Aging processes exhibiting cluster to precipitate transitions were studied in polycrystalline line austenitic iron-base alloys with a Siemens' Guinier camera. This camera combines the Seemann-Bohlin focusing geometry with a curved-crystal monochromator arid thus maximizes the resolution of observed sidebands and the weak precipitate lines. Growth studies encompassing a cluster-size range of 15 to 70 unit cells were followed. For the systems of interest, this coincided with a variation from detectable hardness increase to a stage of maximum hardness immediately preceding precipitation, Cluster sizes were calculated on the basis of the Guinier model; variation with time and temperature permitted calculations of an apparent activation energy in the one system where decomposition was spontaneous. An iron-nickeltitanium alloy was used to study aging in a ternary system. Behavior was classic in that the cluster size present on quenching grew with aging coincident with a simultaneous hardness increase. Calculation of activation energies indicated strongly that transportation of nickel to, or iron from, the cluster was rate determining. Upon overaging, the nickel-titanium enriched clusters gave way to the hexagonal Ni2Ti phase. An iron-nickel-chromium-niobium quaternary, in addition to presenting a clustering system similar to the above ternary, showed two rather interesting phenomena. First, chromium was necessary for precipitation; the ternary ironnickel-niobium did not age. Secondly, a stable Pe2Nb Laves phase present upon quenching from 2200°F disappeared on aging in favor of nickel-niobium clusters; an incubation time for the formation of these clusters existed, and its duration was about 4 hr. An asymmetry was noted in the diffraction intensities about the (311)γ line in both systems. In the iron-nickel-titanium case, the asymmetry was only in intensity, whereas, with the iron-nickel-chromium-niobium alloys, the asymmetry existed in both intensity and position. Interpretation of these observations is made on the basis of anticipated variations in scattering factors, lattice spacings, and cluster sizes.