Abstract：A method for the determination of Si,Mn,P,S,Cr,Ni,Cu,Mo,V,Ti,Nb,Co was established by X-ray fluorescence spectrometry (XRF) with milling machine preparation. The optimal parameters for sample surface preparation by milling machine were determined through analysis of sample surface treatment by miling machine and grinding machine. After the basic analytical conditions of X-ray fluorescence spectrometer were optimized, the regression curves of twenty-one elements in stainless steel sample such as C,Si,Mn,P,S,Cr,Ni,Cu,Al,Mo,V,Ti,Nb,Co,W,Ca,As,Sn,Pb,Sb and Fe were established. After the interference correction for P,S,Cr,Ni,Cu and Co was done, relatively satisfactory results were obtained. The precision of the determination of Cr and Ni in stainless steel by the proposed method and spark source atomic emission spectrometry were compared. It was found that the precision of the proposed method was higher. After precision was validated, the relative standard deviation (RSD,n=11) of Si,Mn,P,S,Cr,Ni,Cu,Mo,V and Co were between 0.08%-3.8%. The stainless steel standard sample was analyzed. The analytical results of the proposed method were consistent with those by wet method or spark source atomic emission spectrometry
