Platinum-palladium concentrate, obtained from copper anode slime through Kaldo furnace smelting,silver electrolysis, and aqua regia gold parting, is primarily used for palladium recovery. Accurate determination ofpalladium content in such concentrates is of great significance for the resource utilization of palladium. A lead fireassay enrichment-dimethylglyoxime gravimetric method was developed for palladium determination in platinum-palladium concentrates. In this method, palladium was pre⁃enriched by lead fire assay, and the precious metal bead wasdigested stepwise with nitric acid（1+4）and hydrochloric acid. Using hydrochloric acid as a precipitant, the solutionwas diluted with water and filtered hot to remove silver interference. In a 10 % hydrochloric acid medium, 40 mL of 20 g/Lethanol solution of dimethylglyoxime was added, and the mixture was left to stand for 5 h before vacuum filtration toseparate palladium for gravimetric determination. The precious metal bead digestion process was optimized in theexperiment by first using nitric acid（1+4）for preliminary digestion, preventing the formation of precipitates from thereaction of silver element and chloride ions that hinders further dissolution of beads, followed by hydrochloric acid additionto form aqua regia medium for complete digestion and to supply chloride ions for the generation of silver precipitationas AgCl. With hydrochloric acid as the precipitation agent and 100 mL water added for dilution, the AgCl was coagulatedby heating, then immediately filtered hot with slow⁃rate filter papers so that the silver element is separated and theeffect of AgCl precipitation on palladium adsorption is eliminated. In a 10 % hydrochloric acid medium, 40 mL of 20 g/Lethanol solution of dimethylglyoxime was added to react with palladium and generate precipitants, and the mixture wasleft to stand for 5 h to ensure complete palladium precipitation from the platinum-palladium concentrate. Interferencetests showed that coexisting elements Au（30 mg）, Pt（70 mg）, Cu（30 mg）, Pb（30 mg）, Bi（50 mg）, and Te（20 mg）did not affect palladium determination. The method exhibited relative standard deviations of 0.37 %-1.05 %（n=7）and spike recoveries of 99.32 %-100.8 %, with good reproducibility and low cost, making it suitable for batch analysisof palladium in platinum-palladium concentrates.