Estimating Mean Crystallite Size of Magnetite using Multivariate Calibration and Powder X-ray Diffraction Analysis

Abstract

Powder X-ray diffractograms for 29 samples of magnetite, acquired using a conventional diffractometer, were used to build PLS calibration-based methods and variable selection to estimate mean crystallite size of magnetite directly from powder X-ray diffractograms. The best IPLS model correspond to the Bragg reflections at 35.4° (h k l = 3 1 1), 43.0° (h k l = 4 0 0), 53.6° (h k l = 4 2 2), and 57.0° (h k l = 5 1 1) in 2theta. The best model was a GA-PLS which produced a model with RMSEP of 0.9 nm, and a correlation coefficient of 0.9976 between mean crystallite sizes calculated using Williamson-Hall approach and the ones predicted by GA-PLS method. These results indicate that magnetite mean crystallite sizes can be predicted directly from Powder X-Ray Diffraction and multivariate calibration using PLS variable selection approach.