NEXAFS microscopy studies of the association of hydrocarbon thin films with fine clay particles

The nature of organic species associated with clay minerals plays a significant role in several processes, from hydrocarbon recovery in oil sands to contaminated soil remediation and water treatment. In this work, we address the use of scanning transmission X-ray microscopy (STXM) in conjunction with near edge X-ray absorption fine structure (NEXAFS) spectroscopy to study the microstructure and chemistry of organic–clay associations in situ. A model system based on methylene blue and illite is used to explore the sensitivity of NEXAFS microscopy to these interactions, and to identify and resolve experimental challenges in these measurements. We find that sample contamination from X-ray induced photodeposition is a significant problem in STXM microscopy, but also that this problem can be substantially reduced with a liquid nitrogen cooled anticontaminator. With appropriate sample preparation and experimental procedures, we find that STXM microscopy is sensitive to thin carbon adsorbates on clay surfaces.