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水質17種苯胺類化合物的測定液相色譜-三重四極桿質譜法ii目 次前言 ii1用圍 12范引文件 13法理 14擾消除 15劑材料 26器設備 3738析驟 49果算表示 610密和確度 8質保和量制 912物理 10附錄A(規(guī)性錄)法的出和定限 附錄B(資性錄)譜參條件 12附錄C(資性錄)法的密和確度 1411水質17種苯胺類化合物的測定液相色譜-三重四極桿質譜法本標準規(guī)定了測定水中17種苯胺類化合物的液相色譜-三重四極桿質譜法。4-2,4-3-4-2-3-2-2,6-2-甲基3,3'-2,6-二乙基苯胺等17種苯胺類化合物的測定。0l701~3μg/L0.4μg/L~12μg/L100ml(50倍10l160.07~0.1,測定0.028μg/L~0.4A。HJ/T91 HJ/T164 樣品經(jīng)過濾后直接進樣或經(jīng)陽離子交換固相萃取柱富集和凈化后進樣,用液相色譜-三重四極桿質譜分離檢測苯胺類化合物。根據(jù)保留時間和特征離子定性,內標法定量。227.1(5.)甲醇(CH3OH)乙醇(C2H5OH)甲酸(HCOOH)乙酸(CH3COOH)鹽酸:ρ(HCl)=1.19g/ml。氨水:ρ(NH3·H2O)=0.91g/ml,優(yōu)級純。(NaOH)。(Na2S2O3)1+1。φ(HCOOH)=0.005%。50.0μl1L3+97。用乙酸(5.4)和水按3:97體積比混合。1+9。用甲醇(5.1)和水按1:9體積比混合。c(NaOH)=1mol/L。稱取4g氫氧化鈉(5.7)溶于水中,用水稀釋至100ml。5+95。用氨水(5.6)和甲醇(5.1)按5:95體積比混合。1+9。用氨水(5.6)和甲醇(5.1)按1:9體積比混合。ρ=100mg/L~1000mg/L。-10ρ=1.00mg/L~10.0mg/L。(5.(523-10.01.00mg/L-10℃以下冷凍、避光保存,可保存1個月。ρ=100mg/L。推薦內標物為苯胺-d5,也可使用其他同位素物質。用標準物質配制,標準物質純度大于99.0%,用甲醇(5.1)溶解,在-10℃以下冷凍、避光保存。也可直接購買有證標準溶液,33參照制造商的產(chǎn)品說明書保存。ρ=1.00mg/L(。將內標貯備液(5.18)按需要用甲醇(5.1)稀釋,在-10℃以下冷凍、避光保存,可保存1個月。ρ=100。替代物為聯(lián)苯胺-d8,用標準物質配制,標準物質純度大于99.0%,用甲醇(5.1)溶解,在-10℃以下冷凍、避光保存。也可直接購買有證標準溶液,參照制造商的產(chǎn)品說明書保存。ρ=1.00參考濃度。將替代物貯備液(5.20)按需要用甲醇(5.1)稀釋,在-10℃以下冷凍、避光保存,可保存1個月?;旌闲完栯x子交換固相萃取柱:填料為苯磺酸化的聚苯乙烯-二乙烯基苯高聚物,150mg/6ml,或其他等效萃取柱。500mg/6濾膜:0.22μm0.45μm5.2599.99%。液相色譜-三重四極桿質譜儀:配有電噴霧離子源(ESI)31502.0mmC18()500ml10μl、50μl、100μl500、1.0。樣品按照JT91和JT146.5pH7~8pH7~8,每500l0g5.843d3,3'-5d7d44樣品(7.1)經(jīng)0.22μm濾膜(5.24)過濾,棄去至少1ml初濾液后,移取1.0ml過濾后的樣品于棕色進樣瓶中,加入10.0μl內標使用液(5.19),混勻待測。將混合型陽離子交換固相萃取柱(5.22)固定在固相萃取裝置(6.4)上,依次用10ml甲醇(5.1)10ml100ml(7.1)20.0μl3ml/min5ml4ml(5.25)107.0ml氨50℃11.0500μl1.0試樣V12.0ml),10.0μl(5.19)注1:不同的混合型陽離子交換固相萃取柱(5.22)對鄰苯二胺的回收率差異很大,若需凈化樣品中的鄰苯二胺等苯胺類化合物(2-硝基苯胺除外),可以選擇硅膠基質陽離子交換固相萃取柱1.0ml~5.0ml15.0ml氨水甲醇溶液Ⅱ(5.15),(5.22)相同。2:4d14d3:(5.9)pH3(5.2)0.45μmpH用實驗用水代替樣品,按照與試樣的制備(7.2)相同的步驟進行實驗室空白試樣的制備。流動相A:甲酸溶液(5.10),流動相B:甲醇(5.1),梯度洗脫程序見表1;流速:0.2ml/min;柱溫:40℃;進樣體積:10μl。55表1梯度洗脫程序時間(min)流動相A(%)流動相B(%)0.09550.595510.0109010.195515.0955離子源:電噴霧離子源(ESI),正離子模式。監(jiān)測方式:多反應監(jiān)測(MRM)。其余條件參見附錄B。校準52-3-10.050.0μg/L100200500μg/L10001.005.0010.0μg/L20.050.0μg/L100μg/L()1.0ml10.0μl(5.19),混勻待測。(.1(2-3-200μg/L20.0μg/L)。661—苯胺聯(lián)苯胺替代物硝基苯胺;14—3-氯苯胺;15—2-萘胺;16—2,6-二甲基苯胺;17—2-甲基-6-乙基苯胺;18—3,3'-二氯聯(lián)苯胺;19—2,6-二乙基苯胺。圖117種苯胺類化合物和內標物、替代物的總離子流色譜圖按照與標準曲線的建立(8.2.1)相同的儀器條件進行試樣(7.2)的測定。按照與試樣測定(8.3)相同的儀器條件進行空白試樣(7.3)的測定。12標化合物的保留時間與標準樣品中該目標化合物的保留時間的相對偏差的絕對值應小于(Kstd)2Ksam

A2100%A1

(1)式中:Ksam——樣品中目標化合物定性子離子的相對豐度,%;77A2——樣品中目標化合物二級質譜定性子離子的響應值;A1——樣品中目標化合物二級質譜定量子離子的響應值。AK 2100%Astd1

(2)式中:Kstd——標準樣品中目標化合物定性子離子的相對豐度,%;Astd2——標準樣品中目標化合物二級質譜定性子離子的響應值;Astd1——標準樣品中目標化合物二級質譜定量子離子的響應值。表2定性確證時相對離子豐度的最大允許偏差Kstd/%Ksam允許的偏差/%Kstd>50±2020<Kstd≤50±2510<Kstd≤20±30Kstd≤10±50樣品中苯胺類化合物的質量濃度(μg/L),按照公式(3)進行計算:i1iD式中:i——樣品中第i種苯胺類化合物的質量濃度,μg/L;1i——iμg/L;D——稀釋倍數(shù)。樣品中苯胺類化合物的質量濃度(μg/L),按照公式(4)進行計算:

(3)1iV1Di V

(4)式中:i——樣品中第i種苯胺類化合物的質量濃度,μg/L;1i——由標準曲線得到的試樣中第i種苯胺類化合物的質量濃度,μg/L;V1——試樣體積,ml;V——取樣體積,ml;D——稀釋倍數(shù)。88測定結果小數(shù)點后位數(shù)的保留與方法檢出限一致,最多保留三位有效數(shù)字。精密度62-3-10.0、100μg/L500μg/L,1.0010.0μg/L50.0μg/L61.5%~15%0.79%~11%0.55%~10%;2.2%~9.8%、3.2%~8.6%和3.1%~6.9%0.1~21.3/~17L和4.9~66.1g/~3、1.7μg/L~21μg/L和6.7μg/L~73μg/L。623100L和50010.0μg/L50.0μg/L61.1%~17%0.59%~19%4.8%~10%4.1%~8.3%1.5μg/L~21μg/L6.1μg/L~99μg/L2.1μg/L~28μg/L8.2μg/L~126。623100L和50010.0μg/L50.0μg/L61.0~8和0.8~56.8~12%1.3μg/L~28μg/L5.5μg/L~762.4μg/L~32μg/L10μg/L~117μg/L。62-3-0.4002.00μg/L10.0μg/L,0.0400.200μg/L1.00μg/L62.5%~16%3.6%~14%1.1%~14%;實驗室間相對標準偏差分別為4.6%~13%、3.4%~13%和5.0%~10%;重復性限分別為0.007μg/L~0.10μg/L、0.032μg/L~0.46μg/L和0.13μg/L~2.0μg/L;再現(xiàn)性限分別為0.008μg/L~0.11μg/L、0.039μg/L~0.89μg/L和0.20μg/L~3.0μg/L。6家實驗室對2-硝基苯胺和3-硝基苯胺的加標濃度為2.00μg/L和10.0μg/L,其余苯胺0.200μg/L1.00μg/L6驗室內相對標準偏差分別為1.7%~18%和2.1%~16%;實驗室間相對標準偏差分別為6.6%~13%4.9%~11%0.034μg/L~0.66μg/L0.14μg/L~2.1μg/L;0.046μg/L~0.77μg/L0.21μg/L~3.4。6家實驗室對2-硝基苯胺和3-硝基苯胺的加標濃度為4.00μg/L和20.0μg/L,其余苯胺990.400μg/L2.00μg/L6實驗室內相對標準偏差分別為1.4%~15%和1.1%~17%;實驗室間相對標準偏差分別為3.8%~16%6.8%~14%0.057μg/L~0.82μg/L0.27μg/L~5.1μg/L;0.062μg/L~1.6μg/L0.42μg/L~8.4μg/L。方法精密度匯總數(shù)據(jù)參見附錄C。準確度623100L和50010.0μg/L50.0μg/L6標回收率范圍分別為80.1%~112%和81.5%~105%,加標回收率最終值分別為90.6%±18.4%~98.4%±12.6%91.5%±15.2%~96.0%±9.4%。623100L和50010.0μg/L50.0μg/L6加標回收率范圍分別為77.7%~116%和80.0~107%,加標回收率最終值分別為87.8%±13.2%~96.8%±15.2%89.3%±15.8%~96.1%±11.2%。6家實驗室對2-硝基苯胺和3-硝基苯胺的加標濃度為2.00μg/L和10.0μg/L,其余苯胺0.200μg/L1.00μg/L6加標回收率范圍分別為75.0%~113%和70.4~107%,加標回收率最終值分別為82.8%±17.6%~90.9%±23.2%83.7%±17.0%~90.5%±17.0%。6家實驗室對2-硝基苯胺和3-硝基苯胺的加標濃度為4.00μg/L和20.0μg/L,其余苯胺0.400μg/L2.00μg/L6定:加標回收率范圍分別為70.8%~112%和69.2%~115%,加標回收率最終值分別為79.7%±11.0%~94.6%±22.6%83.2%±23.0%~91.8%±21.0%。方法準確度匯總數(shù)據(jù)參見附錄C。20(≤20/校準每批樣品應建立標準曲線,相關系數(shù)應≥0.995。20(≤20/20%1010平行樣每20個樣品或每批次(≤20個樣品/批)至少測定一個平行樣,平行樣的相對偏差應≤25%。20(≤20/70%~120%60%~120%之間。替代物采用固相萃取法時,每個樣品都需要加入替代物,替代物的加標回收率應在70%~120%之間。1111附錄A(規(guī)范性附錄)方法的檢出限和測定下限表A.1給出了本方法中目標化合物的方法檢出限和測定下限,固相萃取法以取樣體積為100ml(富集50倍)時計。表A.1方法的檢出限和測定下限序號化合物名稱英文名稱CAS編號直接進樣法固相萃取法檢出限(μg/L)測定下(μg/L)檢出限(μg/L)測定下1鄰苯二胺o-Phenylenediamine95-54-50.20.8——2苯胺Aniline62-53-30.20.80.020.083聯(lián)苯胺Benzidine92-87-50.20.80.0070.0284對甲苯胺p-Toluidine106-49-00.20.80.010.045鄰甲氧基苯胺o-Anisidine90-04-00.20.80.0070.0286鄰甲苯胺o-Toluidine95-53-40.10.40.0070.02874-硝基苯胺4-Nitroaniline100-01-60.20.80.0070.02882,4-二甲基苯胺2,4-Dimethylaniline95-68-10.20.80.0070.02893-硝基苯胺3-Nitroaniline99-09-2280.10.4104-氯苯胺4-Chloroaniline106-47-80.20.80.010.04112-硝基苯胺2-Nitroaniline88-74-43120.10.4123-氯苯胺3-Chloroaniline108-42-90.20.80.010.04132-萘胺2-Aminonaphthalene91-59-80.10.40.0070.028142,6-二甲基苯胺2,6-Dimethylaniline87-62-70.20.80.010.04152-甲基-6-乙基苯胺2-Methyl-6-ethylaniline24549-06-20.20.80.0080.032163,3'-二氯聯(lián)苯胺3,3'-Dichlorobenzidine91-94-10.31.20.0070.028172,6-二乙基苯胺2,6-Diethylaniline579-66-80.10.40.010.041212附錄B(資料性附錄)質譜參考條件a)噴霧電壓:5500V。b)離子源溫度:600℃。c)5Pa(60psi)。d)5Pa(60psi)。e)5Pa(35psi)。f)B.1表B.1目標化合物的多反應監(jiān)測條件序號化合物名稱母離子(m/z)子離子(m/z)駐留時間(s)去簇電碰撞室入碰撞室出碰撞電1鄰苯二胺109.192.1*0.03561072265.13352苯胺-d5(內標)99.082.1*0.03431253154.17413苯胺93.977.0*0.037811-12851.1-1464聯(lián)苯胺-d8(替代物)193.2174.1*0.0370111329148.111345聯(lián)苯胺185.0167.1*0.037971237141.26356對甲苯胺108.191.1*0.03611062865.111377鄰甲氧基苯胺124.1109.1*0.03561042492.13258鄰甲苯胺108.291.1*0.03611062865.111371313續(xù)表序號化合物名稱母離子(m/z)子離子(m/z)駐留時間(s)去簇電(V)碰撞室入口電壓(V)碰撞室出(V)碰撞電94-硝基苯胺139.1122.1*0.03601051992.1630102,4-二甲基苯胺122.1107.2*0.03731082379.1533113-硝基苯胺139.293.1*0.03561022476.1241124-氯苯胺127.993.2*0.03577823111.1933132-硝基苯胺139.0121.0*0.035510211590.91721143-氯苯胺128.093.1*0.03577823111.0933152-萘胺144.1127.1*0.03671023177.0550162,6-二甲基苯胺122.0105.3*0.03531012579.0329172-甲基-6-乙基苯胺136.191.1*0.0343101430117.11326183,3'-二氯聯(lián)苯胺253.1217.2*0.0375101130182.01441192,6-二乙基苯胺150.2105.1*0.03481142891.3732注1:帶*的為二級質譜的定量子離子,另一個為定性子離子。注2:對于不同質譜儀器,參數(shù)可能存在差異,測定前應將質譜參數(shù)優(yōu)化到最佳。1414附錄C()表C.1~表C.4和表C.5~表C.6分別給出了方法的精密度和準確度。表C.1空白樣品加標測定的精密度匯總表(直接進樣法)序號化合物名稱加標濃度(μg/L)總均值(μg/L)實驗室內相對標準偏差(%)實驗室間相對標準偏差(%)重復性限r(nóng)(μg/L)再現(xiàn)性限R(μg/L)1鄰苯二胺1.001.01.7~8.25.90.10.210.010.11.8~9.94.51.72.050.049.31.4~9.33.47.78.52苯胺1.001.03.7~9.39.80.20.310.010.11.4~7.56.81.62.450.049.42.1~7.05.46.39.43聯(lián)苯胺1.001.03.1~9.08.00.20.310.010.12.2~8.24.71.72.050.048.81.4~6.15.76.29.64對甲苯胺1.001.02.9~9.96.00.20.210.010.21.1~9.35.71.72.250.048.51.5~8.85.37.09.65鄰甲氧基苯胺1.001.02.0~9.54.10.20.210.010.00.93~8.15.01.62.050.048.80.57~5.93.16.06.96鄰甲苯胺1.001.01.8~6.32.20.10.110.010.31.6~8.93.21.71.850.049.21.4~7.83.76.67.874-硝基苯胺1.001.01.6~134.90.20.210.010.01.3~8.56.71.62.450.049.10.60~7.16.36.41082,4-二甲基苯胺1.001.01.8~113.60.20.210.010.12.8~9.23.91.41.750.048.20.55~5.73.64.96.71515續(xù)表序號化合物名稱加標濃度(μg/L)總均值(μg/L)實驗室內相對標準偏差(%)實驗室間相對標準偏差(%)重復性限r(nóng)(μg/L)再現(xiàn)性限R(μg/L)93-硝基苯胺10.0102.9~9.35.6221001012.4~9.74.617205004862.3~8.33.16673104-氯苯胺1.001.02.0~103.50.20.210.09.90.79~103.91.71.950.048.80.84~8.14.46.48.4112-硝基苯胺10.0105.2~107.0231001003.1~6.86.014215005031.6~6.33.55771123-氯苯胺1.001.03.3~137.90.20.310.09.81.4~7.44.31.31.750.048.92.0~7.54.26.98.5132-萘胺1.001.01.5~126.50.20.310.010.02.2~7.74.31.61.950.048.91.6~6.74.96.28.8142,6-二甲基苯胺1.001.01.6~145.00.20.210.09.91.4~9.35.01.72.150.049.12.3~7.45.36.59.3152-甲基-6-乙基苯胺1.001.02.8~128.60.20.310.09.71.5~6.48.61.42.650.047.61.4~7.96.95.811163,3'-二氯聯(lián)苯胺1.000.92.4~9.28.50.20.310.09.71.8~117.11.72.550.049.02.1~105.88.611172,6-二乙基苯胺1.001.01.5~158.20.30.310.09.91.2~117.31.82.650.049.01.1~104.79.4111616表C.2實際樣品加標測定的精密度匯總表(直接進樣法)序號化合物名稱樣品類型加標濃度(μg/L)總均值(μg/L)實驗室內相對(%)實驗室間相對(%)重復性限r(nóng)(μg/L)再現(xiàn)性限R(μg/L)1鄰苯二胺地表水10.09.42.7~174.82.22.450.046.33.1~6.84.16.78.2工業(yè)廢水10.08.81.0~9.97.51.72.450.044.72.4~159.010142苯胺地表水10.09.82.1~106.41.82.450.046.91.7~175.81213工業(yè)廢水10.010.21.4~6.38.71.32.750.047.82.6~128.59.4143聯(lián)苯胺地表水10.09.44.0~7.55.91.52.150.047.21.7~196.11314工業(yè)廢水10.09.42.2~146.82.22.750.047.81.9~147.811144對甲苯胺地表水10.09.61.3~9.77.61.72.650.047.01.1~175.81112工業(yè)廢水10.09.31.4~11101.73.150.048.11.7~155.99.8125鄰甲氧基苯胺地表水10.09.72.5~156.82.12.750.047.21.1~9.66.37.711工業(yè)廢水10.09.32.1~12121.73.450.046.31.3~118.57.6136鄰甲苯胺地表水10.09.52.6~115.02.02.350.046.90.59~155.91113工業(yè)廢水10.09.32.0~168.42.43.150.046.41.8~147.98.11374-硝基苯胺地表水10.09.32.2~139.62.13.250.048.00.65~6.14.86.18.5工業(yè)廢水10.09.81.0~12121.73.750.047.11.8~7.19.55.91482,4-二甲基苯胺地表水10.09.81.5~145.92.12.550.046.42.2~105.77.910工業(yè)廢水10.09.81.1~187.02.42.950.047.71.4~107.77.4121717續(xù)表序號化合物名稱樣品類型加標濃度(μg/L)總均值(μg/L)實驗室內相對(%)實驗室間相對(%)重復性限r(nóng)(μg/L)再現(xiàn)性限R(μg/L)93-硝基苯胺地表水100964.2~7.65.316205004711.0~136.799126工業(yè)廢水100972.0~177.128325004681.1~7.87.276117104-氯苯胺地表水10.09.42.1~167.42.22.850.047.41.2~135.48.711工業(yè)廢水10.09.93.1~139.02.33.350.0472.0~8.79.17.314112-硝基苯胺地表水100954.0~117.621285004712.0~117.685126工業(yè)廢水100912.1~129.119295004633.7~7.87.067109123-氯苯胺地表水10.09.61.4~127.21.82.650.047.41.7~9.86.97.812工業(yè)廢水10.09.62.3~127.81.92.750.047.82.2~6.27.65.511132-萘胺地表水10.09.61.3~168.92.43.250.047.01.6~9.14.48.49.6工業(yè)廢水10.09.91.4~119.61.83.150.048.00.94~9.56.16.310142,6-二甲基苯胺地表水10.09.31.4~9.29.21.52.850.045.80.81~108.17.412工業(yè)廢水10.09.31.3~13111.73.450.046.41.1~8.2116.315152-甲基-6-乙基苯胺地表水10.09.22.1~118.51.62.650.046.41.3~8.17.47.212工業(yè)廢水10.09.11.2~8.48.81.32.550.045.61.7~8.6106.014163,3'-二氯聯(lián)苯胺地表水10.09.11.7~13101.52.950.045.81.8~8.88.37.913工業(yè)廢水10.09.12.9~129.71.83.050.046.01.1~159.99.516172,6-二乙基苯胺地表水10.09.31.1~13102.03.250.046.31.0~8.57.26.911工業(yè)廢水10.09.21.5~11121.43.350.046.00.68~7.78.86.1131818表C.3空白樣品加標測定的精密度匯總表(固相萃取法)序號化合物名稱加標濃度(μg/L)總均值(μg/L)實驗室內相對標準偏差(%)實驗室間相對標準偏差(%)重復性限r(nóng)(μg/L)再現(xiàn)性限R(μg/L)1苯胺0.0400.0377.7~138.60.0100.0130.2000.1766.9~9.06.00.0400.0471.000.9181.4~8.86.10.140.202聯(lián)苯胺0.0400.0386.9~106.70.0090.0110.2000.1744.0~115.20.0420.0461.000.9101.4~106.20.180.233對甲苯胺0.0400.0343.4~12120.0070.0130.2000.1694.2~8.88.00.0330.0481.000.8982.6~9.66.10.150.214鄰甲氧基苯胺0.0400.0352.6~13130.0090.0160.2000.1705.0~9.88.30.0340.0501.000.8961.4~7.88.90.140.265鄰甲苯胺0.0400.0362.7~128.80.0070.0110.2000.1703.6~9.07.20.0320.0451.000.8811.8~145.00.180.2164-硝基苯胺0.0400.0342.7~9.98.80.0070.0100.2000.1793.6~129.10.0440.0611.000.8801.9~8.36.90.150.2272,4-二甲基苯胺0.0400.0362.9~11110.0070.0130.2000.1733.8~116.50.0370.0461.000.8901.6~6.97.80.130.2383-硝基苯胺0.4000.363.6~165.00.100.102.001.744.0~12130.460.8910.09.133.0~109.52.03.01919續(xù)表序號化合物名稱加標濃度(μg/L)總均值(μg/L)實驗室內相對標準偏差(%)實驗室間相對標準偏差(%)重復性限r(nóng)(μg/L)再現(xiàn)性限R(μg/L)94-氯苯胺0.0400.0342.5~9.07.00.0070.0090.2000.1715.6~117.20.0400.0501.000.8632.7~8.19.10.160.26102-硝基苯胺0.4000.345.4~128.20.090.112.001.804.2~113.40.380.3910.09.483.9~9.27.61.82.6113-氯苯胺0.0400.0343.8~9.79.00.0070.0110.2000.1655.3~117.80.0350.0481.000.8482.7~9.88.70.160.25122-萘胺0.0400.0363.3~126.80.0090.0110.2000.1685.7~14100.0430.0621.000.8893.3~11100.150.30132,6-二甲基苯胺0.0400.0355.1~9.67.50.0080.0100.2000.1674.8~117.90.0360.0491.000.8542.1~108.10.150.24142-甲基-6-乙基苯胺0.0400.0353.4~9.06.00.0070.0080.2000.1684.6~105.00.0350.0391.000.8381.3~9.57.70.130.22153,3'-二氯聯(lián)苯胺0.0400.0342.9~104.60.0080.0080.2000.1683.8~136.20.0350.0431.000.8991.1~9.88.10.170.26162,6-二乙基苯胺0.0400.0353.8~9.2110.0070.0120.2000.1685.2~135.70.0370.0431.000.8952.1~7.96.60.140.212020表C.4實際樣品加標測定的精密度匯總表(固相萃取法)序號化合物名稱樣品類型加標濃度(μg/L)總均值(μg/L)實驗室內相對(%)實驗室間相對(%)重復性限r(nóng)(μg/L)再現(xiàn)性限R(μg/L)1苯胺地表水0.2000.1821.7~17130.0550.0831.000.9022.5~8.09.70.140.28工業(yè)廢水0.4001.271.7~13110.300.482.002.741.7~8.6110.430.942聯(lián)苯胺地表水0.2000.1753.8~149.40.0490.0651.000.8882.6~12110.190.32工業(yè)廢水0.4000.3314.0~105.80.0720.0852.001.782.9~7.66.80.270.423對甲苯胺地表水0.2000.1705.6~13130.0480.0751.000.882.2~117.20.150.22工業(yè)廢水0.4000.3313.4~128.80.0730.102.001.821.7~8.39.30.290.554鄰甲氧基苯胺地表水0.2000.1704.6~14110.0440.0671.000.9052.7~8.59.40.140.27工業(yè)廢水0.4000.3283.0~13100.0740.122.001.811.4~13100.360.605鄰甲苯胺地表水0.2000.1734.8~139.60.0460.0631.000.8872.3~8.36.80.160.22工業(yè)廢水0.4000.3334.2~115.70.0690.0832.001.811.1~137.30.330.4864-硝基苯胺地表水0.2000.1784.0~149.60.0430.0621.000.8873.8~119.80.170.29工業(yè)廢水0.4000.5433.0~8.8110.0950.182.002.003.3~159.70.500.7172,4-二甲基苯胺地表水0.2000.1744.2~129.30.0410.0591.000.8792.1~106.30.160.21工業(yè)廢水0.4000.4643.5~11120.0880.172.001.891.6~178.20.480.6283-硝基苯胺地表水2.001.765.3~189.80.660.7710.08.993.0~13112.13.4工業(yè)廢水4.003.453.3~13150.821.620.018.02.5~15145.18.42121續(xù)表序號化合物名稱樣品類型加標濃度(μg/L)總均值(μg/L)實驗室內相對(%)實驗室間相對(%)重復性限r(nóng)(μg/L)再現(xiàn)性限R(μg/L)94-氯苯胺地表水0.2000.1724.6~129.30.0440.0601.000.8812.8~9.4110.160.31工業(yè)廢水0.4000.6383.5~14110.130.242.002.005.2~8.9130.360.78102-硝基苯胺地表水2.001.743.4~15110.420.6410.08.442.3~128.21.62.4工業(yè)廢水4.003.382.0~15130.731.420.016.92.8~137.04.04.9113-氯苯胺地表水0.2000.1694.3~12120.0420.0671.000.8422.7~12100.190.30工業(yè)廢水0.4000.4843.0~12110.0930.172.001.824.2~13130.340.75122-萘胺地表水0.2000.1694.8~14110.0400.0631.000.8464.3~9.2110.170.31工業(yè)廢水0.4000.6922.0~10160.110.332.002.064.1~11140.400.88132,6-二甲基苯胺地表水0.2000.1683.1~139.60.0360.0561.000.8553.6~13110.210.32工業(yè)廢水0.4000.3191.4~136.80.0720.0902.001.723.2~128.00.400.53142-甲基-6-乙基苯胺地表水0.2000.1663.5~14110.0380.0601.000.8372.5~14100.210.30工業(yè)廢水0.4000.3214.3~125.20.0720.0802.001.693.8~127.70.350.48153,3'-二氯聯(lián)苯胺地表水0.2000.1673.0~166.60.0380.0461.000.8544.4~164.90.220.23工業(yè)廢水0.4000.3193.3~103.80.0570.0622.001.674.9~109.50.340.54162,6-二乙基苯胺地表水0.2000.1684.7~119.30.0340.0541.000.8683.8~9.98.70.170.26工業(yè)廢水0.4000.3364.9~155.90.0840.0952.001.713.4~11100.310.582222表C.5方法的準確度匯總表(直接進樣法)序號化合物名稱樣品類型樣品濃度(μg/L)加標濃度(μg/L)加標回收率(%)加標回收率P(%)加標回收率最終值P±2S(%)1鄰苯二胺地表水ND10.090.5~10294.494.4±9.050.087.6~97.992.592.5±7.6工業(yè)廢水ND10.080.6~97.587.887.8±13.250.083.2~10489.389.3±15.82苯胺地表水ND10.090.5~10998.498.4±12.650.086.8~10393.793.7±11.0工業(yè)廢水0.7~1.010.082.8~11494.194.1±23.250.084.1~10394.494.4±16.63聯(lián)苯胺地表水ND10.086.3~10294.494.4±11.250.085.8~10094.394.3±11.4工業(yè)廢水ND10.085.2~10194.294.2±12.850.084.6~10395.495.4±14.84對甲苯胺地表水ND10.086.4~10895.695.6±14.450.090.1~10494.194.1±10.8工業(yè)廢水ND10.084.1~10892.892.8±18.850.090.0~10396.196.1±11.25鄰甲氧基苯胺地表水ND10.091.2~11097.197.1±13.250.083.3~10094.494.4±12.0工業(yè)廢水ND10.077.7~11193.293.2±21.850.081.2~10292.592.5±15.46鄰甲苯胺地表水ND10.090.1~10295.195.1±9.450.083.0~97.893.993.9±11.0工業(yè)廢水ND10.084.8~10893.493.4±15.850.084.4~10292.792.7±14.474-硝基苯胺地表水ND10.083.0~11093.493.4±18.050.091.0~10196.096.0±9.4工業(yè)廢水0.2~0.310.084.2~11695.495.4±23.050.083.6~10393.593.5±17.482,4-二甲基苯胺地表水ND10.095.0~11098.298.2±11.650.084.3~99.692.792.7±10.4工業(yè)廢水0.1~0.310.091.7~11296.896.8±15.250.085.3~10295.295.2±15.893-硝基苯胺地表水ND10089.9~10595.895.8±10.250083.7~10194.294.2±12.6工業(yè)廢水ND10091.9~10696.696.6±13.850083.4~99.693.893.8±13.62323續(xù)表序號化合物名稱樣品類型樣品濃度(μg/L)加標濃度(μg/L)加標回收率(%)加標回收率P(%)加標回收率最終值P±2S(%)104-氯苯胺地表水ND10.088.9~10894.394.3±14.050.090.2~10294.794.7±10.2工業(yè)廢水0.3~0.510.081.1~10595.095.0±17.450.082.7~10393.493.4±17.4112-硝基苯胺地表水ND10083.2~10595.395.3±14.450083.8~10094.094.0±14.0工業(yè)廢水ND10081.5~10291.291.2±16.650082.7~99.792.692.6±12.8123-氯苯胺地表水ND10.088.3~10896.196.1±13.850.087.7~10394.794.7±13.0工業(yè)廢水0.210.088.1~10894.794.7±14.650.085.5~10295.295.2±14.2132-萘胺地表水ND10.086.7~11295.995.9±17.050.089.7~10294.194.1±8.6工業(yè)廢水0.3~0.510.084.7~11295.095.0±19.050.087.4~10295.095.0±11.6142,6-二甲基苯胺地表水ND10.085.7~10892.792.7±17.050.084.2~10591.691.6±14.8工業(yè)廢水ND10.084.7~11392.692.6±21.250.080.0~10792.692.6±20.0152-甲基-6-乙基苯胺地表水ND10.082.9~10592.192.1±15.650.083.6~10092.792.7±13.6工業(yè)廢水ND10.082.0~10491.491.4±16.050.080.2~10191.391.3±17.8163,3'-二氯聯(lián)苯胺地表水ND10.080.1~10690.690.6±18.450.081.5~99.491.591.5±15.2工業(yè)廢水ND10.081.1~10491.391.3±17.650.081.4~10492.192.1±18.2172,6-二乙基苯胺地表水ND10.083.7~11092.892.8±19.050.082.7~10192.592.5±13.4工業(yè)廢水ND10.079.1~11091.691.6±21.650.083.2~10292.192.1±16.4注:ND表示未檢出。2424表C.6方法的準確度匯總表(固相萃取法)序號化合物名稱樣品類型樣品濃度(μg/L)加標濃度(μg/L)加標回收率(%)加標回收率P(%)加標回收率最終值P±2S(%)1苯胺地表水ND0.20081.1~11390.990.9±23.21.0077.2~99.790.290.2±17.4工業(yè)廢水0.78~1.050.40082.4~11290.490.4±22.22.0081.2~10791.891.8±21.02聯(lián)苯胺-d8(替代物地表水ND0.20081.0~10694.894.8±21.2工業(yè)廢水ND0.20070.5~91.581.281.2±15.83聯(lián)苯胺地表水ND0.20077.0~10187.787.7±16.81.0079.5~10288.888.8±19.4工業(yè)廢水ND0.40074.2~88.182.782.7±9.82.008

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