The application of synchrotron studies provides an in-depth fundamental understanding of the chemistry at the solid-multi-gas interface which in turn can provide the atomistic details necessary for material design to develop technologies for energy storage and conversion, decontamination, or defense. The utilization of in situ synchrotron capabilities enables the study of materials surface chemistry which probe the changes in catalysts and sorption materials while also correlating to the chemistry in real time. Metal Organic Frameworks (MOFs) are remarkable porous materials with intricate designs and connectivity and have high performance in catalytic transformation applications and materials for the destruction of chemical warfare agents (CWA). Understanding the role of reactive MOF catalysts and adsorbents in the decontamination of chemical warfare agents and in heterogenous catalysis (mild temperatures) is necessary to optimize material properties, thereby promoting favorable interactions between adsorbent and adsorbate molecules for optimal decontamination, defense and performance. Metal supported nanocatalysts are equally promising catalyst with stability for thermally enabled catalytic transformation. This presentation will describe three research thrusts aimed at using porous, high surface area materials such as monometallic or bimetallic MOFs for CWA decontamination technologies and (Pt, Mo, and Ru) metal supported catalysts for C-C bond activation respectively with the focus on using a multimodal scattering and spectroscopic approach to study the behavior of these complex materials under different environments. This in situ approach is crucial to understanding the working mechanism of materials under dynamic relevant conditions.