860.9461.73批內(nèi)標(biāo)準(zhǔn)偏差Swb0.0090.050.11變異系數(shù)CV％4.915.026.09表6實(shí)際樣品測定樣品測定結(jié)果(mg/l)樣品平行號(hào)地表水1（T4）地表水2（T5）廢水1（協(xié)新1#）廢水2（協(xié)新3#）10.1060.06970.2470.31920.1190.07880.2330.33430.1050.09130.2510.37540.1050.08610.2410.34450.1010.0890--------60.1050.0947--------平均值(mg/l)0.1070.08490.2430.343批內(nèi)標(biāo)準(zhǔn)偏差Swb0.0060.0090.0080.024變異系數(shù)CV％5.8110.83.26.9加標(biāo)回收率樣品含量0.2030.1880.4670.554加標(biāo)量0.1000.1000.2000.200回收量0.0960.1030.2240.211回收率％96103112106五、確定方法準(zhǔn)確度表7統(tǒng)一樣品測定樣品測定結(jié)果(mg/l)樣品平行號(hào)04409(0.361±0.016mg/l)7290708(0.796±0.034mg/l)10.3820.73720.3670.79030.3540.78240.347----50.3560.75760.3950.802平均值(mg/l)0.3670.774批內(nèi)標(biāo)準(zhǔn)偏差Swb0.0180.026變異系數(shù)CV％5.023.40表8方法比對結(jié)果樣品名稱廢水（協(xié)新1#）廢水（協(xié)新3#）廢水（中亞毛紡）流動(dòng)注射法mg/L0.2470.2330.3340.3440.1340.145常規(guī)法mg/L0.2510.2480.3360.3510.145