A modification of the Novikoff-Goldfischer alkaline 3,3'-diaminobenzidine medium for visualizing peroxisomes is described. It makes possible light microscopic as well as electron microscopic studies of a recently described class of peroxisomes, the microperoxisomes. Potassium cyanide (5 x 10–3 M) is included in the medium to inhibit mitochondrial staining, the pH is 9.7 and there is a high concentration of H2O2 (0.05%). Two cell types have been chosen to illustrate the advantages of the new procedure for demonstrating the microperoxisomes: the absorptive cells in the human jejunum and the distal tubule cells in the guinea pig kidney. Suggestive relations of microperoxisomes and lipid are described in the human jejunum. The microperoxisomes are strategically located between smooth endoplasmic reticulum that radiates toward the organelles and contains lipid droplets and "central domains" of highly specialized endoplasmic reticulum which do not show the lipid droplets. The microperoxisomes are also present at the periphery of large lipid-like drops. In the guinea pig kidney tubule there is a striking difference between the thick limb of Henle and distal tubule. The distal tubule has a population of cells with large numbers of microperoxisomes readily visible by light microscopy; these cells are not present in the thick limb of Henle. Other differences between the two are also described.