HJ 1474-2026 土壤和沉积物 35种有机磷农药的测定 气相色谱法

中华人民共和国国家生态环境标准HJ1474—2026土壤和沉积物35种有机磷农药的测定气相色谱法Soilandsediment—Determinationof35organophosphoruspesticides—Gaschromatography本电子版为正式标准文件，由生态环境部环境标准研究所审校排版2026-05-15发布2026-08-15实施生态环境部发布I 12规范性引用文件 1 1 1 1 2 3 4 6 6 7 9 汇集：国家、地方、行业和团体、企业标准

qq：286195677人人网文库：/u-680150.html人人网文库：/u-680150.html人人网文库：/u-15216338.html境污染，改善生态环境质量，规范土壤和沉积物中35种有机磷农药的测定方法，制定本标准。本标准规定了测定土壤和沉积物中35种有机磷农药的气相色谱法。本标准自2026年8月15日起实施。1本标准规定了测定土壤和沉积物中35种有机磷农药的气相色谱法。本标准适用于土壤和沉积物中35种有机磷农药的测定。HJ/T91地表水和污水监测HJ442.4近岸海域环境监测技术规范第四部分近岸海域沉积物监测HJ613土壤干物质和水HJ783土壤和沉积物有机物的提取加压流高分离度进行消除，也可采用更换不同性能色谱柱或气相25.1丙酮（CH3COCH3色谱纯。5.2正己烷（C6H14色谱纯。5.3二氯甲烷（CH2Cl2色谱纯。5.6无水硫酸钠（Na2SO4优级纯。450℃下灼烧4h，置于干燥器中冷却至室温，转移至磨口玻璃瓶中密封保存。五氯酚(ρ=1.4mg/mL）、芘(ρ=在450℃下灼烧4h，置于干燥器中冷却至室温，转移至磨口玻璃瓶中密封保存。在450℃下灼烧4h，置于干燥器中冷却至室温，转移至磨口玻璃瓶中密封保存。5.16空气：助燃气，经净化管除水、6.1采样设备：不锈钢采样铲、采土（泥）器或6.2样品瓶：500mL，广口棕色玻6.7提取装置：索氏提取器、加压流体萃取装置或6.8浓缩装置：旋转蒸发仪、氮吹浓缩仪或其他3研磨过样品筛（6.11分取后密封保存于棕色玻注：当需测定的目标化合物包含敌敌畏或甲胺磷时，宜），设定净化程序。将溶剂转化后的提取液装载于凝胶渗透色谱仪（6.9）上，按照设定的净化程序运行。4如提取液（7.4.1）颜色较浅或基质干扰较小时，可选择固相萃取柱用石英砂（5.12）代替样品，按照与试样的制备（7.4）相同的步骤制以10℃/min升温至280℃,保持8min。配制能够覆盖样品浓度范围至少5个浓度点的标准系列溶液。按照仪器参考条件（8.1）由低浓度到高浓度依次对标准系列溶液分析，记录目标化合物的保留时注：速灭磷浓度为（E）-速灭磷和（Z）-速灭磷之和；内吸磷浓度为内吸磷-O513——除线磷；14——久效磷；15——乐果；16——皮蝇磷；17——甲基立枯磷；18——毒死蜱；19——甲基对20——倍硫磷；21——马拉硫磷；22——溴硫磷；23——杀螟硫磷；24——对硫磷；25——育畜磷；26——水胺1——敌敌畏；2——甲胺磷；3——（E）-速灭磷；3’——（Z）-速除线磷；14——久效磷；15——乐果；16——皮蝇磷；17——甲基立枯磷；18——毒死蜱；19——甲基对倍硫磷；21——马拉硫磷；22——溴硫磷；23——杀螟硫磷；24——对硫磷；25——育畜磷；26——水胺稻丰散；28——甲拌磷砜；29——丙硫磷；30——脱叶磷；31——杀虫畏；32——丙溴磷；33——地图235种有机磷农药标准溶液参考气相色谱图（6ri——由标准曲线测得的试样中目标化合物i的质量浓度，μg/mL；V——试样的定容体积，mL；m1——土壤样品的称取量，g；wdm——土壤样品的干物质含量，%。m2——沉积物样品的称取量，g；间相对标准偏差分别为4.5%～11%、6.0%～14%和3.5%～12%；重复性限分别为0.04mg/kg~70.06mg/kg、0.11mg/kg～0.14mg/kg和0.54mg/kg～0.77mg/kg；再现性限分别为0.05mg/kg~0.10mg/kg、0.20mg/kg～0.42mg/kg和0.77mg/kg～1.76mg/kg。0.07mg/kg～0.16mg/kg和0.37mg/kg～0.76mg/kg；再现性限分别为0.05mg/kg～0.11mg/kg、0.17mg/kg～0.41mg/kg和0.57mg/kg～1.82mg间相对标准偏差分别为6.9%～17%、6.8%～22%和5.3%～18%；重复性限分别为0.04mg/kg~0.09mg/kg、0.06mg/kg～0.26mg/kg和0.56mg/kg～1.44mg/kg；再现性限分别为0.06mg/kg~0.13mg/kg、0.21mg/kg收率最终值分别为91.0%±8.7%～107%±23.8%、93.7%±13.6%～103%±20.1%和86.2%±14.4%~率最终值分别为57.9%±26.4%～104%±28.8%、48.5%±18.0%～97.8%±17.1%和49.5%±13.0%~最终值分别为67.4%±15.2%～98.2%±13.6%、55.4%±24.0%～103%±15.4%和66.5%±24.2%~浓度值相对误差应在±30%以内。否则，应重新建立8加标回收率应在30%～140%之间，加标平行样的测定结9当样品取样量为10.0g，定容体积为5.0mL时，35种有机磷农药的方法检出限和测定下限见表10.042Methamidophos0.043速灭磷（E+Z）Mevinphos0.044Demeton0.035297-97-20.046Ethoprophos0.037Phorate298-02-20.0380.039Diazinon0.030.03298-04-40.0326087-47-80.04Dichlofention0.040.050.20Dimethoate0.04Fenchlorphos299-84-30.040.042921-88-20.04Parathion-Methyl298-00-00.04Fenthion0.04Malathion0.042104-96-30.04Fenitrothion0.04Parathion0.04299-86-50.0424353-61-50.04Phenthoate2597-03-70.042588-04-70.040.040.0422248-79-90.040.040.03Carbophenothion0.0424017-47-80.04方法的准确度类型0.040.050.940.224.310.770.250.030.050.730.070.294.1～100.580.254.3～160.050.090.772.4～100.412.6～1540.060.990.254.760.570.250.020.490.090.262.470.760.250.040.070.550.370.743速灭磷40.060.960.254.660.6030.740.300.440.060.912.7～130.344.240.080.990.264.800.530.080.890.264.90.370.620.250.040.090.720.070.310.56类型40.070.214.900.640.080.940.264.350.520.9～100.040.952.0～110.334.420.9540.090.990.204.950.630.090.940.234.460.5～100.040.090.940.294.624.5～8.80.9340.070.990.204.960.630.920.274.80.470.7040.090.830.284.070.8740.080.204.930.630.090.950.224.424.60.450.7～110.040.090.960.304.504.2～9.00.9240.060.270.630.090.960.234.520.4～100.040.090.960.304.500.89类型40.070.224.960.630.090.960.234.480.510.7～100.040.090.950.324.624.0～8.80.940.080.990.230.630.080.910.244.00.390.570.252.8～100.040.090.780.060.270.640.070.424.820.560.250.260.030.940.244.670.540.070.940.344.260.840.060.240.620.930.090.960.244.500.480.940.960.324.520.250.270.060.304.810.650.090.700.410.790.810.260.504.350.97类型50.070.260.530.920.224.420.460.840.090.950.304.540.070.990.240.630.930.090.930.264.360.490.7～100.040.080.960.334.440.070.244.990.630.090.980.304.440.440.970.354.520.950.060.270.640.730.090.950.254.460.460.8～100.040.960.304.440.060.990.234.790.640.960.354.490.4～100.050.980.354.450.95类型～110.050.070.280.530.090.950.274.430.440.9～100.040.950.294.440.850.080.990.274.970.630.080.944.504.40.490.7～110.040.090.960.264.512.2～100.940.060.980.234.974.70.600.830.080.930.294.330.480.8～110.040.080.950.324.340.940.070.990.284.880.540.950.264.450.440.9～110.050.080.950.304.480.940.060.314.880.530.090.970.364.530.440.990.344.540.90类型50.070.260.530.860.250.410.80～100.040.090.970.274.400.7～100.050.080.300.730.070.900.284.250.430.8～100.040.070.980.224.450.250.260.040.050.224.910.620.930.090.970.244.520.480.8～110.050.980.274.612.8～40.060.270.630.080.970.244.670.50～110.040.090.314.672.9～40.060.270.730.090.970.244.580.470.940.960.304.50类型50.070.260.630.090.970.264.700.5040.970.214.650.060.990.290.720.250.260.030.080.920.284.450.470.8～100.040.080.970.294.322.8～120.950.070.990.390.730.900.264.340.4～130.050.080.952.5～120.284.452.8～110.90.060.060.390.640.860.274.470.450.080.910.210.394.374.1～202.0～110.