<p><i>Objective</i>: To study the solid state modifications of ibuprofen (IBU)-loaded spray-congealed glyceryl dibehenate (GB) solid lipid microparticles (SLMs) and the influence of polymeric additives using a combination of calorimetric and spectroscopic techniques.</p> <p><i>Materials and methods</i>: IBU-loaded SLMs were produced by spray congealing with GB as the matrix material. Polyvinyl-2-pyrrolidone-vinyl-acetate (PVP/VA) and ethylcellulose (EC) were employed as additives. Of particular interest in this study were the solid state modifications of the drug and GB matrix induced by spray congealing and the effects of aging, as well as drug–matrix interactions. Fourier transform infrared spectroscopy, nuclear magnetic resonance spectroscopy, differential scanning calorimetry, hot stage microscopy and powder X-ray diffraction provided complementary analyses in understanding drug and lipid matrix polymorphism and interaction. The yield, morphology, drug content and encapsulation efficiencies of SLMs were also investigated.</p> <p><i>Results and discussion</i>: Drug encapsulation efficiencies and yields of spray congealed SLMs were consistently high for all formulations. GB congealed as an unstable α-polymorph which reverted to the stable β′-polymorph within a few weeks. PVP/VA accelerated the polymorphic conversion in less than a week, while EC took about a year. IBU formed a solid solution with GB regardless of the GB polymorphic form.</p> <p><i>Conclusions</i>: Spray congealing is efficient for producing drug-loaded SLMs. It induces polymorphic changes in GB. The latter incorporated 20%, w/w IBU as a solid solution and polymeric additives exerted contrasting effects on the GB polymorphic conversion.</p