采用大体积固相萃取-气相色谱法测定海水中10种多氯联苯的含量.海水样品采用大体积样品采样器与聚苯乙烯/二乙烯基苯固相萃取柱进行萃取.萃取流量为5.0 mL·min-1,丙酮作为洗脱剂.用Agilent HP-5石英毛细管色谱柱(30 m×0.32 mm,0.25 μm)分离,微池电子捕获检测器检测.10种多氯联苯的质量浓度均在10.0 μg·L-1以内与其峰面积呈线性关系,方法的检出限(3S/N)在0.002 3~0.012 μg·L-1之间.测定值的相对标准偏差(n=7)在0.9%~1.3%之间,在0.5,1.5,4.0 μg·L-1等3个浓度水平进行加标回收试验,回收率在80.7%~127%之间.

GC was applied to the determination of 10 polychlorinated biphenyls in seawater with large volume solid phase extraction.The seawater sample was extracted by large volume sampler and cleanert PS solid phase extraction column.Extracting flow rate found was 5.0 mL·min-1,and acetone was used as eluent.The analytes were separated on Agilent HP-5 quartz capillary chromatographic column (30 m×0.32 mm,0.25 μm) and detected by μECD.Linear relationships between values of peak area and mass concentration of 10 polychlorinated biphenyls were kept in the same range within 10.0 μg·L-1,with detection limits (3S/N) in the range of 0.002 3-0.012 μg·L-1.Values of RSD′s (n=7) found were in the range of 0.9%-1.3%.Tests for recovery were made by standard addition method at the concentration levels of 0.5,1.5,4.0 μg·L-1,giving values of recovery in the range of 80.7%-127%.