Determination of hexachlorobutadiene, pentachlorobenzene, and hexachlorobenzene in waste incineration fly ash using ultrasonic extraction followed by column cleanup and GC-MS analysis.

Hexachlorobutadiene (HCBD) was listed as a new controlling persistent organic pollutant in the Stockholm Convention because of its wide industrial applications and potential genotoxicity and carcinogenicity. However, only limited information exists on the release of HCBD from unintentional sources, such as waste incineration. Identification and quantification of HCBD in fly ash, one of the major outputs of waste incineration, is imperative. This work presents a simple method for determining HCBD in waste incineration fly ash based on ultrasonic extraction coupled with a silica gel-Florisil column cleanup followed by gas chromatography-mass spectrometry detection. Two typical persistent organic pollutants, pentachlorobenzene (PeCB) and hexachlorobenzene (HCB), were measured simultaneously. The parameters that influence the extraction efficiency and the quality of instrument detection were studied. Under the optimum experimental conditions, high sensitivity (detection limit 0.25-0.53 ng g-1), acceptable recoveries (64.0-71.4%) at spiking levels of 5-500 ng g-1, and good repeatability [relative standard deviation (n = 3) of 14% or less] were achieved for all target analytes. The validation of this method was performed by analysis of six real fly ash samples from different waste incinerators in eastern China. The concentrations of HCBD detected in these samples (1.39-97.6 ng g-1) were comparable to those of PeCB (1.22-150 ng g-1) and HCB (0.82-120 ng g-1), indicating that the residual HCBD as well as PeCB and HCB in waste incineration fly ash should not be ignored. The results confirm for the first time that waste incineration is an unintentional source of HCBD in China. Graphical abstract An analytical method for hexachlorobutadiene, pentachlorobenzene, and hexachlorobenzene in fly ash from waste incineration. GC-MS gas chromatography-mass spectrometry, Ph-d10 phenanthrene-d10.