In this paper, the chemical procedure of nickel sulphide fire assay has been improved to measure the PGEs contents for pyrite by ICP-MS. The fusion flux and molten slag was changed in order to yield the ideal button without losing any of the sampling weight. The improved method gives the button the optimum capability to extract PGEs from the fusant and avoid PGEs loss from prolonged heating and reaction. The results of different pyrite samples and standard material indicate that this method is an improvement on the previous methods by meeting the requirements for PGEs determination of most pyrite.