Atom probe tomography for isotopic analysis: development of the 34S/32S system in sulfides

Published

November 12, 2021

Author(s)

Phillip Gopon, James Douglas, Frederick Meisenkothen, Jaspreet Singh, Andrew London, Michael Moody

Abstract

Using a combination of simulated data and pyrite isotopic reference materials, we have refined a methodology to obtain quantitative δ34S measurements from atom probe tomography (APT) datasets. This study builds on previous attempts to characterize relative 34S/32S ratios in gold containing pyrite using APT. We have also improved our understanding of the artefacts inherent in laser pulsed APT of insulators. Specifically, we find the probability of multi-hit detection events increases during the APT experiment, which can have a detrimental effect on the accuracy of the analysis. We demonstrate the use of standardized corrected time-of-flight single-hit data for our isotopic analysis. Additionally, we identify issues with the standard methods of extracting background corrected counts from APT mass spectra. These lead to inaccurate and inconsistent isotopic analyses due to human variability in peak ranging and issues with background correction algorithms. In this study, we use the corrected time-of-flight single-hit data, an adaptive peak fitting algorithm, and an improved deconvolution algorithm to extract 34S/32S ratios from the S2+ peaks. By analyzing against a standard material, acquired under similar conditions, we have extracted δ34S values to within ± 5 ‰ (1 ‰ = 1 part per thousand) of the published values of our standards.

Citation

Microscopy and Microanalysis

Pub Type

Journals

Download Paper

https://doi.org/10.1017/S1431927621013568

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Keywords

atom probe, mass spectrometry, isotopic analysis, sulfur, peak fitting, geology

Citation

Gopon, P. , Douglas, J. , Meisenkothen, F. , Singh, J. , London, A. and Moody, M. (2021), Atom probe tomography for isotopic analysis: development of the 34S/32S system in sulfides, Microscopy and Microanalysis, [online], https://doi.org/10.1017/S1431927621013568, https://tsapps.nist.gov/publication/get_pdf.cfm?pub_id=932216 (Accessed October 25, 2025)