This paper describes a new methodology for the analysis of fluorine in glasses and glazes by wavelength-dispersive x-ray fluorescence (WD-XRF) spectrometry. The methodology was developed in order to have a rapid and reliable method, that could be used as a control method. Fluorine-containing glasses and glazes are of interest for a broad range of components, and it has been shown that the introduction of fluoride ions into phosphate glasses has an effect on the structural and optical properties of the glass, so it is necessary to know the fluorine content in this type of glasses in order to predict these optical properties. Besides, in the ceramic industry fluorine is used as an pacifying agent. There are different methodologies for determining the fluorine content in this kind of sample, based on digestion of the sample; the methods exhibit serious interferences and/or problems of loss of the analyte, apart from being tedious and time consuming. In order to develop the methodology, the different process stages, ranging from sample preparation to measurement conditions were optimized; the method was validated by analysing reference materials with known fluorine content and samples that had been analysed by an independent method (potentiometry). The fine-tuned methodology permits the analysis of fluorine concentration, with samples prepared in the form of beads. The method allows the determination of fluorine in a relatively short time in any glasses and glazes and presents low uncertainties with a quantification limit of 0.1% (by weight).
展开▼