Clay Sample Preparation Treatment for XRD Analysis

"Adequate characterisation of clays is becoming increasingly important as operating mines move into areas of more complex ores. The processing therefore needs better mineralogical characterisation to identify problematic ores for better planning before issues arise. While a number of instrumental mineral characterisation methods are available, X-ray Diffraction (XRD) is widely recognised as perhaps the best technique for the identification and quantification of minerals, particularly clays. When an appropriate sequential and systematic sample preparation and treatment protocol is employed with instrumental XRD analysis individual clays can be uniquely identified, and the proportions of interstratified clays can also be quantified. The effect of sample preparation on the XRD analysis and identification of clays was investigated in this study. The results showed that sample preparation protocol is indeed critical to accurately analysis and characterisation of clays. For example, both dry grinding and micronizing affected the degree of crystallinity of kaolinite leading to the formation of reactive surfaces or changes in the physicochemical behavior. It was also found that the apparent degree of preferred orientation in platy minerals correlates directly with the amount of force/pressure applied during the preparation of backfilled powder samples. This work showed that manual preparation can produce highly variable peak intensities especially with minerals that show any preferred orientation. KEYWORDS Clay; XRD; kaolinite INTRODUCTION Clays are important in our life and they have numerous applications in modern world from cosmetics to environmental remediation. Therefore, clays have been extensively investigated for many years. Adequate characterisation of clays is becoming increasingly important as the mineral processing industry faces more complex mineralogy with the need for better mineralogical characterisation to identify problematic ores and plan accordingly. In most studies, X-ray diffraction (XRD) method has shown the unique capability to characterise mineralogy, especially for the fine grained size materials. The XRD technique is particularly diagnostic for clays. It is known that under ideal conditions, the peak intensities of an XRD diffractogram are proportional to the concentrations of individual minerals present in the sample. Hence, the qualitative mineralogical data obtained from XRD can be quantified, using either the internal or external standard methods. However, it is also known that clays are particularly sensitive to the influences of sample preparation method due to their physical characteristics (e.g. fine grain size, morphology, relative physical softness, crystallinity, thermal sensitivity) that could be destroyed by inappropriate preparation prior to the analysis. Thermal and mechanical treatment and grinding of clays can change their crystalline structure, and consequently, their characterisation results by XRD analysis. The behaviour of clays in grinding has been widely studied, especially for kaolinite (Miller and Oulton, 1970, Milocevic et al., 1992, Tomasevic-Canovic et al., 1992). With prolonged grinding time, the crystallinity of the clays can decrease (Filipovic-Petrovic et al., 2002). It has been shown that grinding may gradually cause the loss of hydroxyl ions of kaolinite (Gonzalez Garcia et al., 1991)."