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The purpose of this work was to determine the total amount of water contained in dry powder and wet bead samples of microcrystalline cellulose, MCC, (Avicel PH-101), taken from various stages of the extrusion/marumerization process used to make beads and to determine the kinetic rates of water release from each sample. These samples were allowed to equilibrate in controlled humidity chambers at 25 degrees C. The total amount of water in each sample, after equilibration, was determined by thermogravimetric analysis (TGA) as a function of temperature. The rates of water release from these samples were determined by using isothermal gravimetric analysis (ITGA) as a function of time. Analysis of the results for these studies suggest that water was released from these systems by several different kinetic mechanisms. The water release mechanisms for these systems include: zero order, second order, and diffusion controlled kinetics. It is believed that all three kinetic mechanisms will occur at the same time, however; only one mechanism will be prominent. The prominent mechanism was based on the amount of water present in the sample.

The purpose of this work was to examine the sorption and desorption of water by various samples of microcrystalline cellulose, MCC (Avicel PH-101), taken from the extrusion/marumerization process, and to provide data that may explain how water affects the MCC polymer matrix during the formation of beads. Two isopiestic (humidity) studies were conducted: the first used samples exposed directly to controlled humidity conditions, whereas the second used samples that were freeze-dried before being exposed to controlled humidity conditions. Water sorption and desorption were determined gravimetrically. When both sets of samples were initially exposed to low-humidity conditions, they reached equilibrium by desorbing water. When these samples were initially exposed to high-humidity conditions, the high moisture content samples desorbed water, whereas the low moisture content and the freeze-dried samples sorbed water to reach equilibrium. When the first set of samples was initially exposed to high- and then to low-humidity conditions, they reached the same water content achieved by being equilibrated directly at the low-humidity condition. However, samples that were initially exposed to low- and then to high-humidity conditions had equilibrium water contents that were lower than those achieved by being equilibrated directly at the high-humidity condition. The original MCC systems exhibit a hysteretic effect above 85%, whereas the freeze-dried systems have a broader range hysteretic effect starting at 20% relative humidity. The results suggest that the internal structure of the MCC polymer fibers must change with the sorption and desorption of water, supporting the autohesion theory.