In the present study, the effect both of the botanical source and proportion of starch produced from agricultural surplus on the microstructure properties of starch/chitosan/glycerin films was tested. Effective gas transport properties gas diffusion transfer was performed. Starch/chitosan/glycerol biodegradable films were obtained by casting method from giant squid (Dosidicus gigas) pen chitosan mixed with glycerin and starch. Four starch samples were prepared using exceeding or low quality biomass including broken rice grains, hard yellow corn surplus, banana surplus form exportation activity and low quality cassava in three different weight proportion (chitosan/starch) corresponding to 1/1, 2/1 and 5/1. Extraction of starch from the raw material was carried out by mixing it with a water solution of sodium disulfite (5 wt.%). Afterwards, the obtained suspension was filtered and then decanted at 5°C for 24 h. The obtained starch was washed repeatedly with distilled water and ethanol (96 vol.%). Finally, the starch samples were dried at 55°C for 48 h, crushed and sieved. It was found that the gas diffusion transport properties significantly depend on the starch source used. Differences in diffusion transport rates through the films prepared with different starches are related to the size and distribution of granules of starch in the films and/or the amylose conten.