title: Application of low-temperature CP-Sil 88 column for the isomeric analysis of toxic 2,378-substituted PCDD/Fs in incinerator flyash and sewage sludge using a triple quadrupole GC-MS/MS.
abstract: The seventeen 2378-substituted polychlorinated dibenzo-p-dioxins and dibenzo-p-furans (PCDD/Fs) congeners have been separated and analyzed in sewage sludge and incinerator flyash samples using a CP-Sil 88 column (50 m × 0.25 mm I.D., 0.25 μm film thickness) operating at a maximum oven temperature of 240°C. The column was used on a Varian 450-GC with a Varian 320-MS Triple Quadrupole. Calibration standards were used to determine the transition chemistries of the 2378-substituted PCDD/F congeners in the gas chromatography/mass spectrometry (GC-MS/MS) system. The five-point calibration curve for each of the congeners showed very good linearity with R(2) values greater than 0.999. The recovery of labelled compounds ranged from 50% to 120%. Analytical results from a reference flyash (BCR-490) and a reference sewage sludge (BCR-677) compared very well with the certified values, giving percentage deviations in I-TEQ (international toxic equivalents) of 4.93% and 0.53%, respectively. Results from 'real' flyash samples underscored the level of progress made in the abatement of dioxin emissions from incinerators; the old incinerator flyash contained much higher PCDD/F concentrations than the modern one. In addition, the concentrations profiles of PCDD/Fs in the 'real' sewage sludge from two UK wastewater treatment plants (WWTPs) showed that one contained a total PCDD/Fs content of 314 ng I-TEQ kg(-1), while the other gave a total of 53 ng I-TEQ kg(-1). Over an 18-month period of operation, no significant loss of analytical performance was observed from the low-temperature column.
authors.affiliation: Energy and Resources Research Institute, University of Leeds, LS2 9JT, UK. j.a.onwudili@leeds.ac.uk
authors.forename: Jude A
authors.initials: JA
authors.lastname: Onwudili
authors.forename: Yaghoub
authors.initials: Y
authors.lastname: Hajizadeh
authors.forename: Safari
authors.initials: S
authors.lastname: Zainal
authors.forename: John
authors.initials: J
authors.lastname: Upton
authors.forename: Paul T
authors.initials: PT
authors.lastname: Williams
mesh_terms: D001572:Benzofurans / Q000302:isolation & purification*; D060729:Coal Ash / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000295:instrumentation* / Q000379:methods; D057230:Limit of Detection; D000072317:Polychlorinated Dibenzodioxins / Q000031:analogs & derivatives* / Q000302:isolation & purification; D012722:Sewage / Q000032:analysis*; D013696:Temperature
chemical_list: D001572:Benzofurans; D060729:Coal Ash; D000072317:Polychlorinated Dibenzodioxins; D012722:Sewage