Abstract: Determination of perfluoroisobutylene (PFIB) in fluorine chemicals production is reviewed. The difficulties of determination of PFIB are analyzed. Also，the preparation of PFIB standard，chromatography column (packed column and capillary column)，detector are reviewed. PFIB gas chromatography operational condition is given for reference. Finally，requirement for determination of PFIB at different concentrations and the probable trend of PFIB determination are presented.