Gas chromatographic-sulfur chemiluminescent detector procedures for the simultaneous determination of free forms of volatile sulfur compounds including sulfur dioxide and for the determination of their metal-complexed forms

Ontañón, I. (Universidad de Zaragoza) ; Vela, E. ; Hernández-Orte, P. (Universidad de Zaragoza) ; Ferreira, V. (Universidad de Zaragoza)

Resumen: Three different procedures for the quantitative assessment of free and metal complexed volatile sulfur compounds (VSCs) and for the determination of truly free SO 2 have been developed, taking advantage of a GC-sulfur chemiluminescent detector system (GC-SCD) with cryotrapping. The inertness of the inlet systems, together with the column used (SPB-1 sulfur) makes it possible to obtain a non-saturated perfectly Gaussian peak for SO 2 , well resolved from H 2 S. In the main procedure, the injection of 1 mL of the headspace of a sample prepared in complete anoxia and equilibrated at 30 °C makes it possible to get highly sensitive signals for all VSCs and free SO 2 . Detection limits are 3, 35 and 60 ng/L for H 2 S, MeSH and EtSH, 13 µg/L for truly free SO 2 (at pH = 3.4, or 0.46 µg/L for molecular SO 2 ), and better than 1 µg/L for other relevant sulfur volatiles. Method precision is also satisfactory and linearity covers the whole range of occurrence of these compounds. A second procedure, not making use of the cryotrapping unit, gives also satisfactory results, although with higher detection limits (0.03, 0.25 and 0.37 µg/L for free H 2 S, MeSH and EtSH, respectively). For the analysis of free plus metal-complexed forms, it has been demonstrated that the headspace injection of the vapors on a 1:10 brine dilution of the sample heated at 70 °C for 25 min, gives good estimates of the free + metal-complexed forms of H 2 S and wine mercaptans.

Idioma: Inglés

DOI: 10.1016/j.chroma.2019.02.052

Año: 2019

Publicado en: Journal of Chromatography A 1596 (2019), 152-160
ISSN: 0021-9673

Factor impacto JCR: 4.049 (2019)

Categ. JCR: CHEMISTRY, ANALYTICAL rank: 14 / 86 = 0.163 (2019) - Q1 - T1
Categ. JCR: BIOCHEMICAL RESEARCH METHODS rank: 13 / 77 = 0.169 (2019) - Q1 - T1

Factor impacto SCIMAGO: 1.129 - Analytical Chemistry (Q1) - Organic Chemistry (Q1) - Medicine (miscellaneous) (Q1) - Biochemistry (Q2)

Financiación: info:eu-repo/grantAgreement/ES/DGA/FSE
Financiación: info:eu-repo/grantAgreement/ES/DGA/T29
Financiación: info:eu-repo/grantAgreement/ES/MINECO-FEDER/ALI-2014-59840
Financiación: info:eu-repo/grantAgreement/ES/MINECO-FEDER/ALI-2017-87373

Tipo y forma: Article (PostPrint)

Área (Departamento): Área Química Analítica (Dpto. Química Analítica)