Method for Multiresidue Determination of Halogenated Aromatics and PAHs in Combustion-Related Samples

Abstract

Flue gas and fly ash samples have a complex composition. Thus, thorough extraction and selective cleanup prior to analysis are essential. This paper presents an evaluated method for determining halogenated dibenzo-p-dioxins (PXDD), halogenated dibenzofurans (PXDF), chlorinated biphenyls (PCB), chlorobenzenes (CBz), -phenols (CPh), dibenzo-p-dioxins (DD), dibenzofurans (DF), and polycyclic aromatic hydrocarbons (PAH) in a single sample. Since these combustion byproducts are ubiquitous, harmful environmental contaminants it is very important to obtain reliable assessments of them: especially specific PCDD/F and PCB congeners with Ah-receptor mediated toxicity. The reported method for this purpose includes techniques such as solid-phase extraction, Soxhlet-Dean-Stark extraction, cleanup using open liquid chromatographic columns, and finally GC/MS analysis/determination with quantification by the isotope dilution technique. The validation results presented here show good reproducibility for PXDD/F and PCB and are satisfactory for CPh, CBz, and PAH. An extraction efficiency test revealed that a nonpolar solvent did not completely extract a few analytes, i.e., diCPh and fluorene, which appear to require a more polar extraction agent. To pinpoint and minimize the loss of analytes, specific studies on reductions of their amounts during sample concentration were performed, showing that traditional rotary evaporation and nitrogen blow-down produce equally good results as a novel technique.

Effects of Transient Combustion Conditions on the Formation of Polychlorinated Dibenzo-p-Dioxins, Dibenzofurans, and Benzenes, and Polycyclic Aromatic Hydrocarbons During Municipal Solid Waste Incineration

“…The sample clean-up was performed according to methods described elsewhere (Liljelind et al, 2003) with some modifications; the analytes were applied to an AX21 carbon:celite 545 column (1:11.7 w:w) and eluted with toluene to collect PC 1-8 DD/Fs; and two additional internal standards, 13 C-1,2,3,7,8,9-HxCDF and 13 C-1,2,3,4,7,8,9-HpCDF, were included. Three types of blanks were analyzed: field-, laboratory-, and clean-up blanks.…”

An Ionic‐Liquid Based Probe for the Sequential Preconcentration from Headspace and Direct Voltammetric Detection of Phenols in Wastewaters

“…The methods so far recommended for the determination of these pollutants are intended for the determination of either individual phenolic compounds (GC and GC-MS [13,14]) or total volatile phenols, all being rather time consuming since they require a preliminary distillation or solvent extraction of the analytes from the original sample. In particular, the standard method recommended for the determination of total volatile phenols is the 4-aminoantipyrine colorimetric approach [15], even though it does not allow minority phenols such as those p-substituted with alkyl, aryl, nitro, nitroso, benzoyl or aldehyde groups to be determined.…”

Behavior of PCDF, PCDD, PCN and PCB during low temperature thermal treatment of MSW incineration fly ash

“…In all other aspects, the kiln gas and ash samples were cleaned-up and extracted following published procedures [Lundin and Marklund [11], Liljelind et al [18]]. Extracted POPs (PCDFs and PCDDs in the screening study; PCDFs, PCDDs, PCNs and PCBs in the main study) were analyzed by GC-HRMS using an AutoSpec Ultima NT 2000D instrument (Waters Corporation, Milford, MA), equipped with a DB 5-ms column (Supelco, 60 m, 0.25 mm i.d., 0.25 lm film thickness), operating in single ion monitoring, electron impact ionization mode.…”