Quantification of boron in aluminoborosilicate glasses using Raman and 11B NMR

• Published in: Journal of non-crystalline solids 2019-05, Vol.511, p.50-61
• Main Authors: Jolivet, Valentin, Jossé, Léna, Rivoal, Marion, Paris, Michael, Morizet, Yann, Carole, La, Suzuki-Muresan, Tomo
• Format: Article
• Language: English
• Subjects: 11B Nuclear magnetic resonance; Borosilicate glasses; Chemical Sciences; Environment and Society; Environmental Sciences; Material chemistry; or physical chemistry; Radiochemistry; Raman spectroscopy; Theoretical and
• ISSN: 0022-3093; 1873-4812
• DOI: 10.1016/j.jnoncrysol.2018.12.038

Bulk methods and 11B Nuclear Magnetic Resonance were used to propose a calibration curve to determine the total B2O3 and the boron speciation using the non-destructive and the non-quantitative nature of Raman spectroscopy. The calibration was established from the analyses of 21 aluminoborosilicate glasses synthesised at 1 atm. and 1150 °C and an additional standard aluminoborosilicate glass. The studied glasses have composition in the Na2O-CaO-Al2O3-SiO2-B2O3 system with total B2O3 from 4.7 to 46.6 mol%. Raman spectra exhibit signatures in the 800–1200 and 1200–1600 cm−1 region corresponding to the symmetric stretches of silicate (HF) and borate networks (BO), respectively. The integrated area ratio (AB-O−/AHF) is correlated to the total mol.% B2O3. The mol.% B2O3 data are reproduced within 15% from the Raman spectra. Boron speciation from 11B NMR is correlated to the AB-O−/AHF determined by Raman; however, the mol.% BO4 appears also dependent on the Al2O3 content. We derived a multiple linear regression estimating the mol.% BO4 as a function of AB-O−/AHF and mol.% Al2O3. Results are valid for the investigated glasses and additional work is needed to better constrain the speciation model. •Boron concentration and speciation is determined using Raman spectroscopy.•Raman calibration established using NMR and bulk methods.•Boron speciation is dependent on both Na2O/B2O3 ratio and Al2O3 content.