科研之友
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摘要
An efficient and reliable separation technique based on automated Soxhlet hot extraction (AHSE) was developed and validated. It can be applied to rapid separations of 20 persistent organic pollutants, including two types of brominated flame retardants (BFRs), polybrominated biphenyls (PBBs) and polybrominated diphenyl ethers (PBDEs) contained in nonmetallic component parts of electronic products. The qualitative chromatographic analyses were carried out by using a gas chromatography coupled with a mass spectrometry detector (GC-MS). The 20 persistent organic pollutants were simultaneously and completely separated by a 15 meter HP-5MS short capillary column in 25 minutes. Through the tests of extraction performance, effects of solvent and extraction time on selected BFRs were investigated; toluene and 120 min extraction time were chose as the optimum conditions. Besides, this article examines the influence of temperature on the chromatographic analysis, the optimum temperature parameters were 280 degrees C and 320 degrees C for injector and column, respectively. The ASHE-GCMS method was validated for the analysis of the certified reference material of CRM8110-a and IRMM310. The limits of detection (LOD) for polymer sample was 0.55-4.50 mu g mL(-1); linearity range from 0.11 to 16 mu g mL(-1). The proposed methodology can fully meet the requirement of relational directives.
