An attempt to cast light into starch nanocrystals preparation and cross-linking.

Potato starch was hydrolyzed with 2.2 or 3.7 M hydrochloric acid in order to obtain the nanocrystals which afterwards were chemically cross-linked with sodium hexametaphosphate. The stronger acidity resulted in smaller nanocrystals with mean size of 48 nm in a shorter time. X-ray diffraction confirmed the dominant crystalline nature of particles and Fourier transform infrared spectroscopy suggested the presence of lower number of free hydroxyl groups in nanocrystals after cross-linking. Starch nanocrystals showed two distinctive differential scaning colorimetry endotherms at 26 and 125 °C, attributed to destruction of nanocrystals lattice and moblizing of each nanocrystal's structure, respectively. Cross-linking resulted in a tenacious spatial arrangement of nanocrystals, strengthening the crystals lattice against phase transitions induced by heating. Scanning electron microscopy images confirmed the particle size measured for nanocrystals by light scattering. Atomic force microscopy topographic images suggested that starch nanocrystals were originated from small amylopectin blocklets in granular assembly of starch.