Quantitative determination of the oxidation state of iron in biotite using X-ray photoelectron spectroscopy: I. Calibration

Details Quantitative determination of the oxidation state of iron in biotite using X-ray photoelectron spectroscopy: I. Calibration Quantitative determination of the oxidation state of iron in biotite using X-ray photoelectron spectroscopy: I. Calibration

Nov 1997

adsabs.harvard.edu/cgi-bin/nph-data_query?bibcode=1997gecoa..61.4519r&link_type=abstract

Geochimica et Cosmochimica Acta, vol. 61, Issue 21, pp.4519-4530

Computer Science

3

Scientific paper

X-ray photoelectron spectroscopy (XPS) analyses of were calibrated with nine single crystals of biotite of known content. Peak shape parameters for the component Fe 2+ and Fe 3+ Fe 3p peaks were obtained by a constrained least squares fitting method that minimized the difference between determined by XPS and wet chemistry/electron microprobe (WCEM) analyses. Fe 2+ and Fe 3+ peak separation was estimated from the separation of minima in the second derivative of Fe 3p spectra. The single set of derived peak parameters yielded a good linear correlation ( r = 0.87) between XPS and WCEM values over the sample range of 2-20% . Target transformation factor analysis of a time series of spectra for a sample displaying progressive oxidation during XPS analysis resulted in Fe 2+ and Fe 3+ component peak shapes largely consistent with the constrained least squares fitting method. Peak asymmetry for the Fe 3+ component was the only parameter that differed for the two methods. Beam damage, which appeared to be restricted to three single crystals with low Fe, low , and high , caused increases in that were proportional to the duration of sample exposure.

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