Sulfur isotope analyses by 3×EA/IRMS: Saving helium and energy while
reducing analytical time and costs
Abstract
Rationale: Helium (He) and energy shortages have dramatically
increased prices and reduced their availability of these commodities.
The use of three combustion reactions per acquisition of carbon and
nitrogen isotope ratios saved 50% He and energy used in elemental
analysis/isotope ratio mass spectrometry (EA/IRMS). This approach should
be tested for sulfur isotope analyses. Mathods: A method was
developed to measure sulfur isotope ratios ( d
34S values) in the SO 2 produced from
three sequential combustion reactions in a single EA/IRMS acquisition.
The combustion cycles involved capsules of the same or different
materials. Two other developments are presented: a system for
simultaneous extraction of chromium-reducible sulfur from four sediments
or rock samples and the connections between the SO 2
reference gas and nitrogen cylinders for purging residual gases at the
end of the EA/IRMS sequences. Results: The 3×EA/IRMS- d
34S method was validated with replicate analyses of
international reference materials and laboratory standards with a wide
range of mineralogical compositions and d 34S
values. It was used for d 34S measurements of
CRS-pyrites from Archean black shales and Swiss lake sediments. The
accuracy and precision of the 3×EA/IRMS values were essentially matched
those obtained by conventional EA/IRMS, with good agreement between the
mean ± SD values and the recommended values and their
Conclusions: Compared with the conventional EA/IRMS method. the
proposed method provides accurate and precise sulfur isotope
compositions of sulfate and sulfide samples while saving approximately
50% of the He, energy, SO 2 reference gas, O
2, and analysis time and cost. Notably, 3×EA/IRMS
provided two d 34S values unaffected by
potential memory effects.