Combining thermal hydrolysis and methylation-gas chromatography/mass spectrometry with X-ray photoelectron spectroscopy to characterise complex organic assemblages in geological material

• Main Authors: Graham Purvis, Naoko Sano, Cees van der Land, Anders Barlow, Elisa Lopez-Capel, Peter Cumpson, James Hood, Jake Sheriff, Neil Gray
• Format: Article
• Language: English
• Published: Elsevier 2019-01-01
• Series: MethodsX
• Online Access: http://www.sciencedirect.com/science/article/pii/S2215016119302997

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. Method name: Combining thermal hydrolysis and methylation-gas chromatography/mass spectrometry with X-ray photoelectron spectroscopy, Keywords: XPS, GC/MS, Pyrolysis, TMAH, THM, Geological material, Organic geochemistry, Analysis