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The purpose of the research was to introduce a procedure to derive a powder compression parameter (EM A) representing particle yield stress using an effective medium equation and to compare the EM A parameter with the Heckel compression parameter (1/K). 16 pharmaceutical powders, including drugs and excipients, were compressed in a materials testing instrument and powder compression profiles were derived using the EM and Heckel equations. The compression profiles thus obtained could be sub-divided into regions among which one region was approximately linear and from this region, the compression parameters EM A and 1/K were calculated. A linear relationship between the EM A parameter and the 1/K parameter was obtained with a strong correlation. The slope of the plot was close to 1 (0.84) and the intercept of the plot was small in comparison to the range of parameter values obtained. The relationship between the theoretical EM A parameter and the 1/K parameter supports the interpretation of the empirical Heckel parameter as being a measure of yield stress. It is concluded that the combination of Heckel and EM equations represents a suitable procedure to derive a value of particle plasticity from powder compression data.

Tablet production involves compression of free flowing powder in an enclosed cavity of defined geometry. The complexity of the powder bed system necessitates that a way be found to better understand what occurs during compression. One such approach is by means of compaction equations, of which, the Heckel and Kawakita equations are the best known. This work attempts to experimentally evaluate the applicability of the effective medium (EM) equation introduced by Frenning et al. (2009) to powder systems. Two powder types (sodium chloride and lactose monohydrate), each consisting of three size fractions (<40, 125-212 and 212-300 mu m) were characterised and compressed to a pressure of 500 MPa. These powders were chosen because of their differing mechanical properties. An invariance which is inherent in the EM equation is exposed by varying the starting points of compression, and can yield insights into compression mechanisms. Such invariant regions were observed once plastic particle deformation started to dominate the compression behaviour, and enabled the determination of the point where particle rearrangement stops.

We employ the carbon paper technique with the aim of investigating the effect of spherical-agglomerate (pellet) strength on force distributions, through confined compression of approximately 1 mm sized pellets formed from microcrystalline cellulose and polyethylene glycol. The carbon paper technique relies on the transference of imprints from compressed pellets onto white photo quality paper, which are digitised and processed via image processing software. The investigated pellets can both deform plastically and develop localised cracks in response to an applied stress, while remaining largely intact during confined compression. Our results indicate that such crack formation - henceforth referred to as fracture - has a decisive influence on force distributions. Previous work on non-fracturing systems has found that the distribution of normalized forces tends to narrow with increasing particle deformation. No narrowing is observed after the point of fracture in this study and the width of the distributions - as quantified by the standard deviation of non-normalized forces - is found to increase with the difference between non-normalized mean force and fracture force. Additional corroborative results show that spatial force-force correlations typically exhibit a marked change once the fracture force is exceeded.

We employ the carbon paper technique to aid the understanding of in die force and spatial distributions, upon compression of approximately I mm sized spherical agglomerates (pellets) of microcrystalline cellulose (MCC). The aim in this study was to test for the effect of lubricant film on force and spatial distributions. Pellets of MCC were formed via granulation and extrusion/spheronisation. Investigation of pellet bed compression was performed on a materials tester. Prior to compression studies the pellets were characterised for bulk density. size and deformability. Two pellet types were investigated; MCC and MCC lubricated with magnesium stearate. The carbon paper technique relies upon carbon paper as the medium for transferring imprints from compressed pellets onto photo quality paper. The digitised images of these imprints form the basis of analysis through the use of image processing software. Using the carbon paper technique within the range of 10-30 MPa indicates that lubrication does not have a significant effect on the distribution of forces between spherical agglomerates during uniaxial compression. Spatial analysis of the imprints revealed that the lubricated pellets exhibited a higher packing order than the unlubricated ones at low applied pressures (10 and 20 MPa), a difference that could not be observed at 30 MPa. Hence interparticle friction and/or cohesion appear to influence the initial particle rearrangement, whereas confinement is suggested to dominate at higher pressures.

A simplified model for confined compression of granular materials is considered, which idealizes the collection of particles as a (central) force network. Applying an effective-medium procedure, an equation with micromechanically well-defined parameters is derived, which relates the applied pressure to the engineering strain of the powder during uniaxial compression. Despite the simplicity of the model, comparison with experimental data for mm-sized spherical granules indicates that this equation is able to satisfactorily predict the overall compression profile from single-particle data.