An integrated analytical methodology, including spectroscopic techniques and micromorphology, has been used to analyse mud plaster sequences and natural sediments from the Neolithic site of Catalhoyuk in Turkey in order to explore the uses and perceptions of soils and space at the site. The sediments were analysed using bulk FT-IR spectroscopy, FT-IR microscopy, X-ray diffraction, Scanning Electron Microscopy with Energy Dispersive X-ray Analysis, Atomic Absorption and X-ray fluorescence spectroscopy. Mapping of multiple plaster sequences was conducted using FT-IR microscopy and spatially resolved X-ray diffraction using the synchrotron source at the Daresbury Laboratory. Experiments using the FT-IR microscope in reflectance mode and SEM/EDX were conducted directly upon the surface of thin sections so that the spectroscopic analysis could be directly combined with micromorphological analysis, retaining additional contextual information.