Structural Relaxation of Salmon Gelatin Films in the Glassy State

Mechanical relaxation of glassy carbohydrates has been reported extensively in the literature; however, little work is available on protein-based systems. This study deals with the structural relaxation of salmon (Salmo salar) gelatin in the glassy state. Skin gelatin was obtained by an acid-alkaline extraction method. Molecular weight (M-w) was determined by capillary viscometry. Films prepared by casting (7% w/v) were equilibrated to a moisture content of similar to 18.4% (db). The glass transition temperature (T-g) and enthalpic relaxation were determined by differential scanning calorimetry (DSC). Mechanical properties were assessed using a texture analyzer at constant temperature and moisture content. DSC showed a T-g similar to 34 degrees C, and the selected storage temperature (T-a) was 29 degrees C (T-g-T-a= 5 degrees C). The films were aged for 0, 4, 8, 16, and 40 h. Viscometry produced values of M-w similar to 90.2 kDa. The stress relaxation was modeled by the Kohlrausch-Wlliams-Watts (KWW) equation, reporting an increase in relaxation time (tau(0)) as the ageing time increased (tau(0) similar to 6.41E+03 s for 0 h; tau(0)similar to 9.01E+ 05 s for 40 h). beta parameter was smaller for the aged films, indicating a spread of relaxation times. The derivative of KWW equation (d phi/dt) indicated a more rapid relaxation in a fresh sample compared with aged films. DSC showed an excess in enthalpy (Delta H) on the aged samples due to the non-equilibrium state of the matrix. Delta H increased with ageing time with values of Delta H similar to 2.42 J/g for the films aged for 40 h. This work demonstrated molecular relaxation process of gelatin in the glassy state, which must be taken into account if this material is used as a structure forming matrix.