Classical diffusion measurements in intermetallic compounds are often complicated by low diffusivities or low solubilities of the elements of interest. Using secondary ion mass spectrometry for measurements over a relatively shallow spatial range may be used to solve the problem of low diffusivity. In order to simultaneously obtain measurements on important impurity elements with low solubilities we have used ion implantation to supersaturate a narrow layer near the surface. Single crystal NiAl was implanted with either 12C or both 56Fe and 12C in order to investigate the measurement of substitutional (Fe) versus interstitial (C) tracer diffusion and the cross effect of both substitutional and interstitial diffusion. When C alone was implanted negligible diffusion was observed over the range of times and temperatures investigated. When both Fe and C were implanted together significantly enhanced diffusion of the C was observed, which is apparently associated with the movement of Fe. This supports one theory of dynamic strain aging in Fe alloyed NiAl.