Various solvents and operating conditions were investigated for paperchromatographic separation of the various esters in the mixture obtained by the reaction P4O10+ 4ROH. Optimum separation was obtained with a propanol-isobutanol-water-ammonia solvent at 10° during 16 hr and perchloric acid-ammonium molybdate developer. These conditions were found to produce complete separation in all investigated mixtures, independently of the nature of the organic chain in the esters. Preparative separation of the various products was obtained by column chromatography, using the same solvent as in paper chromatography on a cellulose-packed column.