Studies On The Determination Of The Polybrominated Biphenyls And Polybrominated Diphenyl Ethers In Textiles

Polybrominated biphenyls(PBBs) and polybrominated diphenyl ethers(PBDEs) have been widely used as brominated flame retardants(BFRs) around the world.Unfortunately,PBDEs and PBBs are harmfull compounds and considered to be environmental contaminants,so many directives and standards have been carried out by European Union and other international organizations to forbid their use in textiles,electronic equipments and so on.However,the testing standard of PBDEs and PBBs in textiles has not developed yet.In this paper,eight kinds of PBDEs and PBBs have been chosen,and the pretreatment procedures and accurate gas chromatography analysis method have been developed for the determination in textiles.Ultrasonic extraction and microwave-assisted extraction have been studied for sample pretreatment in this paper.By selection of the best extractant,orthogonal and simple factor experiments,the pretreatment procedures have been designed.The experimental results indicate that hexane + acetone(2:3) was the best extractant for ultrasonic extraction method,and the best pretreatment procedure was that 1.0g textile sample was extracted by hexane + acetone(2:3) in ultrasonic for 10min for 3 times,and the amount of the extractant used were 30mL,20mL and 10mL.The method detection limits(MDL) were 0.000381～0.00930μg/g,the recoveries of spiked samples were 75.42%～119.31%,and the relative standard deviations(RSD) for 6 parallel determinations were 1.65%～11.67%.For the microwave-assisted extraction,the best pretreatment procedure was that 1.0g textile sample was extracted with hexane + dichloromethane(2:3),and the instrument parameters were set as follows:60℃,10min,400W.The MDL was 0.000124～0.000991μg/g,the recoveries of spiked samples were 75.50%～112.91%,and the RSD for 6 parallel determinations were 1.34%～11.79%.Based on the results,it was clear that both of the methods were suitable for the sample pretreatment,and the method of microwave-assisted extraction showed the lower MDL and saved more time and solvents. The method of using concentrated sulphuric acid to purify samples was preliminarily studied in this paper.The result indicated that no disruptor was led into the samples,and the recoveries of PBBs and PBDEs after extraction and cleanup were all above 75%.Therefore,concentrated sulphuric acid can be used to purify the textile samples in this method.The method by using GC-ECD to analyze PBBs and PBDEs has been studied.Gas flow process and temperature process were used together for the optimization of GC-ECD measurement of the compounds,and the effects of inlet temperature and makeup flow were also investigated.Finaly a method of simultaneous analysis of eight PBBs and PBDEs by GC-ECD was developed and it has shown good resolution,good correlation coefficient and low MDL.On the basis of the determination method established,10 kinds of textile samples have been tested,and the results showed that none of the eight analytes studied in this paper was detected.