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Surface chemical compositions of starch nanocrystals (SNC) prepared using sulfuric acid (H 2 SO 4 ) and hydrochloric acid (HCl) hydrolysis were analyzed by X-ray photoelectron spectroscopy (XPS) and FT-IR. The results showed that carboxyl groups and sulfate esters were presented in SNC after hydrolysis with H 2 SO 4 , while no sulfate esters were detected in SNC during HCl-hydrolysis. TEM results showed that, compared to H 2 SO 4 -hydrolyzed sample, a wider size distribution of SNC prepared by HCl-hydrolysis were observed. Zeta-potentials were −23.1 and −5.02 mV for H 2 SO 4 - and HCl-hydrolyzed SNC suspensions at pH 6.5, respectively. Nevertheless, the zeta-potential values decreased to −32.3 and −10.2 mV as the dispersion pH was adjusted to 10.6. After placed 48 h at pH 10.6, zeta-potential increased to −24.1 mV for H 2 SO 4 -hydrolyzed SNC, while no change was detected for HCl-hydrolyzed one. The higher zeta-potential and relative small particle distribution of SNC caused more stable suspensions compared to HCl-hydrolyzed sample.

Surface Chemical Compositions and Dispersity of Starch Nanocrystals Formed by Sulfuric and Hydrochloric Acid Hydrolysis