Abstract: This article studied on the oxygen flask combustion spectrophotometry for determining the chloride content in polyurethane foam. Polyurethane foam was decomposed firt by oxygen flask combustion method, then the chloride content was determined with mercury thiocyanate spectrophotometry. The experimental results indicated that the oxygen flask combustion method-spectrophptometry can determine the chloride content in polyurethane foam effectively. This method was simple, accurate and highly practical, it sensitivity is high, and suitable for the rapid analysis.