Eudragit retard microcapsules were prepared using an improved non-solvent addition phase separation process with tetrahydrofuran as the solvent. The evolution of microcapsule wall formation was studied by direct methodology. Eudragit coacervation was effected by progressive uptake of tetrahydrofuran by the non-solvent cyclohexane in the presence of a protective colloid, polyisobu tylene (PIB). The core materials had a higher affinity for the acrylic that the PIB phase, thus ensuring encapsulation. Microcapsule batch reproducibility depended mainly on the variation in particle size distribution of the recrystallized core material. All batches gave apparent first-order release profiles, confirmed by regression procedures. The release rate was decreased by raising the wall/core ratio, holding constant concentration of either the wall polymer or the core material. Increase in the non-solvent addition rate elevated the release rate, probably due to structural changes in the microcapsule wall. The velocity fell, however, with decrease in particle size of the core material, contrary to expectations. PIB concentration increase elevated the release rate by enhancing wall porosity, shown by scanning electron microscopy.