The present paper describes a procedure for preparing vascular corrosion casts of rat myocardial microvasculature. Essential components of the procedure include: partial self clearing of the heart in vitro; cardiac arrest by infusion of KCl; retrograde aortic root infusion of Mercox-Sevriton casting resin; KOH digestion of ventricular tissue; and desiccation and mounting of casts for scanning electron microscopy. About 50% of rats yielded complete casts. Vasculature closely paralleled muscle fiber orientation. Capillary beds characteristically exhibited branching, many intercapillary cross bridges, and occasional coil-ing. Average capillary cast diameter (5.6 μm) and intercapillary distance (15 μm) are comparable to results from in vivo studies. From preliminary calculations, vascular volume represents about 10% of the ventricular walls. These data indicate that vascular corrosion casts may be useful in the analysis of pathologic states and in determining the role of potential therapeutic interventions