There are two main sample preparation techniques for measurement of powders with XRF—pressed and loose powder methods—neither requiring any chemical processes. In either case the proper sample preparation and accessories need to be selected to prevent breakage of the pressed powder during measurement. When a thin film for analysis surface (hereafter “sample film”) or a binder is used, it is recommended to select the proper sample preparation method to minimize analysis errors of target elements. This note describes key points and considerations for sample preparation by pressed and loose powder methods. In addition, sample preparation technique for the analysis of small quantities of powder sample is introduced.