Cellulose tricarbanilates (CTCs) were prepared from a range of cellulose samples (cotton linters, wood pulps, Avicel, amorphous cellulose, and cellulose II) for molecular weight distribution (MWD) studies by high performance size exclusion chromatography (HPSEC). The HPSEC columns were calibrated using CTC standards with the aid of a microcomputer. CTCs were prepared by reaction of cellulose samples with phenylisocyanate in pyridine at 80°C. For some samples, e.g., cellulose II, activation with liquid ammonia and pyridine was necessary prior to reaction in pyridine. All samples tested were also derivatised in dimethylsulfoxide at 70°C, although for high molecular weight (MW) cellulose samples some MW reduction occurred in this solvent. Conditions were determined for optimum precipitation of CTCs in aqueous methanol without coprecipitation of low MW impurities.