In acidic medium, malonic used as masking agent, let the mixed aqueous of chlorine dioxide and chlorine react with Fe2+, then have the residual Fe2+ coloured with 1.10phenanthroline solution. The authors can quantify the content of chlorine dioxide and chlorine in the water by detecting the difference of absorbtivity of the coloured solution when it is no masking agent and it is added masking agent. The method is simple, innocuity, specific, quick, accurate and sensitive. The mini detect limitation are:Chlorine: 7.66×10-3mg/L,dioxide Chlorine: 2.91×10-3mg/L.R is 0.9997,CV is 2.55%.
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