Mechanisms underlying the limited injectability of hydraulic calcium phosphate paste. Part II: particle separation study.

Calcium phosphate cements (CPCs) are of great interest for bone augmentation procedures. In these a hydraulic calcium phosphate paste is injected through a small bore needle into the bone. The injectability of these pastes is relatively poor, resulting into partial injection only. In earlier studies we have shown that phase separation brings the injection process to a halt. Phase separation is characterized by a faster flow of the liquid than of the solid during paste extrusion. So far it is unclear whether or not particle separation contributes to the poor injectability of such hydraulic pastes. It is hypothesized that fine particles behave like a liquid and thus separate under the injection pressure, leaving larger particles behind. A factorial experimental design was used to examine this hypothesis. The particle size distribution (PSD) of the extrudate was measured over the course of each injection experiment using laser diffraction. The solid content of the paste was further inspected using scanning electron microscopy. A total of 48 experiments covering four factors at two levels each were performed. One factor was the ultrasound exposure duration, to ensure the dispersion quality of the particles during the PSD measurements. Another factor was the location of the samples over the course of the injection, so as to compare the extrudate with the PSDs remaining in the syringe. The liquid:powder ratio (LPR) in the injected paste was another factor investigated. Specifically, two different pastes with 40% and 50% LPR were examined. The dispersal medium was a fourth factor investigated, to ensure adequate dispersion of the particles during the PSD measurements. Analysis of variance showed that sample location did not significantly affect PSD. No apparent PSD change for the extruded paste and the paste remaining in the syringe could be detected by scanning electron microscopy. In conclusion, the present study did not show any evidence suggesting that particle separation occurred over the course of injection and thus that phase separation remains the main phenomenon leading to the poor injectability of CPCs.