A determination procedure has been developed for210Bi and210Po in environmental samples and was applied for pine needles. Bismuth-210 and210Po separated from the parent nuclide210Pb as BiOCl precipitate were extracted simultaneously by TOPO/toluene containing PPO and POPOP. The separation of210Bi and210Po from210Pb was almost satisfactory. The activity of210Bi+210Po in the TOPO/toluene was measured periodically by liquid scintillation counting for about 20 days after separation. The time course of the decreasing pattern of the activity was determined by the initial activity ratio210Po/210Bi. The decreasing pattern of the activity was compared with theoretical patterns, and best estimates for210Po and210Bi were obtained by non-linear least-squares fitting. The activities of210Bi and210Po were determined for one-year and two-year old pine needles fro the same pine tree, and weathering half-time and deposition rate of these nuclides was discussed.