A simple and rapid method is described for the determination of alkene-l-sulfonates in a-olefin sulfonates (AOS). AOS are primarily mixtures (detergent range) of sodium salts of alkene-l-sulfonates (mixture of double bond position isomers) and hydroxyalkane-1sulfonates plus small amounts of disulfonates in a 30-40% aqueous solution. The analysis consists of titrating the sample in 98% acetic acid-2% water solution with a stream of ozone to an indicator endpoint (Rouge Organol B.S.) which is detected photometrically. In tests with model compounds, a long carbon chain alkene-l-sulfonate, sodium hexadecene-1-sulfonate, and a 1-alkene-l-sulfonate, sodium l-propene-l-sulfonate, were quantitatively determined with no interference from a hydroxyalkane-1sulfonate, sodium hydroxytetradecane-l-sulfonate. In contrast, an alternative method of determining unsaturation, Brown hydrogenation, does not quickly and quantitatively determine 1-alkene-l-sulfonates.