土壤和沉积物中多氯联苯单体测定的净化方法研究

摘要

Methods such as concentrated sulfuric acid cleanup, copper powder desulfurization, Florisil cartridge , silica gel column and graphite carbon column were used to purificate extract solution for determination of PCBs in soil and sediment. The recoveries of different pretreatment methods were as follows: 92.4% - 109% by cleanup of concentrated sulfuric acid, 85.7% ~ 108% by purification of Florida soil column with hexane/acetone mixed solution (elution liquid 8 Ml ~ 10 Ml) , 81. 2% - 107% by purification of silica gel column with hexane (elution liquid 8 Ml ~ 10 Ml) , 93. 5% -112% purification of graphite carbon column with toluene (elution liquid 12 Ml). Test results of samples with optimized pretreatment methods obtained desirable precision and recovery.%对浓硫酸净化、铜粉脱硫、氟罗里硅土柱、硅胶柱、石墨碳柱等净化方法在土壤和沉积物多氮联苯单体测定中的应用进行了研究.浓硫酸对多氯联苯单体的净化回收率达92.4％～109％；氟罗里硅土柱用正己烷/丙酮混合溶液淋洗,净化洗脱液体积为8 mL～10 mL时,回收率达85.7％ ～ 108％；硅胶柱用正己烷淋洗,净化洗脱液体积为8 mL～10 mL时,回收率达81.2％～107％；石墨碳柱用甲苯淋洗,净化洗脱液体积为12 mL时,回收率达93.5％ ～ 112％.将优化后的净化方法应用于实际样品测定,精密度与加标回收率均良好.