《煤基液相酚類化合物的全測定全二維氣相色譜-質(zhì)譜/FID聯(lián)用》（征求意見稿）編制說明一、工作簡況1.1任務(wù)來源算焦油中的總酚含量（GB/T24207-2009）。利用4-氨基安替比林分光光度法（HJ503-2009，ASTMD1783-01測定出廢水中酚的總含量。通過氣相色譜分析得到工業(yè)酚油產(chǎn)品中不同酚化合物的含量（GB/T2601-2008）。通過氣相/液相色譜（HJ744-2015，ASTMD2580-06）分析得到廢水中十四種酚類化合物的含量，有明顯局限性。國家標準化管理委員會于2021年下達了制定計劃，制定計劃號：20214017-T-469。1.2工作過程的說明1.2.1預研階段2021年3月，根據(jù)國標委發(fā)〔2021〕3號文——《國家標準化管理委員會煤化工產(chǎn)品檢測方法分會秘書處組織開展了相關(guān)標準的申報1.2.2立項階段2021年6月，太原理工大學申報的《煤基液相酚類化合物的全測定全二該標準正式立項，標準由TC469（全國煤化工標準化技術(shù)委員會）歸口，TC469SC4（全國煤化工標準化技術(shù)委員會煤化工產(chǎn)品檢測方法分會）執(zhí)行。1.2.3起草階段源研究院、南京雪景科技有限公司等相關(guān)標準預研工作組單位成立了起草工作析條件及對應(yīng)的分析方法，并組織各協(xié)同單位開展協(xié)同實驗。書處組織開展全國煤化工標準化技術(shù)委員會煤化工產(chǎn)品檢測方法分技術(shù)委員會本次制定，嚴格按照GB/T20001.4《標準編寫規(guī)則第4部分：試驗方法2.5試驗方法全二維氣相色譜-質(zhì)譜/FID使用條件見表1。全二維調(diào)制器可以根據(jù)需要選（30m×0.25mm×0.25μm）（2.75m×0.1mm×0.1μm）He（純度不低于99.999%）300°C20:11mL/min初始溫度60°C，以3°C/min升至280°C300°C230°Cm/z45-200配置氫火焰離子化分別稱量各酚類化合物（5.4）組分，稱準至0.0001g。用甲醇溶解0.01mg/mL。配制的標準酚溶液中各酚類化合物的含量應(yīng)于待測樣品相近。標準混合物溶液B：準確稱量適量內(nèi)標物2,6-二氯），不同濃度標準混合溶液A溶解轉(zhuǎn)移至具刻度容量瓶中，再用標準混合溶液A定容至刻度。計算內(nèi)標物的濃度，精確至0.01mg/mL。2.5.3采用2mL注射器吸取1.5mL標準混合物溶液B，注入自動進樣器2mL……（1）RRFi——i組分的相對響應(yīng)值VCVi——i組分的峰體積；），計算內(nèi)標物的含量，精確至0.01mg/mL。析，通過FID色譜圖對定性出的不同酚類酚類化合物的相對響應(yīng)因子按其同分異構(gòu)體的平均相對響應(yīng)……（2）CVCV……（3）C）；C）；VVW=……（4）W——焦油樣品中鑒定出的不同酚類化合物的含量（mg/g）CV——初始稱量煤焦油的質(zhì)量（g）五、與有關(guān)的現(xiàn)行法律、法規(guī)和強制性國家標準的關(guān)系無六、重大分歧意見的處理經(jīng)過和依據(jù)七、國家標準作為強制性國家標準或推薦性國家標準的建議八、貫徹國家標準的要求和措施建議（包括組織措施、技術(shù)措施、過渡辦法等九、廢止現(xiàn)行有關(guān)標準的建議十、其他應(yīng)予說明的事項無2.簡述8家實驗室參與協(xié)同試驗，根據(jù)本標準草案所描述的測量方法對測試結(jié)果進行3.樣品的重復性編號物質(zhì)1（%）2（%）3（%）4（%）5（%）6（%）1苯酚2.122.232.042.392.192.012鄰甲酚3.173.353.313.213.043.293間甲酚+對甲酚5.294.874.965.014.885.3142,6-二甲酚1.341.291.181.201.341.1052,4-二甲酚0.971.041.101.150.981.0363-乙基酚0.850.780.820.840.790.9172,3-二甲酚0.240.200.180.220.190.2183,4-二甲酚0.370.310.290.330.380.2710間異丙基苯酚0.150.140.170.160.180.131110.200.270.230.190.180.22123,4,5-三甲基苯酚0.110.080.090.120.090.1013茚醇0.050.060.050.070.060.05141-萘酚0.090.110.100.090.120.11152-萘酚0.140.120.150.100.110.13表2.1#樣品的原始數(shù)據(jù)分析（第2家實驗室）編號物質(zhì)1（%）2（%）3（%）4（%）5（%）6（%）1苯酚2.352.412.522.312.442.392鄰甲酚3.433.313.293.223.483.353間甲酚+對甲酚5.445.035.095.115.295.3542,6-二甲酚1.391.421.431.491.511.4752,4-二甲酚1.051.081.131.211.091.1463-乙基酚0.960.850.930.900.850.9272,3-二甲酚0.210.240.230.210.200.2283,4-二甲酚0.440.410.390.460.430.4810間異丙基苯酚0.160.150.190.170.190.181110.240.280.250.230.200.21123,4,5-三甲基苯酚0.130.100.100.120.110.1513茚醇0.070.080.060.080.090.07141-萘酚0.110.120.110.130.120.15152-萘酚0.160.140.160.130.170.15表3.1#樣品的原始數(shù)據(jù)分析（第3家實驗室）編號物質(zhì)1（%）2（%）3（%）4（%）5（%）6（%）1苯酚2.031.982.112.172.092.192鄰甲酚3.092.982.872.912.813.013間甲酚+對甲酚4.874.984.754.854.914.9542,6-二甲酚1.031.090.971.120.941.0552,4-二甲酚0.960.920.871.061.080.9163-乙基酚0.880.890.910.820.840.9072,3-二甲酚0.190.210.240.200.210.2383,4-二甲酚0.400.390.410.420.390.3710間異丙基苯酚0.140.130.110.150.170.141110.210.190.180.200.210.19123,4,5-三甲基苯酚0.100.110.120.150.090.1313茚醇0.080.070.050.100.080.09141-萘酚0.090.110.100.120.130.10152-萘酚0.130.120.140.150.130.14表4.1#樣品的原始數(shù)據(jù)分析（第4家實驗室）編號物質(zhì)1（%）2（%）3（%）4（%）5（%）6（%）1苯酚2.252.162.182.092.302.192鄰甲酚3.463.653.573.613.523.513間甲酚+對甲酚5.014.994.985.125.095.1142,6-二甲酚1.091.111.141.061.291.1952,4-二甲酚1.020.980.951.041.051.0163-乙基酚0.910.920.890.900.930.9172,3-二甲酚0.210.220.240.190.220.2483,4-二甲酚0.420.410.380.440.400.3910間異丙基苯酚0.190.170.180.160.210.151110.220.250.200.210.200.22123,4,5-三甲基苯酚0.090.120.110.140.100.1213茚醇0.090.080.060.090.100.08141-萘酚0.120.100.110.130.120.11152-萘酚0.140.130.110.140.160.15表5.1#樣品的原始數(shù)據(jù)分析（第5家實驗室）編號物質(zhì)1（%）2（%）3（%）4（%）5（%）6（%）1苯酚2.392.302.312.292.422.442鄰甲酚3.313.393.443.293.493.303間甲酚+對甲酚4.874.894.874.854.794.9442,6-二甲酚0.960.930.911.011.040.9952,4-二甲酚0.960.950.911.051.010.9063-乙基酚0.870.910.930.900.890.8772,3-二甲酚0.190.200.230.180.210.1783,4-二甲酚0.410.390.370.400.390.4110間異丙基苯酚0.200.180.190.200.220.231110.200.210.190.180.190.20123,4,5-三甲基苯酚0.100.110.130.090.100.1413茚醇0.110.090.110.100.130.08141-萘酚0.110.120.090.100.090.13152-萘酚0.130.140.120.100.170.16表6.1#樣品的原始數(shù)據(jù)分析（第6家實驗室）編號物質(zhì)1（%）2（%）3（%）4（%）5（%）6（%）1苯酚2.232.312.342.302.322.332鄰甲酚3.393.313.403.213.373.313間甲酚+對甲酚4.784.804.824.784.804.9142,6-二甲酚1.021.040.981.051.070.9652,4-二甲酚0.910.930.951.021.090.9863-乙基酚0.880.910.920.930.900.8972,3-二甲酚0.170.190.200.180.210.2083,4-二甲酚0.400.380.360.390.370.4010間異丙基苯酚0.190.170.180.170.200.211110.190.220.210.160.150.18123,4,5-三甲基苯酚0.110.130.140.100.120.1313茚醇0.140.100.120.110.140.16141-萘酚0.090.110.100.130.120.11152-萘酚0.140.130.110.140.150.13表7.1#樣品的原始數(shù)據(jù)分析（第7家實驗室）編號物質(zhì)1（%）2（%）3（%）4（%）5（%）6（%）1苯酚2.342.372.432.282.212.192鄰甲酚3.313.393.423.193.293.333間甲酚+對甲酚4.854.794.874.714.734.8242,6-二甲酚0.960.910.930.991.020.9552,4-二甲酚0.900.870.850.811.020.9963-乙基酚0.910.870.930.940.880.9272,3-二甲酚0.160.180.190.170.200.1583,4-二甲酚0.390.420.370.400.390.4110間異丙基苯酚0.220.200.190.200.210.221110.200.210.190.170.160.17123,4,5-三甲基苯酚0.090.110.150.130.130.1213茚醇0.150.140.120.100.150.17141-萘酚0.100.120.110.140.130.12152-萘酚0.150.160.140.130.150.12編號物質(zhì)重復性限標準差重復性限r(nóng)再現(xiàn)性限標準差再現(xiàn)性限R1苯酚0.01330.03740.01450.04062鄰甲酚0.01550.04330.01670.04673間甲酚+對甲酚0.01370.03840.03080.086442,6-二甲酚0.06440.18030.07750.204952,4-二甲酚0.06680.18690.09090.254463-乙基酚0.03240.09060.04090.114572,3-二甲酚0.01860.05210.02360.065983,4-二甲酚0.02550.07140.04070.113910間異丙基苯酚0.01790.05010.02930.08191110.02220.06200.02760.0774123,4,5-三甲基苯酚0.01530.04290.01730.048313茚醇0.08560.23960.09630.2543141-萘酚0.08920.24980.09150.2542152-萘酚0.08080.24030.08580.2402表9.2#樣品的原始數(shù)據(jù)分析（第1家實驗室）編號物質(zhì)1(%)2(%)3(%)4(%)5(%)6(%)13.313.273.413.353.163.5322.172.132.312.142.062.33間甲酚+對甲酚4.254.384.174.424.224.3142,6-二甲酚1.161.131.081.251.061.1752,4-二甲酚0.870.930.880.950.840.7963-乙基酚0.430.400.470.380.510.4972,3-二甲酚0.510.530.390.570.620.4383,4-二甲酚0.390.380.390.410.430.371010.250.230.320.280.190.3113,4,5-三甲酚0.310.280.330.310.270.36122,3,5-三甲酚0.280.280.210.320.290.311350.170.130.190.160.210.1614茚醇0.090.110.070.090.120.111520.120.130.130.090.120.141630.040.030.050.040.040.06172-萘酚0.130.110.160.090.090.13181-萘酚0.090.090.110.120.100.071940.120.130.090.100.090.17表10.2#樣品的原始數(shù)據(jù)分析（第2家實驗室）編號物質(zhì)1(%)2(%)3(%)4(%)5(%)6(%)13.293.213.333.253.143.1122.152.072.192.172.012.313間甲酚+對甲4.234.014.214.194.354.42酚42,6-二甲酚1.091.060.991.081.061.1352,4-二甲酚0.920.950.920.870.960.9463-乙基酚0.430.430.390.430.500.4872,3-二甲酚0.490.510.490.410.520.4383,4-二甲酚0.390.310.290.370.430.471010.260.220.290.290.170.21113,4,5-三甲酚0.300.280.330.350.280.29122,3,5-三甲酚0.310.300.310.230.280.421350.160.130.130.140.210.0914茚醇0.090.110.110.130.070.111520.120.120.180.120.160.091630.040.030.040.060.040.04172-萘酚0.160.180.130.130.140.14181-萘酚0.130.110.140.170.110.131940.150.120.140.210.160.16表11.2#樣品的原始數(shù)據(jù)分析（第3家實驗室）編號物質(zhì)1(%)2(%)3(%)4(%)5(%)6(%)13.293.423.353.163.093.2122.192.162.312.172.092.193間甲酚+對甲酚4.254.214.094.364.414.2342,6-二甲酚1.131.190.991.061.211.1252,4-二甲酚0.880.920.820.870.790.9163-乙基酚0.430.460.510.300.370.3972,3-二甲酚0.490.410.430.460.530.5183,4-二甲酚0.400.390.430.470.390.321010.250.270.250.190.200.31113,4,5-三甲酚0.300.250.390.340.230.3122,3,5-三甲酚0.310.310.310.360.280.261350.170.180.170.140.170.2114茚醇0.080.090.060.110.100.091520.130.160.140.090.110.111630.040.060.050.050.030.04172-萘酚0.140.140.140.190.170.11181-萘酚0.090.080.110.130.090.061940.120.140.100.080.120.19表12.2#樣品的原始數(shù)據(jù)分析（第4家實驗室）編號物質(zhì)1(%)2(%)3(%)4(%)5(%)6(%)13.313.163.093.113.313.4522.152.122.152.162.152.013間甲酚+對甲酚4.174.174.024.344.294.3142,6-二甲酚1.161.051.211.181.161.1852,4-二甲酚0.860.890.910.860.730.7263-乙基酚0.380.320.290.370.430.3872,3-二甲酚0.540.520.510.540.540.6183,4-二甲酚0.350.320.370.340.350.351010.250.240.190.230.290.29113,4,5-三甲酚0.310.360.330.310.310.29122,3,5-三甲酚0.300.290.360.250.320.311350.160.170.170.130.190.1614茚醇0.070.070.050.080.080.11520.120.160.120.110.090.131630.050.040.050.050.070.03172-萘酚0.130.150.090.100.130.11181-萘酚0.070.070.090.060.070.081940.140.120.090.140.180.11表13.2#樣品的原始數(shù)據(jù)分析（第5家實驗室）編號物質(zhì)1(%)2(%)3(%)4(%)5(%)6(%)13.383.513.463.283.263.4522.152.012.382.242.182.163間甲酚+對甲酚4.414.614.354.294.424.4842,6-二甲酚1.131.121.131.321.031.0952,4-二甲酚0.870.830.870.940.790.863-乙基酚0.450.430.450.450.480.4772,3-二甲酚0.500.460.550.520.560.4983,4-二甲酚0.370.310.350.340.280.431010.280.210.290.240.310.31113,4,5-三甲酚0.330.380.310.370.420.35122,3,5-三甲酚0.270.290.210.270.290.191350.170.210.130.210.170.1714茚醇0.050.040.050.070.050.051520.130.130.160.090.140.141630.040.030.030.060.040.04172-萘酚0.140.160.130.130.180.11181-萘酚0.090.080.110.130.080.091940.120.130.090.1213.000.12表14.2#樣品的原始數(shù)據(jù)分析（第6家實驗室）編號物質(zhì)1(%)2(%)3(%)4(%)5(%)6(%)13.513.433.363.523.383.4122.192.162.092.062.192.313間甲酚+對甲酚4.044.164.094.214.194.2142,6-二甲酚1.161.061.161.081.211.2952,4-二甲酚0.890.930.910.830.860.9463-乙基酚0.400.420.460.400.490.3972,3-二甲酚0.500.460.520.590.500.4383,4-二甲酚0.390.320.370.430.480.391010.230.210.290.230.190.19113,4,5-三甲酚0.320.360.310.230.290.41122,3,5-三甲酚0.280.280.240.210.340.311350.190.180.160.210.190.2314茚醇0.080.110.070.080.110.081520.100.100.080.120.130.111630.040.030.040.060.040.05172-萘酚0.120.110.100.130.150.08181-萘酚0.090.060.080.090.070.111940.100.100.120.090.090.11表15.2#樣品的原始數(shù)據(jù)分析（第7家實驗室）編號物質(zhì)1(%)2(%)3(%)4(%)5(%)6(%)123.372.213.422.283.292.173.352.343.512.323.292.213間甲酚+對甲酚4.1