A simple and specific technique is used in analyzing pharmaceutical preparations (capsules, elixirs, syrups, and tablets) for theophylline and related compounds. The procedure consists of dissolving (diluting) appropriate amounts of the preparations and standards in (with) a 1 M KI-water solution, spotting 5 μL of each resultant solution onto filter paper discs, determining the phosphorescence intensities at room temperature and comparing sample signal levels to those of standards. The quantities of active ingredients and standards used in the determinations ranged from 25 ng to 1 μg. The results indicate that room temperature phosphorescence is useful for analyzing pharmaceutical preparations where active ingredients are usually contained in a wide variety of matrices.