000088163 001__ 88163 000088163 005__ 20200716101443.0 000088163 0247_ $$2doi$$a10.1016/j.chroma.2019.02.052 000088163 0248_ $$2sideral$$a111254 000088163 037__ $$aART-2019-111254 000088163 041__ $$aeng 000088163 100__ $$0(orcid)0000-0002-3348-0843$$aOntañón, I.$$uUniversidad de Zaragoza 000088163 245__ $$aGas 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 000088163 260__ $$c2019 000088163 5060_ $$aAccess copy available to the general public$$fUnrestricted 000088163 5203_ $$aThree 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. 000088163 536__ $$9info:eu-repo/grantAgreement/ES/DGA/FSE$$9info:eu-repo/grantAgreement/ES/DGA/T29$$9info:eu-repo/grantAgreement/ES/MINECO-FEDER/ALI-2014-59840$$9info:eu-repo/grantAgreement/ES/MINECO-FEDER/ALI-2017-87373 000088163 540__ $$9info:eu-repo/semantics/openAccess$$aby-nc-nd$$uhttp://creativecommons.org/licenses/by-nc-nd/3.0/es/ 000088163 590__ $$a4.049$$b2019 000088163 591__ $$aCHEMISTRY, ANALYTICAL$$b14 / 86 = 0.163$$c2019$$dQ1$$eT1 000088163 591__ $$aBIOCHEMICAL RESEARCH METHODS$$b13 / 77 = 0.169$$c2019$$dQ1$$eT1 000088163 592__ $$a1.129$$b2019 000088163 593__ $$aAnalytical Chemistry$$c2019$$dQ1 000088163 593__ $$aOrganic Chemistry$$c2019$$dQ1 000088163 593__ $$aMedicine (miscellaneous)$$c2019$$dQ1 000088163 593__ $$aBiochemistry$$c2019$$dQ2 000088163 655_4 $$ainfo:eu-repo/semantics/article$$vinfo:eu-repo/semantics/acceptedVersion 000088163 700__ $$0(orcid)0000-0003-2885-4668$$aVela, E. 000088163 700__ $$0(orcid)0000-0003-3641-9164$$aHernández-Orte, P.$$uUniversidad de Zaragoza 000088163 700__ $$0(orcid)0000-0002-4353-2483$$aFerreira, V.$$uUniversidad de Zaragoza 000088163 7102_ $$12009$$2750$$aUniversidad de Zaragoza$$bDpto. Química Analítica$$cÁrea Química Analítica 000088163 773__ $$g1596 (2019), 152-160$$pJ. chromatogr. A$$tJournal of Chromatography A$$x0021-9673 000088163 8564_ $$s765459$$uhttps://zaguan.unizar.es/record/88163/files/texto_completo.pdf$$yPostprint 000088163 8564_ $$s229971$$uhttps://zaguan.unizar.es/record/88163/files/texto_completo.jpg?subformat=icon$$xicon$$yPostprint 000088163 909CO $$ooai:zaguan.unizar.es:88163$$particulos$$pdriver 000088163 951__ $$a2020-07-16-09:00:48 000088163 980__ $$aARTICLE