title: Determination of trace sulfur in biodiesel and diesel standard reference materials by isotope dilution sector field inductively coupled plasma mass spectrometry.
abstract: A method is described for quantification of sulfur at low concentrations on the order of mgkg(-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 (32)S and (34)S 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 (32)S 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.
authors: Group of Applied Instrumental Analysis, Department of Chemistry, Federal University of São Carlos, São Carlos, SP, Brazil.
authors: Renata S
authors: RS
authors: Amais
authors: Chemical Sciences Division, National Institute of Standards and Technology, Charleston, SC, United States.
authors: Stephen E
authors: SE
authors: Long
authors: Group of Applied Instrumental Analysis, Department of Chemistry, Federal University of São Carlos, São Carlos, SP, Brazil.
authors: Joaquim A
authors: JA
authors: Nóbrega
authors: Chemical Sciences Division, National Institute of Standards and Technology, Charleston, SC, United States. Electronic address: steven.christopher@nist.gov.
authors: Steven J
authors: SJ
authors: Christopher
mesh_terms: D056804:Biofuels / Q000032:analysis* / Q000592:standards; D002623:Chemistry Techniques, Analytical / Q000379:methods*; D005742:Gasoline / Q000032:analysis* / Q000592:standards; D006861:Hydrogen Peroxide / Q000737:chemistry; D057230:Limit of Detection; D013058:Mass Spectrometry / Q000592:standards; D008872:Microwaves; D010100:Oxygen / Q000737:chemistry; D010758:Phosphorus / Q000737:chemistry; D012015:Reference Standards; D013455:Sulfur / Q000032:analysis* / Q000592:standards; D013460:Sulfur Isotopes / Q000737:chemistry
chemical_list: D056804:Biofuels; D005742:Gasoline; D013460:Sulfur Isotopes; D010758:Phosphorus; D013455:Sulfur; D006861:Hydrogen Peroxide; D010100:Oxygen
keywords: Diluted nitric acid; Fuel; ID-SF-ICP-MS; Isotope dilution; Microwave-assisted digestion; Sulfur