title: Separation of non-ortho polychlorinated biphenyl congeners on pre-packed carbon tubes. Application to analysis in sewage sludge and soil samples.
abstract: The analysis of planar (non-ortho) polychlorinated biphenyls (PCB) by HRGC-ECD or HRGC-HRMS requires a fractionation step to avoid the interferences of the bulk of PCB, usually in much higher concentration than the planar ones. In this paper, a new method, based on the fractionation of PCB on SPE commercial tubes pre-packed with Carbopack B, has been developed. After the extract has been applied on the stationary phase, the bulk of PCD are eluted with 15 ml of hexane (fraction I), mono-ortho PCB with 20 ml of hexane/toluene 99:1 (fraction II) and planar PCB with 20 ml of toluene (fraction III) in a station under vacuum. The method has been validated: accuracy (expressed as recovery in %) is >70% and precision (expressed as % RSD) is <20% considering changes of day, analyst and batch of tubes. The method is linear in the range studied. Other advantages are that the method is simple, rapid and it can be easily automated. The application of this separation to the determination of planar PCB in fly-ash extracts from an intercalibration exercise and to sewage sludge, sediment and soil samples has been successful. In addition, this method removes hydrocarbons from the planar PCB fraction and allows its concentration to very small volumes.
authors.affiliation: Environmental Laboratory, Institut Químic de Sarrià (Ramon Llull University), Barcelona, Spain. medam@iqs.url.es
authors.forename: L
authors.initials: L
authors.lastname: Molina
authors.forename: M
authors.initials: M
authors.lastname: Cabes
authors.forename: J
authors.initials: J
authors.lastname: Díaz-Ferrero
authors.forename: M
authors.initials: M
authors.lastname: Coll
authors.forename: R
authors.initials: R
authors.lastname: Martí
authors.forename: F
authors.initials: F
authors.lastname: Broto-Puig
authors.forename: L
authors.initials: L
authors.lastname: Comellas
authors.forename: M C
authors.initials: MC
authors.lastname: Rodríguez-Larena
mesh_terms: D002244:Carbon; D005591:Chemical Fractionation / Q000379:methods; D008401:Gas Chromatography-Mass Spectrometry; D011078:Polychlorinated Biphenyls / Q000302:isolation & purification*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012722:Sewage / Q000032:analysis*; D012987:Soil / Q000032:analysis*
chemical_list: D012722:Sewage; D012987:Soil; D002244:Carbon; D011078:Polychlorinated Biphenyls