Evaporation and sublimation of boric acid:: Application for boron purification from organic rich solutions

We report in this paper a series of experiments whose purpose is to test the long held idea of boron volatility when neutral to acidic solutions containing traces of boron are evaporated. Boron recoveries have been measured precisely by isotopic dilution and boron isotopic ratios have also been determined. Most of the evaporations have been conducted at 60-65 degreesC. It was found that no loss of boric acid occurs when c. 1 mug of B is evaporated in water, HCl, HF and acetone solutions. At the same time, we did not observe any associated B isotopic fractionation. In contrast to previous studies on B volatilisation, it was not found necessary to use mannitol to prevent B losses during the evaporation of acidic solutions. Important losses of boron were observed from solutions of methanol, ethanol and organic-rich natural solutions. In the presence of methanol and ethanol, a volatile methyl (or ethyl) borate is likely to be formed. In contrast to these studies, we show that boron is highly volatile when the dried residues of an evaporation are heated further. The sublimation of boron that then occurs can be moderated by the use of mannitol, but a slight increase of the temperature allows B volatilisation. Despite the substantial losses of B by sublimation, no B isotopic fractionation was observed at 60-65 degreesC. The property of boron to sublime was used to separate B from on organic matrix. A miniaturized sublimation apparatus, comprising a 5 ml Teflon beaker, and the associated microsublimation technique are described. The 100% boron recovery and the absence of B isotopic fractionation make this method suitable for extracting B from organic-rich samples.