Automated method for volatile fatty acids determination in anaerobic processes using in-syringe magnetic stirring assisted dispersive liquid-liquid microextraction and gas chromatography with flame ionization detector
•The sensitivity and precision for the VFAs determination was improved.•In-syringe-DLLME prior GC-FID is an effective, economic and green method.•Optimization of extraction conditions was performed.•Good accuracy and recoveries were obtained.•The automated method data was comparable to the standard...
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Published in | Journal of Chromatography A Vol. 1643; p. 462034 |
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Main Authors | , , , |
Format | Journal Article |
Language | English |
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Elsevier B.V
26.04.2021
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Abstract | •The sensitivity and precision for the VFAs determination was improved.•In-syringe-DLLME prior GC-FID is an effective, economic and green method.•Optimization of extraction conditions was performed.•Good accuracy and recoveries were obtained.•The automated method data was comparable to the standard method.
Volatile fatty acids (VFAs) are key parameters to monitor anaerobic digestion processes. Thus, a fast, simple and precise determination of these analytes is necessary for a timely characterization of the biological processes present in municipal solid waste and wastewater treatment plants. In this work, an automated method for the extraction and preconcentration of VFAs, based on dispersive liquid-liquid microextraction with magnetic stirring in syringe, and gas chromatography with flame ionization detector for the separation and detection, is described. The effect of parameters such as the type and volume of extraction solvent, pH, salting out effect and stirring time, was studied using a multivariate and univariate experimental design. Extraction and preconcentration were performed simultaneously using tert-butyl methyl ether (TBME) as the extraction solvent, after stirring 100 s at a constant rate. The detection limits were in the range of 0.1 - 1.3 mg L−1 and a good linearity was observed up to 1000 mg L−1 of the studied VFAs, with a range of R2 between 0.9997 and 0.9999. The intra and interday precision expressed as relative standard deviation (n= 5) varied between 0.7 and 2.4% and between 1.7 and 7.0%, respectively. Subsequently, the developed method was successfully applied to evaluate the presence of VFAs in wastewater samples from anaerobic treatments and an average relative recovery of 102% was obtained. |
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AbstractList | •The sensitivity and precision for the VFAs determination was improved.•In-syringe-DLLME prior GC-FID is an effective, economic and green method.•Optimization of extraction conditions was performed.•Good accuracy and recoveries were obtained.•The automated method data was comparable to the standard method.
Volatile fatty acids (VFAs) are key parameters to monitor anaerobic digestion processes. Thus, a fast, simple and precise determination of these analytes is necessary for a timely characterization of the biological processes present in municipal solid waste and wastewater treatment plants. In this work, an automated method for the extraction and preconcentration of VFAs, based on dispersive liquid-liquid microextraction with magnetic stirring in syringe, and gas chromatography with flame ionization detector for the separation and detection, is described. The effect of parameters such as the type and volume of extraction solvent, pH, salting out effect and stirring time, was studied using a multivariate and univariate experimental design. Extraction and preconcentration were performed simultaneously using tert-butyl methyl ether (TBME) as the extraction solvent, after stirring 100 s at a constant rate. The detection limits were in the range of 0.1 - 1.3 mg L−1 and a good linearity was observed up to 1000 mg L−1 of the studied VFAs, with a range of R2 between 0.9997 and 0.9999. The intra and interday precision expressed as relative standard deviation (n= 5) varied between 0.7 and 2.4% and between 1.7 and 7.0%, respectively. Subsequently, the developed method was successfully applied to evaluate the presence of VFAs in wastewater samples from anaerobic treatments and an average relative recovery of 102% was obtained. |
ArticleNumber | 462034 |
Author | Vargas-Muñoz, M.A. Cerdà, Víctor Cadavid-Rodríguez, L.S. Palacio, Edwin |
Author_xml | – sequence: 1 givenname: M.A. orcidid: 0000-0001-7263-7500 surname: Vargas-Muñoz fullname: Vargas-Muñoz, M.A. organization: Group of Environmental Analytical Chemistry, University of the Balearic Islands, Cra.Valldemossa km 7.5, 07122 Palma de Mallorca, Spain – sequence: 2 givenname: Víctor surname: Cerdà fullname: Cerdà, Víctor organization: Group of Environmental Analytical Chemistry, University of the Balearic Islands, Cra.Valldemossa km 7.5, 07122 Palma de Mallorca, Spain – sequence: 3 givenname: L.S. surname: Cadavid-Rodríguez fullname: Cadavid-Rodríguez, L.S. organization: Department of Engineering, Faculty of Engineering and Administration, Universidad Nacional de Colombia - Sede Palmira, Cra. 32 No 12-00, Palmira, Colombia – sequence: 4 givenname: Edwin surname: Palacio fullname: Palacio, Edwin email: edwin.palacio@uib.es organization: Group of Environmental Analytical Chemistry, University of the Balearic Islands, Cra.Valldemossa km 7.5, 07122 Palma de Mallorca, Spain |
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CitedBy_id | crossref_primary_10_1016_j_greeac_2022_100023 crossref_primary_10_1016_j_biteb_2022_101123 crossref_primary_10_1016_j_cej_2022_137833 crossref_primary_10_1016_j_biteb_2023_101715 crossref_primary_10_1016_j_microc_2022_107863 crossref_primary_10_1016_j_compchemeng_2023_108524 crossref_primary_10_3390_molecules27217279 |
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Keywords | volatile fatty acids anaerobic treatment , automation gas chromatography In-syringe magnetic-stirring-assisted dispersive liquid-liquid microextraction (In syringe-MSA-DLLME) |
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Snippet | •The sensitivity and precision for the VFAs determination was improved.•In-syringe-DLLME prior GC-FID is an effective, economic and green method.•Optimization... |
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SubjectTerms | anaerobic treatment , automation gas chromatography In-syringe magnetic-stirring-assisted dispersive liquid-liquid microextraction (In syringe-MSA-DLLME) volatile fatty acids |
Title | Automated method for volatile fatty acids determination in anaerobic processes using in-syringe magnetic stirring assisted dispersive liquid-liquid microextraction and gas chromatography with flame ionization detector |
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