Silica gel chemically modified with dithiocarbamate groups (DTCS) was used for separation and preconcentration of precious metals and their subsequent determination in geological samples and their processing products by inductively coupled plasma optical emission spectrometry and inductively coupled plasma mass-spectrometry. DTCS was characterized by TGA/DSC, FT-IR, and CHNS-analysis. DTCS quantitatively extracted Au 3+ , Pd 2+ , Pt 2+ , Pt 4+ at 20°C from 0.5-4.0 M HCl media and Rh 3+ , Ir 4+ , Ru 4+ ,Os 4+ at 95°C in the presence of 0.025M SnCl 2. Two-column procedure was proposed to separate precious metals from matrix components and to separate kinetically inert precious metals from kinetically labile ones.