《水质 挥发性消毒副产物的测定 气相色谱法（征求意见稿）》编制说明

1《水质挥发性消毒副产物的测定气相色编制说明2近年来备受关注。此外，随着重大公共卫生事件（如SARS、禽流感、新冠病毒3乙酸、二氯乙酸、三氯乙酸、一溴乙酸、二溴乙酸、氯化氰、2,4,6-三氯酚、亚测协字〔2022〕16号广东省分析测试协会下达了编制“水质挥发性消毒副2、主要工作过程2.1标准初稿的起草4负责起草单位将完成的标准初稿和标准计划项目任务书提交至广东省分析测试2.2标准计划立项2.3征求意见稿的起草（1）2022年11月～12月，建立标准编制小组，并制定本标准研制的技术52.4标准的征求意见见为XX条。征集意见采纳XX条，不采纳XX条，部分采纳XX条。根据回函三、本标准与国内外标准关系的说明了一些消毒副产物分析方法标准，如美国环保局发布的分析方法标准EPA6（1）建立的标准分析方法能够满足各项方法特性指标的要求。（3）建立的标准分析方法的准确度、精密度方法准确可靠，满足各项方（4）建立的标准分析方法符合监测行业人员的技术水平，能被国内主要（5）建立的标准分析方法具有普遍适用2、确定标准主要内容的依据要求的基础上，同时参考GB/T20001.4-2015《标准编写规则第4部分：试验7（4）无水硫酸钠：使用时为避免试剂中有机污染物对试验的干扰，8（1）带电子捕获检测器（ECD）气相色谱仪。（3）采样瓶：棕色磨口具塞玻璃瓶或具有聚四氟乙烯衬垫瓶盖的棕色螺口水样中挥发性消毒副产物经过滤以及甲基叔丁基醚萃取后，用气相色谱分水样（6.1）经0.45μm的滤膜（4.11）过滤，弃去至少1mL初滤液后，移取91.广东省科学院测试分析研究所（中国广州分析测试中无12345分流比10:16789101110:112101010201030104010501061,1-二氯丙酮010701080109010101,1,1-三氯丙酮01011010120101301014123.7133.81455.1061,1-二氯丙酮DCP77.1589101,1,1-三氯丙酮TCP11.12111217.141318.1411表1-5检出限及测定下限(µg/L）123453.16061,1-二氯丙酮DCP789101,1,1-三氯丙酮TCP11120.31613定结果的相对标准偏差为1.01%～6.43%，12表1-6方法精密度和正确度（空白水）序号加标浓度测定结果(µg/L）平均值RSD（%）回收率（%）12345671三氯甲烷54.775.014.734.854.872.1497.43109.339.163.132018.7317.8918.4518.6718.9118.6519.0118.621.982三氯乙腈54.724.774.734.824.811.47108.277.957.287.727.307.897.815.2578.132018.1318.4418.1818.5118.3417.9718.2918.271.0291.333一氯乙腈55.125.335.184.855.275.355.445.223.74109.7210.199.343.1996.312017.2917.9516.8318.7316.2717.7617.354一溴二氯55.135.225.285.355.165.455.325.272.13105.461010.1410.339.3510.214.6397.572018.3717.5516.9117.3416.2917.0217.173.915二氯乙腈55.375.445.485.345.475.355.245.381.59107.691010.7511.4610.415.55104.012018.3417.8818.3518.2517.5018.2918.1890.9161,1-二氯丙酮55.145.125.235.215.135.165.151.01103.061010.5710.3310.1511.0710.4310.9210.7810.613.132019.4920.2720.0119.6718.8018.8119.532.867三氯硝基54.724.674.744.584.234.574.5691.171010.019.188.729.135.4191.312016.3517.7817.0916.4916.8215.9415.983.9383.188二溴一氯55.355.305.285.035.275.155.29105.8313109.5510.039.383.3995.012017.3218.0516.2317.9816.1917.8917.244.6386.189一溴一氯55.435.485.175.145.385.055.243.45108.339.133.422020.1619.7920.2320.1719.8620.3220.211.83101.04101,1,1-三氯丙酮55.345.135.125.235.015.224.11109.738.7510.199.382015.3216.2916.1415.9316.3615.6315.5615.892.5079.4511三溴甲烷55.325.125.455.235.425.175.245.282.34105.571010.4510.739.4310.0310.2210.1510.114.24101.102017.8919.5518.1619.0219.2718.4919.3518.823.4112三氯乙酰氨55.165.264.875.135.235.445.173.39103.341010.4210.5210.9510.164.71101.562016.4619.4318.7818.9419.6117.5518.6393.1513三碘甲烷55.155.325.235.015.225.335.163.32103.20109.7510.159.5710.4310.032.8699.572017.4520.7920.8720.1820.5318.9820.3819.8899.41表1-7方法精密度和正确度（地表水）序号加标浓度测定结果(µg/L）平均值RSD回收率（%）12345671三氯甲烷108.338.779.129.1391.332三氯乙腈108.137.887.798.168.1481.443一氯乙腈108.529.189.739.339.759.37144一溴二氯1010.259.739.309.733.4597.335二氯乙腈1011.5410.3710.2410.0310.7461,1-二氯丙酮1010.0310.1810.3710.141.73100.777三氯硝基109.239.349.279.273.3192.718二溴一氯108.778.759.222.379一溴一氯108.579.019.278.733.6787.29101,1,1-三氯丙酮109.419.538.155.4911三溴甲烷109.7510.019.329.532.4712三氯乙酰氨109.259.339.359.759.522.3895.2413三碘甲烷109.759.522.971.4小结实验结果表明：该方法检出限和测定下限较低，重复性好、方法准确可靠，具有普遍适用性，满足水中13中挥发性消毒副产物检测的工作要求。无2.2仪器参考条件1234567892.3.1标准曲线的绘制过程及主要结果表2-3标准曲线系列浓度102030405060701680109010101,1,1-三氯丙酮010110101201013010表2-4标准曲线及相关系数1234561,1-二氯丙酮DCP789101,1,1-三氯丙酮TCP1112132.3.2方法检出限和测定下限表2-5检出限及测定下限(µg/L）120.312340.1130.45151761,1-二氯丙酮DCP780.3169101,1,1-三氯丙酮TCP110.13412132.3.3方法精密度及正确度18表2-6方法精密度和正确度（空白水）序号加标浓度测定结果(µg/L）平均值RSD（%）回收率（%）12345671三氯甲烷54.954.715.174.934.914.912.9298.18109.017.867.828.318.165.652016.1717.6016.8016.403.152三氯乙腈54.474.424.474.434.914.624.615.0392.22107.277.957.287.727.307.8976.412018.4018.3417.8018.2018.1017.9019.2018.282.5391.393一氯乙腈55.335.305.194.955.675.755.375.375.14107.331010.5210.599.359.775.7597.732017.2917.9516.8318.7316.2717.7617.3586.774一溴二氯55.235.205.245.255.765.815.425.424.83108.331010.739.419.159.817.472015.4717.2515.9016.3415.1916.0216.124.365二氯乙腈55.575.545.585.405.575.455.525.521.25110.351011.7511.8010.9710.9511.4111.174.42111.752016.3417.3517.2515.5017.2916.9161,1-二氯丙酮55.245.225.325.385.195.235.265.261.24105.261011.7510.7511.5711.0711.3411.2911.8711.383.43113.782018.4919.7219.1019.7617.8019.8119.347三氯硝基54.614.564.634.474.124.393.95109.128.319.128.514.122015.5316.8717.3817.7116.7883.928二溴一氯55.465.415.775.395.145.565.455.463.47109.12191010.3910.419.539.912016.2317.9917.0516.3215.7916.234.259一溴一氯55.555.975.705.345.785.783.95115.69108.239.232021.7621.9221.3021.7121.2321.094.18105.47101,1,1-三氯丙酮55.375.465.405.305.205.145.315.31106.221010.309.735.9397.322014.2315.8915.4115.1915.6314.6315.6515.233.9676.1711三溴甲烷55.235.215.255.435.505.375.345.331011.4511.3710.3311.0311.055.20108.582017.9018.7118.0218.7217.3918.5318.423.9792.1012三氯乙酰氨55.185.274.915.335.535.315.31106.261011.2411.2511.5910.9210.0110.544.852015.6420.3319.9719.4920.6118.5519.2813三碘甲烷55.455.425.434.765.315.425.305.30105.991010.7510.7511.3411.1310.9710.76107.552018.4521.7921.8721.8121.5021.8321.30106.52表2-7方法精密度和正确度（地表水）序号加标浓度测定结果(µg/L）平均值RSD（%）回收率（%）12345671三氯甲烷109.368.239.729.125.442三氯乙腈108.127.787.637.777.617.893.4278.91203一氯乙腈109.529.1310.249.7210.655.3897.414一溴二氯1010.829.5210.329.339.3610.015.8198.315二氯乙腈1011.4410.5411.7710.4210.2310.3310.875.5061,1-二氯丙酮1010.1310.2810.7310.2810.343.55103.367三氯硝基108.328.275.5788.278二溴一氯108.379.559.179.329.145.5191.409一溴一氯108.119.118.148.919.3887.87101,1,1-三氯丙酮1010.1410.359.519.389.437.3111三溴甲烷1010.719.2710.3210.5810.23102.2912三氯乙酰氨1010.339.259.574.2897.7613三碘甲烷1010.1411.410.3911.5710.5210.655.952.4小结实验结果表明：该方法检出限和测定下限较低，重复性好、方法准确可靠，具有普遍适用性，满足水中13中挥发性消毒副产物检测的工作要求。213.广东粤海水务检测技术有限公司3.1基本信息无3.2仪器参考条件12345分流比10:16789101110:1123.3验证结果3.3.1标准曲线的绘制过程及主要结果表3-3标准曲线系列浓度1010201030104010501061,1-二氯丙酮01070102280109010101,1,1-三氯丙酮010110101201013010141234561,1-二氯丙酮DCP789101,1,1-三氯丙酮TCP1112133.3.2方法检出限和测定下限表3-5检出限及测定下限(µg/L）123450.3162361,1-二氯丙酮DCP789101,1,1-三氯丙酮TCP11120.316133.3.3方法精密度及正确度24表3-6方法精密度和正确度（空白水）序号加标浓度测定结果(µg/L）平均值RSD（%）回收率（%）12345671三氯甲烷55.014.834.932.0398.51109.218.739.163.4787.972017.1717.6316.7816.3416.5816.3916.1816.7283.622三氯乙腈54.774.324.534.734.815.014.824.714.75108.277.587.367.177.7877.832019.418.9117.7718.5818.3918.9219.2318.7493.713一氯乙腈55.164.975.225.055.395.435.175.203.21103.97109.329.2510.169.719.1595.442018.3917.7317.7417.6317.6317.2517.6617.721.914一溴二氯55.035.215.332.58101.74109.3610.4198.512016.7717.3517.6616.4816.8716.1917.0216.912.9584.535二氯乙腈55.445.145.315.155.245.265.232.281010.5710.7110.1110.253.17102.502018.3418.1817.7717.2817.4418.0318.2417.902.3061,1-二氯丙酮54.784.815.15.035.142.761010.159.5510.12.862018.5919.1618.7917.853.567三氯硝基54.724.574.534.214.754.5691.14109.219.138.759.163.3291.592015.3516.7817.0417.1616.1716.4916.5616.513.7082.548二溴一氯55.145.334.934.765.155.053.59101.00251010.118.739.1410.5310.2810.1998.172016.2316.3915.7517.2316.7416.7915.9816.443.1182.229一溴一氯55.055.145.275.175.325.264.785.143.57102.83109.619.728.329.339.156.1691.542020.3620.5620.2921.4321.1721.552.44101,1,1-三氯丙酮54.734.675.034.525.134.82109.349.225.292014.4414.9815.3915.4415.3715.3714.5615.082.8275.3911三溴甲烷55.235.215.255.435.505.375.345.331010.319.4310.2310.7910.1510.124.11101.202016.7918.5717.2417.2817.2718.9317.3517.6388.1612三氯乙酰氨55.175.194.735.635.11101.571011.2511.1210.8510.9511.0110.3410.784.38107.792018.4620.1320.9719.1620.6521.420.245.29101.2213三碘甲烷55.565.835.175.675.015.245.135.37107.461010.5710.549.5710.4311.3310.7711.1910.635.43106.292019.5420.9721.7721.2121.1521.9720.3821.003.94表3-7方法精密度和正确度（地表水）序号加标浓度测定结果(µg/L）平均值RSD回收率（%）12345671三氯甲烷107.888.328.277.765.362三氯乙腈107.438.777.897.838.128.105.8581.04263一氯乙腈108.259.119.128.729.434.394一溴二氯109.219.259.2310.1310.014.375二氯乙腈1010.1210.329.139.556.1161,1-二氯丙酮1010.2110.7210.039.573.457三氯硝基108.729.138二溴一氯109.739.419.165.1691.579一溴一氯109.129.419.134.45101,1,1-三氯丙酮109.5310.1511三溴甲烷109.729.5710.1195.9112三氯乙酰氨109.259.759.535.0195.2713三碘甲烷109.3910.439.199.2510.523.4小结实验结果表明：该方法检出限和测定下限较低，重复性好、方法准确可靠，具有普遍适用性，满足水中13中挥发性消毒副产物检测的工作要求。27无4.2仪器参考条件12345分流比10:16789101110:1124.3.1标准曲线的绘制过程及主要结果表4-3标准曲线系列浓度1010201030104010501061,1-二氯丙酮010701080109010101,1,1-三氯丙酮01011010120101301014表4-4标准曲线及相关系数1234561,1-二氯丙酮DCP789101,1,1-三氯丙酮TCP1112134.3.2方法检出限和测定下限表4-5检出限及测定下限(µg/L）10.43120.10134561,1-二氯丙酮DCP0.1137890.112101,1,1-三氯丙酮TCP11120.117134.3.3方法精密度及正确度偏差为2.34%～7.91%。30表4-6方法精密度和正确度（空白水）序号加标浓度测定结果(µg/L）平均值RSD（%）回收率（%）12345671三氯甲烷55.195.355.215.565.575.245.271010.179.378.316.552017.2819.4318.4917.5018.1193.322三氯乙腈54.394.433.974.594.534.4188.11109.217.828.148.127.958.375.5483.032016.5517.3717.5017.9919.7316.5717.1517.5587.763一氯乙腈54.734.594.734.324.455.185.184.7494.831011.9111.1610.3110.587.13105.812014.6815.9115.4015.5816.9214.8315.0915.4977.434一溴二氯54.835.355.205.475.575.205.50103.931011.8511.7010.479.5510.5210.51105.152016.7518.3117.8218.1520.1516.7517.5117.925二氯乙腈55.565.635.755.725.785.791.53113.901011.1711.799.739.7110.1110.38103.782015.3016.7715.9615.6517.5614.6515.4315.906.1479.5261,1-二氯丙酮55.655.565.625.675.655.725.741.07113.171011.6911.9011.1110.6211.3911.214.22112.062017.5319.3718.5519.0121.2317.4718.7593.757三氯硝基54.294.383.764.234.121011.8311.009.3110.16101.612020.3020.3520.3017.4118.5219.5597.748二溴一氯55.414.784.344.294.7531109.15.3187.392016.2616.5616.1816.3418.2816.4615.7516.5582.749一溴一氯54.614.555.405.374.951011.3111.7911.3610.1010.2911.3011.9111.156.25111.522019.6721.1721.8119.3019.5520.344.76101.70101,1,1-三氯丙酮55.295.705.555.615.782.81112.021010.358.729.416.182014.1915.6615.3315.5817.9516.1116.8515.957.4779.7611三溴甲烷55.535.785.765.765.415.535.565.62112.401010.6111.4210.1210.1410.32103.152016.7618.5418.3318.4520.5517.3818.2991.4512三氯乙酰氨54.914.934.8397.561010.349.7210.549.112016.5318.5618.7320.3318.4618.0718.6293.1013三碘甲烷55.585.525.555.545.185.385.38107.601011.7211.9410.4210.2410.0310.62106.212019.2821.1320.1221.9521.8221.1720.91104.55表4-7方法精密度和正确度（地表水）序号加标浓度测定结果(µg/L）平均值RSD回收率（%）12345671三氯甲烷109.129.179.779.318.739.183.7992.792三氯乙腈108.218.329.377.503一氯