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

Autor(es)

Amais, Renata S. ^[1] ; Long, Stephen E. ^[2] ; Nobrega, Joaquim A. ^[1] ; Christopher, Steven J. ^[2]

Afiliação do(s) autor(es)

^[1] Univ Fed Sao Carlos, Dept Chem, Grp Appl Instrumental Anal, BR-13560 Sao Carlos, SP - Brazil

^[2] NIST, Div Chem Sci, Charleston, SC - USA

• Tipo de documento: Artigo Científico
• Fonte: Analytica Chimica Acta; v. 806, p. 91-96, JAN 2 2014.
• Citações Web of Science: 18

Resumo

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 S-32 and S-34 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 S-32 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. Published by Elsevier B.V. (AU)

• Processo FAPESP: 10/17387-7 - Avaliação de técnicas espectroanalíticas e procedimentos de preparo de amostras para a determinação de enxofre em biodiesel e misturas com diesel
• Beneficiário: Renata Stábile Amais
• Modalidade de apoio: Bolsas no Brasil - Doutorado
• Processo FAPESP: 12/00920-0 - Avaliação da espectrometria de massas de alta resolução com plasma acoplado indutivamente para a determinação de enxofre em biodiesel e misturas com diesel
• Beneficiário: Renata Stábile Amais
• Modalidade de apoio: Bolsas no Exterior - Estágio de Pesquisa - Doutorado