A practical method for simultaneous determination of lead and arsenic in food stuffs and others has been studied. The established procedure is as follows: Samples are destructed with a mixture of nitric acid and perchloric acid. Transfer the wet ash to a 100 ml separating-funnel, dilute to about 50 ml and neutralize. Add 5 ml of 1 M tartaric acid and 1 ml of 0.01 M I_2-KI solution and adjust the pH to about 3 with diluted hydrochloric acid. After adding 5 ml of 0.4% APDC, extract lead with 10 ml of MIBK by shaking for 4 minutes, and determine lead in the separated organic phase by measuring the atomic absorption at 2833A. Transfer the residual aqueous phase into a reaction bottle(see Fig.4), add 5 ml of hydrochloric acid(1+1),2 ml of 1 M potassium iodide and 0.5 ml of 40% stannous chloride, and let stand for 15 minutes. Add 3 g of granular zinc, immediately connect the reaction bottle to the collection unit and allow the mixture to react for 60 minutes. After absorbing of arsine to 5 ml of 0.5 M sodium bicarbonate-0.01 M I_2-KI solution (1:5), transfer the solution to a 100 ml separating-funnel, add 4 ml of 10% ammonium molybdate,5 ml of hydrochloric acid and 10 ml of MIBK, and shake for 4 minutes. After discarding the aqueous phase, wash the organic phase with diluted hydrochloric acid (1+10) for 3 times and then measure arsenic by the indirect atomic absorption method using molybdenum lamp. Recovery from citrus juice was 98.8%for lead and 73.3%for arsenic. Error of this method is 1.42% for lead and 2.0% for arsenic.