Validation of a method for the determination of boron in ceramic materials by X-ray fluorescence spectrometry

A method is proposed for boron determination in ceramic materials, boracic raw materials and ceramics frits of different compositions by wavelength dispersive X-ray fluorescence technique. The instrumental conditions were studied and the sample preparation procedures were optimized. The reference method used was the potentiometric titration of mannitol–boric complex acid and the technique was optimized for the determination of B2O3 in each of the materials used. The samples for XRF determination were obtained as pellets and as glass discs. For the pellets different binders were studied, such as mannitol and cellullose for the samples of raw materials, and polyvinylpirrolidone and methyl cellullose (PVP+MC) for the ceramic frits. Samples were obtained in the form of glass discs using lithium tetraborate and a barium-lead glass (BaPbG) as materials to melt, dilute and homogenize the samples, and increase the analytical signal. A series of calibration curves were obtained and the instrumental variables were optimized. The results obtained with the XRF method were compared with the reference method for several unknown samples. The results obtained with both techniques showed relative errors from 0.7 to 3.2% for B2O3 content ranging between 40.8 and 6.3%, respectively.