An Fe–1 at.% Cu model alloy was examined by atom probe (3DAP) and small-angle neutron scattering (SANS) to verify the accordance of the gained results. The Fe-Cu alloy was heat-treated for various times at 500°C, forming Cu-rich precipitates within the Fe matrix. The chemical compositions of the precipitates and matrix found by 3DAP were used to calculate the magnetic scattering contrast. Additionally, a magnetic moment of the precipitates that contain a significant amount of Fe was taken into account for the calculation of magnetic scattering contrast. This in turn is used for the evaluation of the magnetic scattering curves gained by SANS. Both the 3DAP data as well as the scattering curves were analyzed with regard to radius, number density, and volume fraction of the precipitates as a function of aging time. The results yielded by both techniques are in good agreement and correspond to the development of the hardness of the alloy. Minor differences can be related to the cluster search algorithm used for the analysis of the 3DAP data as well as Fe overestimation based on different field phases.