PCDDs/PCDfs의 전 동질체 210종 에 대한 분리분석방법 연구

Abstract

An analytical method for 210 congeners of polychlorinated dibenzo-p-dioxins/polychlorinated dibenzofurans (PCDDs/PCDFs) was investigated. The Korean Standard Test Method (KSTM) was used for sampling and analysis of PCDDs/PCDFs. The various column cleaning methods were tested to review the cleaning efficiency. The multi-layer silica gel column with 150 mL of normal (n)-hexane showed higher cleaning efficiency than the single-layer silica gel column with 150 mL of n-hexane to remove the chemical impurities excluding substances like as PCDDs/PCDFs and PCBs. The alumina column cleaned with 100 mL n-hexane as first eluant and 150 mL n-hexane with 50% dichloromethane (DCM) as second eluant was more efficient than that cleaned with 100 mL n-hexane with 2% DCM as first eluant and 150 mL n-hexane with 50% DCM as second eluant, to remove PCBs and to obtain all congeners of PCDDs/PCDFs. The internal standards to analyze MoCDDs/Fs-TrCDDs/Fs were used for each congener, and the calibration standards were prepared with native and internal standards. The high resolution gas chromatograph/high resolution mass spectrometer (HRGC/HRMS) was used. The analytical conditions for MoCDDs/MoCDFs-TrCDDs/TrCDFs and TeCDDs/ TeCDFs-OCDD/OCDF were distinguished due to distinctive properties of each homology. The recoveries were in the range of 45 to 64% in MoCDDs/MoCDFs through TrCDDs/TrCDFs and 73 to 105% in TeCDDs/TeCDDFs through OCDD/OCDF. A total of 166 peaks of PCDDs/PCDFs congeners were distinguished, of which 44 peaks overlapped with the methods to be studied.