A quantitative separation procedure for210Po in lead has been developed by cupferron and dithizone extraction. The210Po activity is plated on a silver foil for counting with a ZnS(Ag) scintillator, or by α-spectrometry with a surface barrier semiconductor. Different lead samples were analyzed ranging from very old lead with a negligible210Po content to recently manufactured lead samples showing up to 9100 disintegrations per hour and per gram of lead. The reproducibility and the accuracy of the analyses are satisfactory.