煤基液相酚类化合物的全测定 全二维气相色谱-质谱FID联用 编制说明

《煤基液相酚类化合物的全测定全二维气相色谱-质谱/FID联用》（征求意见稿）编制说明一、工作简况1.1任务来源算焦油中的总酚含量（GB/T24207-2009）。利用4-氨基安替比林分光光度法（HJ503-2009，ASTMD1783-01测定出废水中酚的总含量。通过气相色谱分析得到工业酚油产品中不同酚化合物的含量（GB/T2601-2008）。通过气相/液相色谱（HJ744-2015，ASTMD2580-06）分析得到废水中十四种酚类化合物的含量，有明显局限性。国家标准化管理委员会于2021年下达了制定计划，制定计划号：20214017-T-469。1.2工作过程的说明1.2.1预研阶段2021年3月，根据国标委发〔2021〕3号文——《国家标准化管理委员会煤化工产品检测方法分会秘书处组织开展了相关标准的申报1.2.2立项阶段2021年6月，太原理工大学申报的《煤基液相酚类化合物的全测定全二该标准正式立项，标准由TC469（全国煤化工标准化技术委员会）归口，TC469SC4（全国煤化工标准化技术委员会煤化工产品检测方法分会）执行。1.2.3起草阶段源研究院、南京雪景科技有限公司等相关标准预研工作组单位成立了起草工作析条件及对应的分析方法，并组织各协同单位开展协同实验。书处组织开展全国煤化工标准化技术委员会煤化工产品检测方法分技术委员会本次制定，严格按照GB/T20001.4《标准编写规则第4部分：试验方法2.5试验方法全二维气相色谱-质谱/FID使用条件见表1。全二维调制器可以根据需要选（30m×0.25mm×0.25μm）（2.75m×0.1mm×0.1μm）He（纯度不低于99.999%）300°C20:11mL/min初始温度60°C，以3°C/min升至280°C300°C230°Cm/z45-200配置氢火焰离子化分别称量各酚类化合物（5.4）组分，称准至0.0001g。用甲醇溶解0.01mg/mL。配制的标准酚溶液中各酚类化合物的含量应于待测样品相近。标准混合物溶液B：准确称量适量内标物2,6-二氯），不同浓度标准混合溶液A溶解转移至具刻度容量瓶中，再用标准混合溶液A定容至刻度。计算内标物的浓度，精确至0.01mg/mL。2.5.3采用2mL注射器吸取1.5mL标准混合物溶液B，注入自动进样器2mL……（1）RRFi——i组分的相对响应值VCVi——i组分的峰体积；），计算内标物的含量，精确至0.01mg/mL。析，通过FID色谱图对定性出的不同酚类酚类化合物的相对响应因子按其同分异构体的平均相对响应……（2）CVCV……（3）C）；C）；VVW=……（4）W——焦油样品中鉴定出的不同酚类化合物的含量（mg/g）CV——初始称量煤焦油的质量（g）五、与有关的现行法律、法规和强制性国家标准的关系无六、重大分歧意见的处理经过和依据七、国家标准作为强制性国家标准或推荐性国家标准的建议八、贯彻国家标准的要求和措施建议（包括组织措施、技术措施、过渡办法等九、废止现行有关标准的建议十、其他应予说明的事项无2.简述8家实验室参与协同试验，根据本标准草案所描述的测量方法对测试结果进行3.样品的重复性编号物质1（%）2（%）3（%）4（%）5（%）6（%）1苯酚2.122.232.042.392.192.012邻甲酚3.173.353.313.213.043.293间甲酚+对甲酚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间异丙基苯酚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#样品的原始数据分析（第2家实验室）编号物质1（%）2（%）3（%）4（%）5（%）6（%）1苯酚2.352.412.522.312.442.392邻甲酚3.433.313.293.223.483.353间甲酚+对甲酚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间异丙基苯酚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#样品的原始数据分析（第3家实验室）编号物质1（%）2（%）3（%）4（%）5（%）6（%）1苯酚2.031.982.112.172.092.192邻甲酚3.092.982.872.912.813.013间甲酚+对甲酚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间异丙基苯酚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#样品的原始数据分析（第4家实验室）编号物质1（%）2（%）3（%）4（%）5（%）6（%）1苯酚2.252.162.182.092.302.192邻甲酚3.463.653.573.613.523.513间甲酚+对甲酚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间异丙基苯酚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#样品的原始数据分析（第5家实验室）编号物质1（%）2（%）3（%）4（%）5（%）6（%）1苯酚2.392.302.312.292.422.442邻甲酚3.313.393.443.293.493.303间甲酚+对甲酚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间异丙基苯酚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#样品的原始数据分析（第6家实验室）编号物质1（%）2（%）3（%）4（%）5（%）6（%）1苯酚2.232.312.342.302.322.332邻甲酚3.393.313.403.213.373.313间甲酚+对甲酚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间异丙基苯酚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#样品的原始数据分析（第7家实验室）编号物质1（%）2（%）3（%）4（%）5（%）6（%）1苯酚2.342.372.432.282.212.192邻甲酚3.313.393.423.193.293.333间甲酚+对甲酚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间异丙基苯酚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编号物质重复性限标准差重复性限r再现性限标准差再现性限R1苯酚0.01330.03740.01450.04062邻甲酚0.01550.04330.01670.04673间甲酚+对甲酚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间异丙基苯酚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#样品的原始数据分析（第1家实验室）编号物质1(%)2(%)3(%)4(%)5(%)6(%)13.313.273.413.353.163.5322.172.132.312.142.062.33间甲酚+对甲酚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#样品的原始数据分析（第2家实验室）编号物质1(%)2(%)3(%)4(%)5(%)6(%)13.293.213.333.253.143.1122.152.072.192.172.012.313间甲酚+对甲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#样品的原始数据分析（第3家实验室）编号物质1(%)2(%)3(%)4(%)5(%)6(%)13.293.423.353.163.093.2122.192.162.312.172.092.193间甲酚+对甲酚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#样品的原始数据分析（第4家实验室）编号物质1(%)2(%)3(%)4(%)5(%)6(%)13.313.163.093.113.313.4522.152.122.152.162.152.013间甲酚+对甲酚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#样品的原始数据分析（第5家实验室）编号物质1(%)2(%)3(%)4(%)5(%)6(%)13.383.513.463.283.263.4522.152.012.382.242.182.163间甲酚+对甲酚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#样品的原始数据分析（第6家实验室）编号物质1(%)2(%)3(%)4(%)5(%)6(%)13.513.433.363.523.383.4122.192.162.092.062.192.313间甲酚+对甲酚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#样品的原始数据分析（第7家实验室）编号物质1(%)2(%)3(%)4(%)5(%)6(%)123.372.213.422.283.292.173.352.343.512.323.292.213间甲酚+对甲酚4.1