In this work we present a suitable way to release lead and polonium from sediments and other samples. Results obtained by hot-acid dissolution and cold leaching showed that while good recoveries of 210Pb were obtained in both the cases, 210Po recovery in hot dissolution was poor due to volatility of polonium, and might lead to erroneous results due to non-equilibration of added 208Po tracer and 210Po in the matrix. A Sr-resin column was used for separation of Pb and Po. We also studied the possibility of reusing columns used earlier. The most significant problem in reuse is the reduction in column capacity, resulting in a reduction to half of its initial capacity. Other natural radionuclides do not interfere in the determination of 210Pb and 210Po and we found no measurable contamination of the column on repeated usage.