Tropical soils characterization at low cost and time using portable X-ray fluorescence spectrometer (PXRF): effects of different sample preparation methods

Abstract

Portable X-ray fluorescence spectrometer (pXRF) has been recently adopted by the Soil Science community for uses in both field and laboratory, obtaining the total content of several chemical elements in a few seconds. Sulfuric acid digestion is an expensive and time-consuming laboratory analysis that provides contents of Fe2 O3 , Al2 O3 , SiO2 , TiO2 and P2 O5 , important for soil studies. Due to few pXRF studies in tropical soils, this work aimed to compare contents of Fe2 O3 , Al2 O3 , SiO2 , TiO2 and P2 O5 obtained by pXRF with sulfuric acid digestion results, and to evaluate the effects of varying forms of preparing soil samples and scanning with pXRF on the resulting values in Brazilian soils. Soils were scanned in five conditions in-field (in situ) and in laboratory, evaluating varying sample preparation methods, particle sizes and soil moisture. Four pXRF scanning operational modes were tested. Linear regressions were adjusted between results of pXRF and sulfuric acid digestion. Equations were validated with an independent set of samples. Statistical analyses compared the methods of preparing the samples. Adequate linear models reached R2 of 0.99 and 0.89 for Fe2 O3 and TiO2 , respectively. Validation promoted R2 greater than 0.97 and RMSE and ME close to zero for both oxides. Statistical differences of pXRF results were found among the methods of preparing samples. pXRF spectrometer has great potential to obtain Fe2 O3 and TiO2 content rapidly and economically with high correspondence with laboratory results of sulfuric acid digestion analysis. Varying methods of preparing the samples promote differences in the results of pXRF.