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:10.5194/gi-8-97-2019

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

Journal Article · Thu Mar 14 00:00:00 EDT 2019 · Geoscientific Instrumentation, Methods and Data Systems (Online)

DOI:https://doi.org/10.5194/gi-8-97-2019· OSTI ID:1542389

Macholdt, Dorothea S. ^[1];

^[1]; Müller, Maren ^[1];

^[1]; Kappl, Michael ^[1];

^[2]; Weigand, Markus ^[3]; Leitner, Jan ^[1]; Jochum, Klaus Peter ^[1];

^[1];

^[4]

Max Planck Society, Mainz (Germany)
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Advanced Light Source (ALS)
Max Planck Society, Stuttgart (Germany)
Max Planck Society, Mainz (Germany); King Saud Univ., Riyadh (Saudi Arabia)

The spatial distribution oftransition metal valence states is of broad interest in the microanalysis ofgeological and environmental samples. An example is rock varnish, a naturalmanganese (Mn)-rich rock coating, whose genesis mechanism remains a subjectof scientific debate. We conducted scanning transmission X-ray microscopywith near-edge X-ray absorption fine-structure spectroscopy (STXM-NEXAFS)measurements of the abundance and spatial distribution of different Mnoxidation states within the nano- to micrometer thick varnish crusts. Suchmicroanalytical measurements of thin and hard rock crusts require samplepreparation with minimal contamination risk. Focused ion beam (FIB) slicingwas used to obtain ~100–1000 nm thin wedge-shaped slices of thesamples for STXM, using standard parameters. Yet, while this preparationis suitable for investigating element distributions and structures in rocksamples, we observed artifactual modifications of the Mn oxidation states atthe surfaces of the FIB slices. Our results imply that the preparationcauses a reduction of Mn⁴⁺ to Mn²⁺. We draw attention tothis issue, since FIB slicing, scanning electron microscopy (SEM) imaging,and other preparation and visualization techniques operating in thekilo-electron-volt range are well-established in geosciences, but researchersare often unaware of the potential for the reduction of Mn and possibly otherelements in the samples.

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Research Organization:: Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)

Sponsoring Organization:: USDOE Office of Science (SC)

Grant/Contract Number:: AC02-05CH11231

OSTI ID:: 1542389

Journal Information:: Geoscientific Instrumentation, Methods and Data Systems (Online), Vol. 8, Issue 1; ISSN 2193-0864

Publisher:: European Geosciences UnionCopyright Statement

Country of Publication:: United States

Language:: English

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