Polonium-210 in phosphoric acid has been recognized as a significant source of alpha contamination of processed Si-wafers for memory devices of computer. In the present work, a convenient method was developed for the determination of trace210Po in phosphoric acid of high purity. For the determination,209Po was used as a yield tracer. The present method consists of (1) addition of the tracer to 5 ml aliquot of phosphoric acid sample, (2) pH adjustment (to 2) of the sample solution to make up electrolytic solution, (3) electrodeposition for the simultaneous achievement of Po separation and preparation of counting source on stainless-steel disc, and (4) alpha-ray spectrometry. By the developed method, more than 95% of Po was separated from phosphoric acid sample onto counting disc. The minimum detectable radioactivity of210Po in 5 ml of phosphoric acid was about 0.03 mBq by counting the electrodeposited alpha-activity for 10 days under a counting efficiency of ≈30%.