Artifacts from manganese reduction in rock samples prepared by focused ion beam (FIB) slicing for X-ray microspectroscopy

Macholdt, Dorothea S.; Förster, Jan-David; Müller, Maren; Weber, Bettina; Kappl, Michael; Kilcoyne, A. L. David; Weigand, Markus; Leitner, Jan; Jochum, Klaus Peter; Pöhlker, Christopher; Andreae, Meinrat O.

doi:https://doi.org/10.5194/gi-8-97-2019

Articles | Volume 8, issue 1

https://doi.org/10.5194/gi-8-97-2019

© Author(s) 2019. This work is distributed under
the Creative Commons Attribution 4.0 License.

https://doi.org/10.5194/gi-8-97-2019

© Author(s) 2019. This work is distributed under
the Creative Commons Attribution 4.0 License.

Articles | Volume 8, issue 1

Research article

|

14 Mar 2019

Research article |

| 14 Mar 2019

Artifacts from manganese reduction in rock samples prepared by focused ion beam (FIB) slicing for X-ray microspectroscopy

Dorothea S. Macholdt, Jan-David Förster, Maren Müller, Bettina Weber, Michael Kappl, A. L. David Kilcoyne, Markus Weigand, Jan Leitner, Klaus Peter Jochum, Christopher Pöhlker, and Meinrat O. Andreae

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Final revised paper (published on 14 Mar 2019)
Preprint (discussion started on 29 Jun 2018)

Interactive discussion

Status: closed

AC: Author comment | RC: Referee comment | SC: Short comment | EC: Editor comment

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RC1: 'review of gi-2018-20', Adam Hitchcock, 02 Jul 2018
- AC1: 'Response to referee Adam Hitchcock', Meinrat O. Andreae, 21 Jan 2019
RC2: 'Reviewer’s comments on manuscript titled “Artifacts from manganese reduction in rock samples prepared by focused ion beam (FIB) slicing for X-ray microspectroscopic analysis” by Macholdt el al.', Anonymous Referee #2, 15 Oct 2018
- AC2: 'Response to referee #2', Meinrat O. Andreae, 21 Jan 2019

Post-review adjustments

AA: Author's adjustment | EA: Editor approval

AA by Jan-David Förster on behalf of the Authors (06 Mar 2019) Author's adjustment Manuscript

EA: Adjustments approved (08 Mar 2019) by Maria Genzer

Short summary

Focused ion beam (FIB) slicing is a widely used technique to prepare ultrathin slices for the microanalysis of geological and environmental samples. During our investigations of the manganese oxidation states in rock varnish slices, we found an FIB-related reduction of manganese(IV) to manganese(II) at the samples’ surfaces. This study characterizes the observed reduction artifacts and emphasizes that caution is needed in the analysis of transition metal oxidation states upon FIB preparation.