铂钯精矿是以铜阳极泥为原料，经卡尔多炉粗炼—银电解—王水分金后得到的产物，多用于回收钯，准确测定铂钯精矿中钯对实现铂钯精矿中钯资源化利用具有重要意义。建立了铅试金富集—丁二酮肟重量法测定铂钯精矿中钯的检测技术。实验采用铅试金预富集，硝酸（1+4）和盐酸分步消解贵金属合粒后，以盐酸为沉淀剂，加水稀释后立即趁热过滤，消除银元素干扰，在10 %盐酸介质下，加入 40 mL 20 g/L丁二酮肟乙醇溶液，静置 5 h，抽滤分离钯，丁二酮肟重量法测定钯。实验优化了贵金属合粒消解方法，先采用硝酸（1+4）初步消解，避免银元素与氯离子生成沉淀阻碍合粒的进一步溶解，之后加入盐酸生成王水介质，合粒消解完全，同时提供氯离子与银形成氯化银沉淀；以盐酸为沉淀剂，加入 100 mL水稀释，加热使氯化银沉淀凝聚，立即用慢速滤纸趁热过滤，实现银元素分离，并消除氯化银沉淀对钯的吸附影响；在 10 %盐酸介质下，加入 40 mL 20 g/L丁二酮肟乙醇溶液与钯反应生成沉淀，静置 5 h，确保铂钯精矿中钯沉淀完全。通过干扰实验确定共存元素 Au（30 mg）、Pt（70 mg）、Cu（30 mg）、Pb（30 mg）、Bi（50 mg）、Te（20 mg）不干扰钯的测定。本方法测定结果的相对标准偏差（n＝7）为 0.37 %~1.05 %，加标回收率为 99.32 %～100.8 %，且方法重现性好、成本低，适用于批量分析铂钯精矿中钯。

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.