An introduction to key determinative methods in clay science

This workshop will take place on Sunday 13th July: registration at 8.30-9.00, workshop at 9:00-17:00.
Without doubt, X-ray diffraction, thermal methods, infrared spectroscopy and electron microscopy can be considered as the key methods that are employed universally across research and industrial analysis of clays and clay materials. Additionally, in clay science, a multi-method approach is often the only way to advance many research questions. This workshop is designed to provide delegates with a foundational introduction to four key methods, each introduced by an expert in the field. No prior knowledge is assumed, and the workshop will strive to provide a solid foundation in the applications of each of these methods, covering the do’s and the don’ts, and the strengths and weaknesses of each, including ample opportunity for delegates to ask questions and benefit from the advice of the experts.
Sunday 13th July: registration at 8.30-9.00, workshop at 9:00-17:00.
Cost: €80 (incl VAT)
Programme
09:00-09:15 Welcome
09:15-10:45 X-ray diffraction and the identification and structure determination of clay minerals: An updated perspective
Bruno Lanson, ISTerre, CNRS, Univ. Grenoble Alpes, France
The finely divided and bidimensional character of clay minerals, and other lamellar compounds, has led to the development of specific approaches for their identification and the determination of their crystal structures using X-ray diffraction. This lecture will review the basic concepts of this identification, including practical aspects of sample preparation and data collection. It will also introduce basic concepts of X-ray diffraction profile modelling as a key tool allowing the description of lamellar structures, including disruptions of periodicity such as interstratification and stacking faults.
10:45-11:00 Break
11:00-12:30 Electron microscopy for clay science: what can be done and what to be considered
Toshihiro Kogure, Department of Earth & Planetary Science, School of Science, The University of Tokyo, Japan
Electron microscopy, with resolutions ranging from the micron to angstrom levels, is a unique and essential tool for investigating the morphology, structure, and composition of typically fine and heterogeneous clay particles. As is well known, electron microscopes are broadly classified into SEM and TEM/STEM, with the choice depending on the sample form (bulk or thin film) to be observed. The resolution of SEM for surface observation is approximately 1 nm, and selecting the appropriate accelerating voltage is crucial when examining clay minerals. TEM/STEM can provide atomic-scale structural information about clay minerals through electron diffraction and so-called high-resolution TEM (HRTEM); however, electron radiation damage must be carefully managed. This lecture will introduce various observation and analysis examples and highlight key considerations for beginners using electron microscopy in clay science.
12:30-13:30 Lunch
13:30-15:00 Thermal Analysis in Clay Science
Katja Emmerich, Faculty of Civil Engineering, Geo- and Environmental Sciences
Karlsruhe Institute of Technology, Germany
Thermal analysis was one of the first analytical methods used to characterize clay minerals and has developed ever since. Clay minerals and associated minerals and phases in soils and rocks undergo various thermal reactions (e.g. dehydration, dehydroxylation, oxidation, decomposition, recrystallisation, phase transition). Their characteristics provide information on the amount of a mineral, its size and structure even if it is turbostratic disordered like swellable clay minerals. Sensitivity is enhanced by coupled analysis of evolved gases. The lecture will provide a basic introduction to thermal analysis and thermal reactions of clay components.
15:00-15:15 Break
15:15-16:45 Infrared spectroscopic techniques for the non-invasive study of clays
Georgios Chryssikos, Institute of Theoretical & Physical Chemistry, National Hellenic Research Foundation, Greece
This lecture will introduce the application of attenuated total reflectance (ATR) in the mid-infrared and diffuse reflectance in the near infrared (NIR) for the study of clay minerals with minimum or no sample preparation. The aim is to isolate and study the spectrum of the water and hydroxyl species that decorate the internal and external surfaces of clays. Beyond mineral identification, these spectra provide intrinsic proxies for the octahedral sheet, the termination of the tetrahedral sheet, the layer charge, the contents of the interlayer etc. Tips for the proper measurement of samples in the range from mg to tons as well as efficient techniques for band separation (including practical methods for H/D exchange) will be presented.
16:45-17:00 Closing remarks / Discussion
Cost: €80 (incl VAT)
