Abstract: The content of rhodium in solution was determined by the flame atomic absorption spectrometry method. This article studied different factors that influenced the determination of rhodium, including releasing agent, inorganic acid and coexistence metal ions. The result showed that the determination sensitivity of rhodium can be increased and the interference of inorganic acid and coexistence metal ions can be disappeared by adding CuSO4-LaCl3 as releasing agent. The experiments indicated that the adding amount for 5 ml rhodium solution was 1 ml each of CuSO4 and LaCl3 solutions (the concentrations were both 5 mg/ml). The recovery of standard addition ranged from 99.85% to 105.05%. The adding quantity of releasing agent in this paper is less than others. The method is simple, rapid and accurate.