Functionalized PVDF membrane platforms were developed for environmentally benign in-situ nanostructured Fe/Pd synthesis and remediation of chlorinated organic compounds. To prevent leaching and aggregation, nanoparticle catalysts were integrated into membrane domains functionalized with poly (acrylic acid). Nanoparticles of 16–19 nm were observed inside the membrane pores by using focused ion beam (FIB). This technique prevents mechanical deformation of the membrane, compared to the normal SEM preparation methods, thus providing a clean, smooth surface for nanoparticles characterization. This allowed quantification of nanoparticle properties (size and distribution) versus depth underneath the membrane surface (0–20 µm). The results showed that nanoparticles were uniformly sized and evenly distributed inside the membrane pores. However, the size of nanoparticles inside the membrane pores was 13.9% smaller than those nanoparticles located on the membrane surface. Investigating nanoparticles inside membrane pores increases the accuracy of kinetic analysis and modeling aspects. Furthermore, the Fe/Pd immobilized membranes showed excellent performance in the degradation of chlorinated organics: Over 96% degradation of 3,3',4,4',5-pentachlorobiphenyl (PCB 126) was achieved in less than 15 s residence time in convective flow mode. The regeneration and reuse of this catalytic membrane system were also studied. Particles were examined in XRD upon formation, after deliberate oxidation, and after regeneration. The regenerated sample showed the same crystalline pattern as the original sample. Repeated degradation experiments demonstrated successful PCB 126 dechlorination with nanoparticles regenerated for four cycles with only a small loss in reactivity. It demonstrated that Fe/Pd immobilized membranes have the potential for large-scale remediation applications.