Journal
INDUSTRIAL & ENGINEERING CHEMISTRY RESEARCH
Volume 56, Issue 47, Pages 13983-13996Publisher
AMER CHEMICAL SOC
DOI: 10.1021/acs.iecr.7b03316
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- Electrical Power Research Institute [EP-P43257/C18781]
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Temperature-dependent Raman studies of the aqueous speciation of boric acid and sodium borate have been carried out at 25 and 80 degrees C. Normalized solvent-corrected reduced isotropic Raman spectra were obtained from perpendicular and parallel polarization measurements using perchlorate anion, [ClO4](+), as an internal standard. The intensity variations of these bands with concentration and temperature provided strong evidence that these arise from boric acid B(OH)(3,) borate [B(OH)(4)], and the polyborate species [B3O3(OH)(4)], [B4O5(OH)(4)](2-), and [B5O6(OH)(4)](-). A very weak high frequency shoulder on the borate band may indicate the presence of the diborate species [B2O(OH)(5)](-). Temperature- and concentration-independent quantitative Raman molar scattering coefficients (S) for the symmetric vibrational bands of boron-containing species were calculated, consistent with the mixed solvent electrolyte model reported by Wang et al. (Pure Appl. Chem. 2013, 85, 2117-2144) up to approximately 100 degrees C. The band assignments and scattering parameters reported here provide a framework for using reduced isotropic Raman spectroscopy as a research tool for measuring quantitative speciation of boric acid/polyborate solutions under conditions relevant to nuclear reactor primary coolant circuits and spent fuel bays, among other applications.
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