This paper describes and compares three techniques that can be used to characterize the substituent content of hydroxypropylcellulose (HPC and L-HPC) and hydroxypropyl methylcellulose (HPMC): gas-liquid chromatography (GLC) with a BP1 column and FI detection, 13C-NMR spectroscopy of hydrolysed samples, and Raman spectroscopy. GLC and 13C-NMR spectroscopy both allow independent quantification of hydroxypropoxyl and methoxyl contents. 13C-NMR spectroscopy, though requiring lengthier sample preparation, has the advantage of also quantifying the degree of substitution at each substitutable glucopyranose hydroxyl. Raman spectroscopy may be useful for rapid approximate estimation of hydroxypropoxyl content.