Detection of Interlayered Illite/Smectite Clay Minerals with XRD, SEM Analyses and Reflectance Spectroscopy

Accurate determination of clay minerals can be challenging due to the natural occurrence of interlayered phases, i.e., layers of different clay species such as illite and smectite. The overlap of peaks of the constituent minerals (e.g., illite and smectite), and the similarity of diffraction patterns when not treated with ethylene glycol, hampers identification, especially when the clay content is low. We investigated the occurrence of interlayered illite/smectite in a rock sample from Rodalquilar, Spain, using X-ray diffraction, scanning electron microscopy and reflectance spectroscopy in the short-wave infrared wavelength range. For the first time, a precise determination of interlayered I/S conducted on the extracted clay fraction treated with ethylene glycol using such different approaches was provided. X-ray diffraction results demonstrated the presence of an I/S peak at around 8.4 degrees in the untreated fraction coupled with a peak splitting at 6.7 degrees and 9.4 degrees 2 theta when solvated with ethylene glycol. While spectroscopy indicated the occurrence of interlayered structures as a mixture of the two constituent minerals, the results of X-ray analysis showed that the interlayered clay consisted of two discrete phases (illite and smectite). The two discrete phases were observed in both the whole rock analysis and in the extracted clay fraction. This study shows that X-ray diffraction and validation with a scanning electron microscope is a mandatory, integrating tool for detecting interlayered phases since reflectance spectroscopy alone cannot be used to differentiate between interlayered clay minerals and non-interlayered mixtures. This work highlights the limits and advantages of three sensors (X-ray diffraction, scanning electron microscopy and reflectance spectroscopy) to investigate clay mixtures and interlayering, representing a significant contribution to confidence in the interpretation of interlayered clays, this being essential in mineral exploration and prospecting.