X-ray emission spectra have been recorded from several biologic tissues using a multichannel energy-dispersive analyzer with a retractible semiconductor detector coupled to a Cambridge Mark II scanning electron microscope. Particular attention has been given to the detection of silver in experimental argyria, of calcium in dermoid scales and in experimental necrosis of the kidney and of sulfur in the inner and outer portions of reptilian skin. Sulfur and chlorine have been found associated with silver in argyria. Phosphorus was associated with calcium both in the dermal scales and in necrotic areas. In addition to these elements, trace amounts of copper, zinc, lead, sodium, potassium, iron, arsenic, osmium and uranium have been detected in various normal and experimental situations. The applicability of the combined instrument to cytochemical problems is briefly discussed.