Fluorine loss determination in bioactive glasses by laser‐induced breakdown spectroscopy (LIBS)

Abstract Fluoride‐containing bioactive glasses and glass‐ceramics in the SiO ₂ ‐P ₂ O ₅ ‐CaO‐CaF ₂ system are of great interest for dental applications, where the precipitation of fluorapatite supports tooth remineralization. Fluorine quantification in those glasses is key to estimate thermal properties and crystallization tendency. This work presents a study on fluorine determination by laser induced breakdown spectroscopy (LIBS) in four melt‐derived glass powders with varying P ₂ O ₅ concentrations. LIBS enables fluorine quantification with a reduced analysis time, minimal to no sample preparation, and high spatial resolution. The fluorine calibration curve was obtained from CaF ₂ and SiO ₂ mixtures as reference samples, and the fluorine loss upon glass melting has been determined as a function of P ₂ O ₅ content. The P ₂ O ₅ ‐free glass shows the lowest fluorine loss (13%), with HF volatilization likely being responsible for the loss. By contrast, the glass with the highest P ₂ O ₅ content (11.33 wt%) exhibits the largest fluorine loss (55%), owing to additional mechanisms involving the volatilization of phosphorus species like POF ₃ .