The present study optimized the planetary ball milling of synthetic pyrrhotite doped with trace metals in order to enhance homogeneity. It has been demonstrated that milling at 400 rpm with acetone is an effective method of reducing particle size, whilst also preventing oxidation and secondary phase formation, in contrast to the process of dry grinding. Annealed samples demonstrated excellent trace element uniformity (RSD ~2-3%) by LA-ICP-MS, comparable to or superior to existing standards. The work underlines the pivotal role of milling conditions in the production of reliable sulfide standards, which are essential for accurate analysis in geochemistry and materials science.