Radiolabeling of Ivalon (polyvinyl alcohol sponge) particles permits localization of injected particles during embolization through the use of a portable gamma camera and provides a means to prevent potentially fatal complications such as pulmonary embolization. A more efficient technique of labeling Ivalon particles with technetium-99m sulfur colloid was developed. An increase in labeling efficiency allowed more accurate determination of the distribution of injected Ivalon particles. Scanning electron microscopy demonstrated the stability of the Ivalon particles during this new labeling process. Two patients with arteriovenous malformations underwent therapeutic embolization with radiolabeled Ivalon particles; gamma camera imaging of the lesion and chest was performed throughout the procedure.