Abstract:Rhodium ore is an important source of rhodium, but the content of rhodium in the ore is very low and unevenly distributed. Accurate determination of its content has always been a difficult problem in analysis. In this study, a lead assay graphite furnace atomic absorption spectrometry method for highly enriching rhodium in ore was established. Using gold as protective agent，gold rhodium alloy was formed after lead fire assay separation and preconcentration. The gold rhodium alloy was dissolved in aqua regia and determined by graphite furnace atomic absorption spectrometry (GFS). Result indicated that when flux ratio m(Na2B4O7): m(Na2CO3): m(PbO): m(C6H12O6)=5:5:10:1, gold protective regent 15mg, cupellation temperature 900℃, 50 μg of rhodium was enriched. Under the selected GFS instrument conditions, The RSD（n=11）of rhodium was 6.97%～11.23%, the recovery was between 99.36%～100.94%, other coexisting precious metals 10 times as much as rhodium had no interference with the determination. This method is reliable, simple and rapid. It can be used for daily determination of Rh in mineral sample. This study is of great significance to the exploration and exploitation of rhodium resources and the comprehensive utilization of rhodium minerals.