HWasu Corporation produces an enormous amount of PVC acetylene gas to wash waste sulfuric acid every year, and the composition of waste acid impurity is complex. The stench restricts the reuse of waste sulfuric acid, This paper establishes the detection scheme which is divide int three parts,respectively: escaping of the exhaust gas, liquid slag washing and washing slag quantitative analysis.Burning waste acid solid content of 11.40%, light component is 97.18%, sulfuric acid content of 79.22%, after washing slag of weight percent is 7.30%, Washing liquid slag quality percentage of 4.10%.Escaping gases mainly contain acetylene, hydrogen chloride, sulfur oxide impurities. Washing slag liquids mainly contain phosphoric acid root, organophosphorus, chloride, calcium, magnesium,iron ions and sulfuric acid root ion. Washing slags mainly contain silicon dioxide, carbon, hydrogen, calcium oxide, magnesium oxide, ferric oxide,and etc. Finally through the balance calculation of data, We can figure out that the experimental data is accurate and reliable for comprehensive utilization of wast sulfuric acid to provide basic theory data.