Determination of trace sulfur in biodiesel and diesel standard reference materials by isotope dilution sector field inductively coupled plasma mass spectrometry

• Sulfur mass fractions are measured below 10 mg kg−1 in diesel fuel materials.
• SF-ICP-MS resolves molecular interferences, including oxygen and sulfur hydrides.
• A detection limit of 0.7 mg kg−1 (in the fuel sample) was obtained.

A method is described for quantification of sulfur at low concentrations on the order of mg kg−1 in biodiesel and diesel fuels using isotope dilution and sector field inductively coupled plasma mass spectrometry (ID-SF-ICP-MS). Closed vessel microwave-assisted digestion was employed using a diluted nitric acid and hydrogen peroxide decomposition medium to reduce sample dilution volumes. Medium resolution mode was employed to eliminate isobaric interferences at 32S and 34S related to polyatomic phosphorus and oxygen species, and sulfur hydride species. The method outlined yielded respective limits of detection (LOD) and limits of quantification (LOQ) of 0.7 mg kg−1 S and 2.5 mg kg−1 S (in the sample). The LOD was constrained by instrument background counts at 32S but was sufficient to facilitate value assignment of total S mass fraction in NIST SRM 2723b Sulfur in Diesel Fuel Oil at 9.06 ± 0.13 mg kg−1. No statistically significant difference at a 95% confidence level was observed between the measured and certified values for certified reference materials NIST SRM 2773 B100 Biodiesel (Animal-Based), CENAM DRM 272b and NIST SRM 2723a Sulfur in Diesel Fuel Oil, validating method accuracy.

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