A d.c. polarographic method at pH 3.6 in Britton-Robinson buffer and a differential-pulse polarographic method at pH 2.6 in the same buffer system have been developed for the assay of methaqualone and methaqualone dosage forms. The differential-pulse method has increased sensitivity and is easier to use than the d.c. polarographic method. The results obtained by both methods agreed well with manufacturers' analytical data and with values obtained by non-aqueous titrimetry.