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.