Various procedures for preparation of the biopolymers chitin and chitosan have been developed over the years. Preparation methodology and analysis of physicochemical properties of these biopolymers are reviewed in terms of crustacean species and diverse characterization methodology. Such properties influence biopolymer functionality differing with crustacean species and preparation methods. Monitoring of the relationship between process conditions and chitin/chitosan products is needed to insure uniformity and proper product quality control. Research with chitosan derived from crawfish processing operations indicates the need for a more integrated approach for total resource utilization. Examples of value-added processing by-products, coupled with chitosan recovery, are noted.