A novel computer-assisted (13)C NMR spectroscopic method for the identification and determination of chlorohydrins in reaction mixtures formed during the manufacture of glycerol, is described. It utilizes the unique features of quantitative and edited (13)C NMR spectrometry and avoids chromatographic separation for identification and quantification of the mixture components. It is simple, specific and quicker than the GC-MS and GC-IR methods.