Laser-induced breakdown spectroscopy (LIBS) and partial least squares regression (PLSR) have been applied to perform quantitative measurements of a multiple-species parameter known as loss on ignition (LOI), in a combined set of run-of-mine (ROM) iron ore samples originating from five different iron ore deposits. Global calibration models based on 65 samples and their duplicates from all the deposits with LOI ranging from 0.5 to 10 wt% are shown to be successful for prediction of LOI content in pressed pellets as well as bulk ore samples. A global independent dataset comprising a further 60 samples was used to validate the model resulting in the best validation <i>R</i><sup>2</sup> of 0.87 and root mean square error of prediction (RMSEP) of 1.1 wt% for bulk samples. A validation <i>R</i><sup>2</sup> of 0.90 and an RMSEP of 1.0 wt% were demonstrated for pressed pellets. Data preprocessing is shown to improve the quality of the analysis. Spectra normalization options, automatic outlier removal and automatic continuum background correction, which were used to improve the performance of the PLSR method, are discussed in detail.
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