88163 20200716101443.0 doi 10.1016/j.chroma.2019.02.052 sideral 111254 ART-2019-111254 eng (orcid)0000-0002-3348-0843 Ontañón, I. Universidad de Zaragoza 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 2019 Access copy available to the general public Unrestricted 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. info:eu-repo/grantAgreement/ES/DGA/FSE info:eu-repo/grantAgreement/ES/DGA/T29 info:eu-repo/grantAgreement/ES/MINECO-FEDER/ALI-2014-59840 info:eu-repo/grantAgreement/ES/MINECO-FEDER/ALI-2017-87373 info:eu-repo/semantics/openAccess by-nc-nd http://creativecommons.org/licenses/by-nc-nd/3.0/es/ 4.049 2019 CHEMISTRY, ANALYTICAL 14 / 86 = 0.163 2019 Q1 T1 BIOCHEMICAL RESEARCH METHODS 13 / 77 = 0.169 2019 Q1 T1 1.129 2019 Analytical Chemistry 2019 Q1 Organic Chemistry 2019 Q1 Medicine (miscellaneous) 2019 Q1 Biochemistry 2019 Q2 info:eu-repo/semantics/article info:eu-repo/semantics/acceptedVersion (orcid)0000-0003-2885-4668 Vela, E. (orcid)0000-0003-3641-9164 Hernández-Orte, P. Universidad de Zaragoza (orcid)0000-0002-4353-2483 Ferreira, V. Universidad de Zaragoza 2009 750 Universidad de Zaragoza Dpto. Química Analítica Área Química Analítica 1596 (2019), 152-160 J. chromatogr. A Journal of Chromatography A 0021-9673 765459 http://zaguan.unizar.es/record/88163/files/texto_completo.pdf Postprint 229971 http://zaguan.unizar.es/record/88163/files/texto_completo.jpg?subformat=icon icon Postprint oai:zaguan.unizar.es:88163 articulos driver 2020-07-16-09:00:48 ARTICLE