Related Experiment Video
Updated: Mar 24, 2026

Preparation of Authigenic Pyrite from Methane-bearing Sediments for In Situ Sulfur Isotope Analysis Using SIMS
Published on: August 31, 2017
Improved analysis of micro- and nanomole-scale sulfur multi-isotope compositions by gas source isotope ratio mass
David Au Yang1,2, Guillaume Landais1, Nelly Assayag1
1Laboratoire de Géochimie des Isotopes Stables, Institut de Physique du Globe de Paris, Université Paris Diderot, CNRS UMR 7154, Sorbonne Paris-Cité, 1 rue de Jussieu, 75005, Paris, France.
Rationale:
Multiple sulfur isotope compositions are usually measured on relatively large samples (in the range of micromoles); however, sometimes only small amounts are available and thus it is necessary to analyze small (sub-micromole) samples. We report an improved method to measure multiple sulfur isotope compositions: δ(33) S, δ(34) S and δ(36) S values on the SF6 molecule (m/z 127, 128, 129, 131) for quantities down to 0.1 micromole, and δ(33) S and δ(34) S values for quantities down to 20 nanomoles.
Methods:
Multiple sulfur isotope analyses including fluorination and purification of two international Ag2 S standards, IAEA-S1 and IAEA-S3, were carried out at various low concentrations on a dual-inlet isotope ratio mass spectrometer using a microvolume and modified resistor capacities.
Results:
The analyses yielded a narrow range of δ(34) S values vs CDT (the international standard), with an overall standard deviation of ±0.2 ‰, which was within the range of certified values. This demonstrates the feasibility of determining both Δ(33) S and Δ(36) S values on the sub-micromole scale, and Δ(33) S values on the nanomole scale with similar accuracy to conventional dual-inlet analyses.
Conclusions:
The analysis of the three S-isotope ratios on the SF6 molecule using the so-called conventional fluorination method and dual-inlet ion ratio mass spectrometry is reliable for sample sizes down to ~20 nanomoles. Despite being close to the theoretical limits for maintaining the viscous flow regime of gas in the capillary, errors were not limited by counting statistics, but probably relate to sample gas purification. Copyright © 2016 John Wiley & Sons, Ltd.
More Related Videos
12:47Workflow Based on the Combination of Isotopic Tracer Experiments to Investigate Microbial Metabolism of Multiple Nutrient Sources
Published on: January 22, 2018
08:37Measurement of H2S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection
Published on: December 10, 2015
Related Concept Videos
Mass Spectrometry: Isotope Effect
Mass Spectrometry: Complex Analysis
GC–MS is a powerful hyphenated method commonly used in forensics and environmental...
Gas Chromatography–Mass Spectrometry (GC–MS)
A gas chromatograph consists of a long, narrow capillary column with a polysiloxane coating on the inner wall....
Tandem Mass Spectrometry
High-Resolution Mass Spectrometry (HRMS)
Mass Spectrum: Interpretation