Illite polytypes are used to elucidate the geological record of formations, such as the timing and provenance of deformations in geological structures and fluids, so the ability to characterize and identify them quantitatively is key. The purpose of the present study was to compare three X-ray powder diffraction (Q-XRPD) methods for illite polytype quantification for practical application to directly date clay-rich fault rocks and constrain the provenance of deformation-related fluids in clay-rich brittle rocks of the upper crust. The methods compared were WILDFIRE© (WF) modeling, End-member Standards Matching (STD), and Rietveld whole-pattern matching (BGMN®). Each technique was applied to a suite of synthetic mixtures of known composition as well as to a sample of natural clay gouge (i.e. the soft material between a vein wall and the solid vein). The analytical uncertainties achieved for these synthetic samples using WF modeling, STD, and Rietveld methods were ±4–5%, ±1%, and ±6%, respectively, with the caveat that the end-member clay mineral used for matching was the same mineral sample used in the test mixture. Various particle size fractions of the gouge were additionally investigated using transmission electron microscopy (TEM) to determine polytypes and laser particle size analysis to determine grain size distributions. The three analytical techniques produced similar 40Ar/39Ar authigenesis ages after unmixing, which indicated that any of the methods can be used to directly date the formation of fault-related authigenic illite. Descriptions were included for pre-calculated WF illite polytype diffractogram libraries, model endmembers were fitted to experimental data using a least-squares algorithm, and mixing spreadsheet programs were used to match end-member natural reference samples.

Radiometric dating of fault gouges has become a useful tool for regional tectonics studies and for exploring and understanding fault and earthquake processes. Methods to define the absolute age of faults achieved a solid scientific foundation almost 25 years ago when the development and application of illite age analysis for investigating sedimentary burial and thermal histories found a new potential application – defining the age of fold-and-thrust development. Since then, the methods have benefitted from further development and incorporation of the 40Ar/39Ar micro-encapsulation method and quantitative clay mineral evaluation to distinguish polytypes (Wildfire). These refinements to the methods have improved their application in fold-and-thrust terrains and have opened up applications in normal and strike-slip fault environments. Another important development is the use of absolute dating methods in retrograde clay gouges in which clays in a fault develop from igneous or metamorphic wall rocks that contain no clays. In addition, the method has also been shown to be useful at dating folds in fold-and-thrust belts. We think the method is now an established part of the geological toolkit, look forward to future fault structural and tectonic studies that incorporate fault ages and hope that researchers continue to probe and discover ways that the method can assist fault process studies, including earthquake fault studies.