Evaluating intragrain gradients in the δ34S of pyrite using a 7f-GEO SIMS

Recent work has highlighted the need to distinguish the contribution(s) of different populations of petrographically and isotopically distinct pyrites to interpret bulk δ 34 S pyr sedimentary values. To address this, we developed a method for micron-scale isotopic characterization of petrographically diverse sedimentary pyrites within a multimineralic matrix using ion imaging with a 7f-GEO secondary ion mass spectrometer (SIMS), aiming to rapidly and precisely analyze the isotopic composition of pyrites over relatively wide fields of view. By using primary beam currents in the range 1–11 pA and raster widths of 15–80 μm, precise data can reproducibly be acquired over a relatively large field of view, with negligible penetration into underlying mineral phases. Instrumental artifacts are a factor in cases where phosphate or halide minerals are intergrown with pyrite or where surface topographic variation is significant. However, a 1 pA beam method with smaller rasters can eliminate these artifacts if those situations cannot be avoided. The precision (1σ) on individual regions of interest (ROI) is <1‰ at all beam currents tested, provided the total accumulated number of measured 34 S counts exceeds one million. Isotopic gradients within grains can be resolved across areas as small as 20 μm 2 (5 μm diameter) and features as small as 1.5 μm 2 (∼1.4 μm diameter) can be resolved with a precision of 1.5‰ (1σ). The achievable sub-micron spatial resolution with a 1pA primary current allowed for data to be extracted from specifically desired regions within pyrite (e.g., distinguishing primary/early diagenetic pyrite from late-stage components), with minimal contamination from neighboring minerals. • Novel method for high-precision micron-scale isotopic analysis of pyrite by SIMS ion imaging. • Ion imaging allows for a posteriori identification of regions of interest that can be characterized in parallel by SEM/EDS. • The isotopic composition of complex, intergrown pyrite textures can be spatially resolved. • Artifacts associated with adjacent minerals, epoxy/void space, and surface topography are assessed and minimized.

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Publication Details

Journal
Chemical Geology
Published
2024-08-15
DOI
https://doi.org/10.1016/j.chemgeo.2024.122335
Primary Topic
Ion-surface interactions and analysis
Type
article
Field-Weighted Citation Impact
0.00

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article

Evaluating intragrain gradients in the δ34S of pyrite using a 7f-GEO SIMS

Jennifer Houghton, David A. Fike, Clive Jones
Chemical Geology
Ion-surface interactions and analysis
article

Evaluating intragrain gradients in the δ34S of pyrite using a 7f-GEO SIMS

Jennifer Houghton, David A. Fike, Clive Jones
article en

Abstract

Recent work has highlighted the need to distinguish the contribution(s) of different populations of petrographically and isotopically distinct pyrites to interpret bulk δ 34 S pyr sedimentary values. To address this, we developed a method for micron-scale isotopic characterization of petrographically diverse sedimentary pyrites within a multimineralic matrix using ion imaging with a 7f-GEO secondary ion mass spectrometer (SIMS), aiming to rapidly and precisely analyze the isotopic composition of pyrites over relatively wide fields of view. By using primary beam currents in the range 1–11 pA and raster widths of 15–80 μm, precise data can reproducibly be acquired over a relatively large field of view, with negligible penetration into underlying mineral phases. Instrumental artifacts are a factor in cases where phosphate or halide minerals are intergrown with pyrite or where surface topographic variation is significant. However, a 1 pA beam method with smaller rasters can eliminate these artifacts if those situations cannot be avoided. The precision (1σ) on individual regions of interest (ROI) is <1‰ at all beam currents tested, provided the total accumulated number of measured 34 S counts exceeds one million. Isotopic gradients within grains can be resolved across areas as small as 20 μm 2 (5 μm diameter) and features as small as 1.5 μm 2 (∼1.4 μm diameter) can be resolved with a precision of 1.5‰ (1σ). The achievable sub-micron spatial resolution with a 1pA primary current allowed for data to be extracted from specifically desired regions within pyrite (e.g., distinguishing primary/early diagenetic pyrite from late-stage components), with minimal contamination from neighboring minerals. • Novel method for high-precision micron-scale isotopic analysis of pyrite by SIMS ion imaging. • Ion imaging allows for a posteriori identification of regions of interest that can be characterized in parallel by SEM/EDS. • The isotopic composition of complex, intergrown pyrite textures can be spatially resolved. • Artifacts associated with adjacent minerals, epoxy/void space, and surface topography are assessed and minimized.

Chemical GeologyVol. 668
Planetary Science Institute (US), Washington University in St. Louis (US)
National Science Foundation, Biological and Environmental Research
Openalex Percentile: Top 86%
Ion-surface interactions and analysis
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