Micro-scale measurement of the mechanical properties of compressed pharmaceutical powders. 1: The elasticity and fracture behavior of microcrystalline cellulose.

The feasibility of using very small compacts ( approximately 8.0 x 4.5 x 0.4 mm; approximately 20 mg) to determine the elasticity and fracture behavior of compressed pharmaceutical powders using the three-point beam-bending technique was evaluated. Compacts of microcrystalline cellulose with a range of porosities were tested using a thermomechanical analyzer and values for the Young's modulus and critical stress intensity factor at zero porosity (E(0) and K(IC0)) were determined by extrapolation. The value of E(0) measured at ambient relative humidity on un-notched beams was found to be in close agreement with that reported for much larger samples, and the value of K(IC0) for the small notched compacts was at the lower limit of the accepted range of values for microcrystalline cellulose. The fracture toughness (R) and total energy of fracture (U) for the notched specimens were also determined and used to estimate the apparent surface energies for crack initiation (gamma(i)) and for total fracture (gamma(f)). To further probe the utility of the micro-scale mechanical testing techniques, the effects of humidity on the various mechanical properties of the small microcrystalline compacts were examined and it was found that E(0), K(IC0), R(0), gamma(i0) and gamma(f0) each decreased as the surrounding humidity (and water content of the samples) increased.