Multi-Technique Analytical Approach to Quantitative Analysis of Spodumene

The aim of this study was to establish the capability of X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) methods to determine different spodumene forms (α-, β- and γ-spodumene) occurring during heat treatment of lithium spodumene. It is essential to correctly identify and quantify the presence of different forms of spodumene after heat treatment to ensure optimum lithium extraction. A sample from the Haapaluoma lithium-pegmatite (western Finland) was used for this study. An experimental programme was initiated to model the progression of the mineral transformation at different stages through heat treatment. The specimen was broken down and split into five portions. One of the splits was analysed unheated with XRD, FTIR, XRF and ICP; the other four splits were analysed with XRD and FTIR after heat treatment at different temperatures from 850 to 1100 °C. In this study, we show that both laboratory-based XRD and portable FTIR methods are effective in identifying and quantifying α-, β- and γ-spodumene as well as impurities. The accuracy of the quantification of the minerals with XRD was established by using a mass balance calculation and was compared with the actual chemistry of the sample measured with ICP analysis. Fully quantitative XRD analysis of heat-treated spodumene is considered a challenge due to peak overlaps between the β-, and γ-spodumene forms, particularly when gangue minerals and amorphous content are present. The novelty of this study consists of the use of the XRD technique complemented by the Rietveld method to fully quantify the different forms of spodumene from one another: α-, β- and γ-spodumene, along with the gangue minerals and the amorphous content. It is also shown that reproducible systematic changes occur in the FTIR spectra that track the spodumene transformation during heat treatment. With more samples and cross-validation between the XRD results, the FTIR methodology could be developed further to provide semi-quantitative information on the different spodumene forms in the future. This would permit the use of a fast, cost-effective and portable technique for quality control of the spodumene forms, which would open opportunities across the Li value chain