An evaluation of six techniques for measuring porosity of ribbons produced by roller compaction

Ribbon porosity is a critical parameter to monitor in the roller compaction process. In this study, six techniques for measuring the porosity of solid compacts, i.e., manually by caliper (Caliper), X-ray microtomography (µCT), off-line near-infrared spectroscopy (NIR), laser triangulation (Laser), mercury intrusion porosimetry (MIP), and GeoPyc, were compared using a set of rectangular ribblets of microcrystalline cellulose (MCC). These ribblets, which were compressed at 8-130 MPa on a compaction simulator, exhibited porosities over the range of 0.09 - 0.52. Subsequently, porosities of MCC ribbons made on a roller compactor at specific roll forces of 1.8 kN/cm and 8.8 kN/cm were measured. The Caliper method is convenient for samples with a simple shape but not suitable for real ribbons. The accuracy of GeoPyc measurement relies on accurate conversion factor (unit in cm³/mm), sample shape and size, and sufficient sample volume percentage in the medium. The µCT data is more accurate at lower porosities (< 0.2), while the MIP data is more accurate at higher porosities (> 0.4). The Laser method has good accuracy and is more reproducible compared to other methods in the ribblets measurement. The NIR method is fast, which makes it suitable for in-line monitoring of changes in ribbon quality, but porosity quantification is sensitive to sample presentation, such as surface curvature and roughness. These insights could assist in the choice of the most appropriate method for monitoring ribbon porosity to guide the development and optimization of a roller compaction process for a given formulation.