Abstract: The continuous determination of 12 elements in geochemical samples by inductive coupled plasma-atomic emission spectrometry (ICP-AES) and flame atomic absorption spectrometry (FAAS) was reported in this paper. Samples were digested with mixed acid of HCl-HF-HNO₃-HClO₄ and Cu, Pb, Zn, Co, Ni, Cr, Sr, Ba, V, Mn in the sample solution were determined directly by ICP-AES. Then, Ag and Cd in the same sample solution were enriched by extraction with potassium iodide-methyl isobutyl ketone (KI-MIBK) and determined by FAAS. The precision of FAAS method for Ag and Cd was 6.5% and 4.7% RSD (n=12), respectively. In comparison with the common analytical method, the proposed method provides the higher sensitivity, good accuracy and precision, high economy, high efficiency and is suitable for routine analysis of these elements in geochemical samples.