title: Determination of alcohol sulfates in wastewater treatment plant influents and effluents by gas chromatography-mass spectrometry.
abstract: In the present paper, we developed an accurate method for the analysis of alcohol sulfates (AS) in wastewater samples from wastewater treatment plant (WWTP) influents and effluents. Although many methodologies have been published in the literature concerning the study of anionic surfactants in environmental samples, at present, the number of analytical methodologies that focus in the determination of AS by gas chromatography in the different environmental compartments is limited. The reason for this is that gas chromatography-mass spectrometry (GC-MS) technique requires a previous hydrolysis reaction followed by derivatization reactions. In the present work, we proposed a new procedure in which the hydrolysis and derivatization reactions take place in one single step and AS are directly converted to trimethylsilyl derivatives. The main factors affecting solid-phase extraction (SPE), hydrolysis/derivatization and GC-MS procedures were accurately optimised. Quantification of the target compounds was performed by using GC-MS in selected ion monitoring (SIM) mode. The limits of detection (LOD) obtained ranged from 0.2 to 0.3 μg L(-1), and limits of quantification (LOQ) from 0.5 to 1.0 μg L(-1), while inter- and intra-day variability was under 5%. A recovery assay was also carried out. Recovery rates for homologues in spiked samples ranged from 96 to 103%. The proposed method was successfully applied for the determination of anionic surfactants in wastewater samples from one WWTP located in Granada (Spain). Concentration levels for the homologues up to 39.4 μg L(-1) in influent and up to 8.1 μg L(-1) in effluent wastewater samples.
authors.affiliation: Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, University of Granada, Campus of Fuentenueva, E-18071 Granada, Spain.
authors.forename: C
authors.initials: C
authors.lastname: Fernández-Ramos
authors.forename: O
authors.initials: O
authors.lastname: Ballesteros
authors.forename: R
authors.initials: R
authors.lastname: Blanc
authors.forename: A
authors.initials: A
authors.lastname: Zafra-Gómez
authors.forename: I
authors.initials: I
authors.lastname: Jiménez-Díaz
authors.forename: A
authors.initials: A
authors.lastname: Navalón
authors.forename: J L
authors.initials: JL
authors.lastname: Vílchez
mesh_terms: D000438:Alcohols / Q000032:analysis*; D004784:Environmental Monitoring; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D057230:Limit of Detection; D052616:Solid Phase Extraction; D013431:Sulfates; D013501:Surface-Active Agents / Q000032:analysis*; D014297:Trimethylsilyl Compounds / Q000737:chemistry*; D062065:Wastewater / Q000737:chemistry*; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D000438:Alcohols; D013431:Sulfates; D013501:Surface-Active Agents; D014297:Trimethylsilyl Compounds; D062065:Wastewater; D014874:Water Pollutants, Chemical