Naturally Occurring Montmorillonite-Based Polymer Monolith Composites as Stationary Phases for Capillary Liquid and Gas Chromatography

This work is associated with the preparation of capillary chromatographic columns containing inorganic-organic composites comprised of naturally occurring montmorillonite (MMT) clay mineral and polymethacrylate monolithic material. The prepared composites combine the best qualities of both constitue...

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Main Authors: Ahmad Aqel, Munir Obbed, Ayman A. Ghfar, Kareem Yusuf, Ameen M. Alsubhi, Ahmed Badjah-Hadj-Ahmed
Format: Article
Language:English
Published: MDPI AG 2022-11-01
Series:Separations
Subjects:
Online Access:https://www.mdpi.com/2297-8739/9/12/389
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author Ahmad Aqel
Munir Obbed
Ayman A. Ghfar
Kareem Yusuf
Ameen M. Alsubhi
Ahmed Badjah-Hadj-Ahmed
author_facet Ahmad Aqel
Munir Obbed
Ayman A. Ghfar
Kareem Yusuf
Ameen M. Alsubhi
Ahmed Badjah-Hadj-Ahmed
author_sort Ahmad Aqel
collection DOAJ
description This work is associated with the preparation of capillary chromatographic columns containing inorganic-organic composites comprised of naturally occurring montmorillonite (MMT) clay mineral and polymethacrylate monolithic material. The prepared composites combine the best qualities of both constituents, offering desirable properties for use under the disparate conditions of both GC and HPLC at the same time. The stationary phases were investigated by scanning electron microscopy (SEM), the specific surface area, and thermogravimetric analysis (TGA) and examined in terms of various conditions utilized for GC and HPLC methods. The prepared columns demonstrated an excellent permeability and stability against common chromatographic conditions, such as the eluent type, flow rate, pressure, and temperature. The results confirmed that the addition of small amounts of MMT into the monolith induced significant improvement in the specific surface area, which contributed to the formation of more active sites and enhanced the retention of analytes. The registered column backpressures did not exceed 980 kPa and 16,500 kPa for the prepared GC and HPLC columns, respectively. The prepared columns were subjected to the separation of various interesting compounds possessing different chemistries and polarities, including alkanes, alkylbenzenes, polycyclic aromatic hydrocarbons (PAHs), alcohols, ketones, phenols, some common organic solvents, and isomeric mixtures. Under the optimal conditions, the efficiency of the columns fell between 4900–38,500 plates m<sup>−1</sup> for GC and 3400–58,800 plates m<sup>−1</sup> for capillary HPLC applications. In all cases, the measured chromatographic resolution was more than 1.38, with excellent an peak symmetry and low tailing factors. In comparison with the most commonly used commercial columns, the polysiloxane open tubular column for GC and silica-based C<sub>18</sub> packed column for HPLC, the prepared GC columns demonstrated a faster separation with a higher efficiency, comparable resolution and tailing factors, and lower consumption of carrier gas. Regarding the capillary columns prepared for HPLC, the chromatographic experiments exposed a much lower run time with a comparable efficiency and resolution and drastically lower consumption of mobile phase solvents and samples. The results demonstrate that the MMT-based polymethacrylate monolith composites are applicable as novel and promising separation media for analyzing various mixtures of interest in different fields, such as petrochemical and environmental samples.
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spelling doaj.art-5e73abffb9294fcb9ea2f5d0f10de0462023-11-24T17:59:16ZengMDPI AGSeparations2297-87392022-11-0191238910.3390/separations9120389Naturally Occurring Montmorillonite-Based Polymer Monolith Composites as Stationary Phases for Capillary Liquid and Gas ChromatographyAhmad Aqel0Munir Obbed1Ayman A. Ghfar2Kareem Yusuf3Ameen M. Alsubhi4Ahmed Badjah-Hadj-Ahmed5Department of Chemistry, College of Science, King Saud University, Riyadh 11451, Saudi ArabiaDepartment of Chemistry, College of Science, King Saud University, Riyadh 11451, Saudi ArabiaDepartment of Chemistry, College of Science, King Saud University, Riyadh 11451, Saudi ArabiaDepartment of Chemistry, College of Science, King Saud University, Riyadh 11451, Saudi ArabiaDepartment of Chemistry, College of Science, King Saud University, Riyadh 11451, Saudi ArabiaDepartment of Chemistry, College of Science, King Saud University, Riyadh 11451, Saudi ArabiaThis work is associated with the preparation of capillary chromatographic columns containing inorganic-organic composites comprised of naturally occurring montmorillonite (MMT) clay mineral and polymethacrylate monolithic material. The prepared composites combine the best qualities of both constituents, offering desirable properties for use under the disparate conditions of both GC and HPLC at the same time. The stationary phases were investigated by scanning electron microscopy (SEM), the specific surface area, and thermogravimetric analysis (TGA) and examined in terms of various conditions utilized for GC and HPLC methods. The prepared columns demonstrated an excellent permeability and stability against common chromatographic conditions, such as the eluent type, flow rate, pressure, and temperature. The results confirmed that the addition of small amounts of MMT into the monolith induced significant improvement in the specific surface area, which contributed to the formation of more active sites and enhanced the retention of analytes. The registered column backpressures did not exceed 980 kPa and 16,500 kPa for the prepared GC and HPLC columns, respectively. The prepared columns were subjected to the separation of various interesting compounds possessing different chemistries and polarities, including alkanes, alkylbenzenes, polycyclic aromatic hydrocarbons (PAHs), alcohols, ketones, phenols, some common organic solvents, and isomeric mixtures. Under the optimal conditions, the efficiency of the columns fell between 4900–38,500 plates m<sup>−1</sup> for GC and 3400–58,800 plates m<sup>−1</sup> for capillary HPLC applications. In all cases, the measured chromatographic resolution was more than 1.38, with excellent an peak symmetry and low tailing factors. In comparison with the most commonly used commercial columns, the polysiloxane open tubular column for GC and silica-based C<sub>18</sub> packed column for HPLC, the prepared GC columns demonstrated a faster separation with a higher efficiency, comparable resolution and tailing factors, and lower consumption of carrier gas. Regarding the capillary columns prepared for HPLC, the chromatographic experiments exposed a much lower run time with a comparable efficiency and resolution and drastically lower consumption of mobile phase solvents and samples. The results demonstrate that the MMT-based polymethacrylate monolith composites are applicable as novel and promising separation media for analyzing various mixtures of interest in different fields, such as petrochemical and environmental samples.https://www.mdpi.com/2297-8739/9/12/389stationary phaseseparation columnclay mineralmontmorillonitemonolithpolymethacrylate
spellingShingle Ahmad Aqel
Munir Obbed
Ayman A. Ghfar
Kareem Yusuf
Ameen M. Alsubhi
Ahmed Badjah-Hadj-Ahmed
Naturally Occurring Montmorillonite-Based Polymer Monolith Composites as Stationary Phases for Capillary Liquid and Gas Chromatography
Separations
stationary phase
separation column
clay mineral
montmorillonite
monolith
polymethacrylate
title Naturally Occurring Montmorillonite-Based Polymer Monolith Composites as Stationary Phases for Capillary Liquid and Gas Chromatography
title_full Naturally Occurring Montmorillonite-Based Polymer Monolith Composites as Stationary Phases for Capillary Liquid and Gas Chromatography
title_fullStr Naturally Occurring Montmorillonite-Based Polymer Monolith Composites as Stationary Phases for Capillary Liquid and Gas Chromatography
title_full_unstemmed Naturally Occurring Montmorillonite-Based Polymer Monolith Composites as Stationary Phases for Capillary Liquid and Gas Chromatography
title_short Naturally Occurring Montmorillonite-Based Polymer Monolith Composites as Stationary Phases for Capillary Liquid and Gas Chromatography
title_sort naturally occurring montmorillonite based polymer monolith composites as stationary phases for capillary liquid and gas chromatography
topic stationary phase
separation column
clay mineral
montmorillonite
monolith
polymethacrylate
url https://www.mdpi.com/2297-8739/9/12/389
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