As part of the National Acid Precipitation Assessment Program (NAPAP), the U. S. Geological Survey is cooperating with other agencies to test the effects of acid deposition on building stone. A 10-year test-site study has been organized for the purpose of correlating possible stone deterioration with environmental factors. In Summer 1984, slabs of building stone, 3 by 2 by 2 inches, were exposed to the atmosphere at four test sites where the pH of precipitation and other meteorological variables are continuously monitored. This paper examines the development of one experimental technique used in this study - the application of diffuse spectral reflectance methods for laboratory and in situ measurement of those properties of stone which may be affected by acid deposition.