ABSTRACT: Carboxymethyl starch (CMS) with degree of substitution (DS) ranging from 0.1 to 0.32 was prepared from sago (Metroxylon sagu) starch in non-aqueous medium using isopropanol as a solvent. The physico-chemical, rheological, and thermal properties of the starches were investigated. At room temperature (25 °C), CMS hydrated readily, resulting in higher swelling power compared with native (unmodified) starch. Light microscopy revealed that CMS granules imbibed more water than native starch at room temperature and thus caused a larger increase in granule size. Some of the CMS granules lost their integrity. Scanning electron microscopic observation revealed fine fissures on the surface of CMS (DS 0.32) granules compared with a relatively smooth surface of native starch granules. Carboxymethylated sago starch exhibited excellent dispersibility and cold water solubility as judged by the absence of peak viscosity in the pasting profile (determined by Rapid ViscoAnalyzer). Pasting profile of CMS was qualitatively similar to pregelatinized starch. Despite exhibiting greater swelling power, CMS showed significantly lower pasting viscosity compared with the native starch. Intrinsic viscosity was also greatly reduced by carboxymethylation. Studies using differential scanning calorimetry (DSC) showed that transition temperatures and enthalpies decreased with an increase of degree of substitution. CMS at higher substitution levels (DS 0.27 and 0.32) showed significantly lower retrogradation tendency, as indicated by lower setback, absence of DSC endotherm upon storage at 4 °C and lower syneresis upon repeated freeze-thaw cycles. The results suggested that retrogradation might be effectively retarded by the presence of the bulky carboxymethyl group.