A new method for the analysis of volatile analytes using a stopped-flow injection system originating from either a gas or liquid phase has been developed. It uses an integrated fiber optic detector which also serves as a reactor. This system combines the advantages of gas diffusion and stopped flow, making the overall assay very sensitive. Both gas streams and aqueous solutions containing ammonia were analyzed. The limits of detection are 40 ppb for gas phase analysis and 1.0 ppm for aqueous phase analysis.