Implementing Light Elements Detection and Quantification in Aluminosilicate Materials Using a Low-Z Total-Reflection X-ray Fluorescence Spectrometer

Total-reflection X-ray fluorescence (TXRF) is a well-established atomic spectroscopy technique used for the elemental characterization of different kinds of matrixes in several fields. Previous works demonstrated its applicability for the elemental quantification of aluminosilicates and, in particular, clays. However, one of the limits of the previously developed methods was the detection and quantification of light elements, in particular for those elements with an atomic number (Z) below 13 (Al). In the present work a new TXRF-based analytical method for the quantification of light elements in aluminosilicate materials is described, using an in-house built Low-Z TXRF spectrometer equipped with a Cr source, a multilayer monochromator, an SDD detector equipped with an ultrathin Si3N4 window and a vacuum chamber. Samples were prepared as simple slurries (dispersing 50 mg of powder into 2.5 mL of 1%-Triton X-100 water solution and adding Ag as internal standard) and 10 mu L were deposited onto a quartz carrier and dried before the analysis. Light elements such as F, Na and Mg were quantified with a limit of detection of 682, 260 and 133 mg/kg, respectively. Carbon and oxygen could also be detected. The new method allowed a complete analysis of major elements in aluminosilicates from F to Fe. The method showed a good accuracy in the range of 80-120% and the results agreed with the data obtained with a commercial TXRF spectrometer (for elements >13) and WDXRF, employed as reference methods. Despite a lower precision in respect to WDXRF, in some samples the quantification of F was possible only by using the Low-Z TXRF spectrometer. Finally, the method demonstrated to be suitable for the analysis of aluminosilicates, in particular when low amounts of sample (few milligrams) are available.