The aging behavior of precipitation hardenable 17-4 PH stainless steel is studied by analyzing the changes in microstrain, crystallite size, and dislocation density derived from the modified Williamson–Hall (mWH) method and the Fourier analysis of XRD profiles. Aging treatment of this steel at 380, 430, and 480 °C for 0.5, 1, and 3 h durations leads to changes in the microstrain due to precipitation and substructural changes caused by dislocation annihilation. The microstrain estimated from the mWH method is dominated by the precipitate-induced effects. The influence of precipitates and dislocations on the mean squared strain 〈ε2(L)〉 are separated by fitting the variation of 〈ε2(L)〉 with an expression P
0 + P
1/L + P
2, where the parameter (P
0)0.5 and P
1 are shown to be related to the precipitate-induced and dislocation density-induced microstrain, respectively. The study shows that the XRD profile analysis can be used to separate the combined effects of precipitation and dislocation annihilation.