In situ oxygen isotope analysis of silicate minerals has been validated by interlaboratory calibration using an excimer laser (KrF fill gas, 248 nm), F 2 gas fluorinating reagent, and O 2 gas as mass spectrometer analyte. A value of δ 18O SMOW = 5.82%. (±0.03, 4 analyses) was obtained for almandine UWG-2 compared to a recommended value of 5.8%0 (Valley et al., 1995). The interhalogen BrF5 was tested by comparing in situ analyses made alternatively with either BrF 5 or F 2 gas on crystals of almandine, epidote, forsterite, tourmaline, and zircon. Results for different pressures of BrF 5 (20 to 40 torr) in the reaction chamber show that δ 18O values decrease by 1 permil for an increase of 10 torr in BrF 5 pressure. In strong contrast, δ 18O values measured with purified F 2 gas are precise and accurate over a range of from 15 to 150 torr F 2 gas pressure. Use of F 2 gives higher yields of O 2 than with BrF 5. Values of δ 17O and δ 18O measured in situ on a variety of silicates all plot on the terrestrial mass fractionation line, provided that NF 3 contamination is eliminated from the O 2 gas analyte.
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