X-ray diffraction is a widely use method to measure phase content and crystallite size of catalytic nanoparticles for electrodes of fuel cells. Newer instrumentation and analysis techniques, such as external standard (K-factor) and pattern cleaning, can be used to extend the functionality of X-ray diffraction to monitor catalytic loading and the thickness of catalytic electrode layers on catalyst coated membranes (CCM). Furthermore, wide-angle X-ray scattering and near-infrared spectroscopy can be used to monitor the free water content and crystallinity of the Nafion membrane during film deposition and heat treatments. These techniques can be combined for both research-level in-situ measurements to optimize the fuel cell performance and as a quality control tool during production. This presentation will demonstrate how XRD and NIR can be more fully utilized for characterization of CCM's and membrane electrode assemblies.