Selective determination of polychlorinated biphenyls in waste oils using liquid-liquid partition followed by headspace solid-phase microextraction and gas chromatography with atomic emission detection.
A procedure for the determination of the total content of polychlorinated biphenyls (PCBs) in industrial oil samples using gas chromatography coupled to atomic emission detection (GC-AED) is presented. Analytes were extracted from the samples using dimethylsulfoxide (DMSO), this extract was diluted with water, and PCBs were concentrated on a PDMS-DVB solid-phase microextraction (SPME) fibre using the headspace (HS) mode. Fibres were thermally desorbed for 3 min in the splitless injection port of the GC-AED system. Influence of liquid-liquid extraction conditions on the performance of the analytical procedure is presented and the need of a sample oxidation step, previous to the extraction of the PCBs with DMSO, discussed. Working under optimal conditions, quantification limits from 0.5 to 1 microg/g (total PCBs content) were obtained for several Aroclor mixtures in transformer oil samples. The repeatability of the whole sample preparation procedure (liquid-liquid partition followed by headspace SPME and GC-AED determination) ranged from 4 to 7%.
Ramil Criado
M
M
Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigacíon y Análisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain.
Rodríguez Pereiro
I
I
Cela Torrijos
R
R
D002849:Chromatography, Gas / Q000379:methods*; D009821:Oils / Q000032:analysis*; D011078:Polychlorinated Biphenyls / Q000032:analysis*; D012680:Sensitivity and Specificity
D009821:Oils; D011078:Polychlorinated Biphenyls