Combining Thermal Hydrolysis and Methylation-Gas Chromatography/Mass Spectrometry with X-ray Photoelectron Spectroscopy to Characterise Complex Organic Assemblages in Geological Material

Abstract What follows is a method applicable generically to the analysis of low levels of organic matter that is embedded in either loose fine-grained or solid geological material. Initially, the range of organic compounds that could be detected in a geological sample using conventional pyrolysis chromatography/mass spectrometry was compared to the range that was detected using thermally assisted hydrolysis and methylation-gas chromatography/mass spectrometry (THM-GC/MS). This method was used to validate the synthetic components fitted to X-ray photoelectron spectroscopy (XPS) carbon spectra of the sample. Reciprocally, XPS analysis was able to identify the constituent carbon-carbon, carbon-oxygen and carbon-nitrogen bonds of the functional groups in the compounds identified by THM-GC/MS. The two independently derived outputs from the THM-GC/MS and the XPS techniques mutually validated the identification of organic compounds in our geological samples. We describe in detail the improvements to: • The preparation of geological samples for analysis by XPS. • Measurements of organic material in geological samples using GC/MS. • The use of THM-GC/MS and XPS data used together to characterise low levels of organic material in geological samples.