The Study Of Analysis Checkout Method Of Perfluorooctane Sulfonate In Textile And Chelating Agent

This paper describes methods for the extraction, derivatization and determination of small quantity and harmful perfluorooctane sulfonate in textile and chelating agent, especially textile samples which were finished by oil, water and soil repellent finishing agent, utilizing gas chromatography/mass spectrometry method.The concrete content includes the following aspects:1. Searching information, a series of solvent were compared in order to choose the best extraction solvent for the extract of PFOS in textile. And methanol aqueous solution was chosen according to the extracting effect on real sample;2. Searching information, some extraction methods were studied, including methods of Soxhlet、ultrasonic、boiling and ultrasonic-microwave synergistic extraction, and in the end the ultrasonic-microwave synergistic extraction was chosen as the best way of extracting method according to its highest extraction rate;3. Triethylorthoacetate (TEOA) as the derivatization agent, perfluorooctane sulfonate was conveniently converted to corresponding ethyl PFOS;4. Analysis was performed by gas-chromatography with mass spectrometric detection (GC/MS) and selected ion monitoring (SIM) mode. PFOS was positively confirmed by retention times and characteristic ion.Programmed-temperature was used in the method and analysis process needed 40.27 min. The limit of detection (LOD) is 0.0135μg/mL. The spiked recovery is 80%～100%, and the relative standard deviation (RSD) is less than 10%. In addition, repeatability and precision were also satisfied with RSD<1% and RSD<10% respectively according to the retention time and peak area on the detection of PFOS during 5 continuous days. So, after further investigation of correlation coefficient, relative standard deviation and limit of detection, and a promising method will be established, this is efficient for the trace determination of PFOS.