Rationale: Sulfate precipitates are often contaminated with nitrates and organic materials (OM), which reduce the precision and accuracy of measurements of δ18 O and Δ17 O values in the sulfate. Although nitrates can be effectively removed using diethylenetriaminepentaacetic acid solution, removing OM from the precipitates is often difficult. One effective approach is to heat powdered precipitates to high temperatures. In this study, the effect of this procedure on the δ18 O and Δ17 O values of BaSO4 precipitate was fully examined.
Methods: OM-contaminated BaSO4 precipitates and 18 O- and 17 O-labeled purified BaSO4 precipitates were loaded into alumina and gold crucibles and heated at 450 °C, 600 °C and 800 °C for 2 h. The nitrogen and carbon contents in the initial and the final BaSO4 were measured using an elemental analyzer. The values of δ18 O and Δ17 O were measured using a temperature conversion/elemental analyzer coupled with an isotope ratio mass spectrometer, and a CO2 laser system coupled with an isotopic ratio mass spectrometer.
Results: OM was effectively (88 ± 17%) removed from the BaSO4 precipitates by this treatment, and heating at 800 °C had the highest removal efficiency (98%). The differences in δ18 O and Δ17 O values between the final and initial BaSO4 precipitates was -0.6‰ to 0.3‰ (average of -0.1‰) and -0.24‰ to 0.10‰ (average of -0.02‰), respectively. Significant positive relationships between the δ18 O and Δ17 O values of the initial BaSO4 precipitate and those of the high-T-treated aliquots were found, with slopes having mean values of 0.96 ± 0.06 and 1.04 ± 0.01, respectively.
Conclusions: The result demonstrates high removal efficiency for OM in BaSO4 precipitates and no significant differences in the oxygen isotopic compositions between high-T treated BaSO4 and initial BaSO4 . This study indicates that the modified high-T treatment (800 °C, 2 h) is an effective method for purifying BaSO4 precipitated from geological and environmental samples with a high OM content for δ18 O and Δ17 O measurements. Copyright © 2016 John Wiley & Sons, Ltd.
Copyright © 2016 John Wiley & Sons, Ltd.