Si-Si(B) doping superlattices (pipi structures) were grown by MBE and studied using double crystal x-ray diffraction and SIMS. Detailed analysis of the complex x-ray rocking curves required comparison of experimental data with theoretically simulated data. It is demonstrated that this technique is sensitive to irregularities in the dopant composition, dopant distribution and superlattice period. The B concentration profile is shown to spread well into the intrinsic layers and the extent and magnitude of the dopant distribution has been quantified. A comparison of this data with SIMS showed good agreement for the distribution of B and reasonable agreement for the peak values of B concentration.