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The intrinsic diffusivities of individual components in several binary systems have been determined with vapor‐solid type diffusion couples. In this type of couple a high vapor‐pressure component is diffused from the vapor phase into a slab of lower vapor pressure initially containing inert markers on its surface. Diffusivities may then be calculated from marker movement and diffusion‐penetration curve data. Equations necessary for analysis of such couples are developed. The alpha brass, copper‐nickel, and silver‐gold systems were investigated. Observations of polygonization during diffusion and dimensional changes normal to the diffusion direction were also made. Porosity formation, which occurred only in the vapor‐solid silver‐gold couples, was investigated in detail and was compared to porosity formation in corresponding sandwich couples. The general use and limitations of such couples in diffusion studies are discussed.