Single-stage separation and quantitation of anionic and cationic forms of transition metals from environmental water using organo-functionalized ordered mesoporous silica

• Surface functionalization of SBA-15 matrix with different groups (i.e., -EDTA (ethylenediamine triacetic acid), and -N(CH 3 ) 3 + Cl - ) were achieved by a facile silylating reaction. • Highly developed mesoporous structure expediting effective eco-toxicants removal. • Cooperative static and dynamic adsorption of pollutants in situ. • The adsorbents with high adsorption capacity and very fast eluted. • Broad applicability to diverse cationic and anionic forms of eco-pollutants in real waters. A simple methodology was proposed for the separation and quantitation of toxic heavy metals (Pb 2+ , Cr 3+ , Cu 2+ , Mn 2+ , Cd 2+ , CrO 4 2- and MnO 4 - ) in the fixed-bed column and batch adsorption experiments using functionalised mesoporous silicas. For this reason, SBA-15 silica with covalently immobilized ethylenediaminetriacetic acid (referred to as MS/EDTA) and quaternary ammonium groups (labelled to as MS/QAS) has been successfully prepared using a post-synthesis approach. The MS/EDTA and MS/QAS samples were characterized by N 2 adsorption/desorption isotherms, FTIR, XPS, SEM and TEM measurements, elemental and titrimetric analysis. Functionalized materials of the SBA-15 type was shown to have a specific surface area of approximately 715-745 m 2 /g. This kind of materials was applied for the adsorption process at static and dynamic conditions after corresponding optimizations with respect to pH values, amount of adsorbent, contact time, interfering compounds on the removal of target ions. All adsorbents exhibit fast adsorption rate and high adsorption capacity. Excellent maximum adsorption capacity of MS/EDTA sample was observed for Pb(II) and Cr(III) ions (until 1.55 mmol/g) at pH 6.5. The K d values of target cations was reached up to 1.8×10 4 mL/g. Interfering effects caused by the presence of alkali metal ions, earth alkali metal ions and some anions were negligible. To reused of adsorbents during four-five cycles with high adsorption capacity using HNO 3 solution (1 M). At the same time, the surface area and concentration (∼4 %) of functional groups on the surface of the adsorbents unchanged after four regeneration cycles. The MS/QAS sample was applied to the selective and efficient removal of Cr(VI) and Mn(VII) ions. The extraction of CrO 4 2- ions at pH 7.5 by the MS/QAS adsorbent is practically unchanged in the presence of other divalent anions such as CO 3 2- and SO 4 2- . The results indicated that the adsorption capacity of the column was lower than that of the batch system. The synthesized mesoporous materials are used as effective energy-efficient adsorbents for simultaneous removal of heavy metal ions in various forms from natural water samples.

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Journal
Chemical Engineering Journal Advances
Published
2025-03-28
DOI
https://doi.org/10.1016/j.ceja.2025.100741
Citations
3
Primary Topic
Analytical chemistry methods development
Type
article
Field-Weighted Citation Impact
1.50

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article

Single-stage separation and quantitation of anionic and cationic forms of transition metals from environmental water using organo-functionalized ordered mesoporous silica

Natalia Kobylinska
3 citations
Chemical Engineering Journal Advances
Analytical chemistry methods development
1.50
article

Single-stage separation and quantitation of anionic and cationic forms of transition metals from environmental water using organo-functionalized ordered mesoporous silica

Natalia Kobylinska
article en
3 citations

Abstract

• Surface functionalization of SBA-15 matrix with different groups (i.e., -EDTA (ethylenediamine triacetic acid), and -N(CH 3 ) 3 + Cl - ) were achieved by a facile silylating reaction. • Highly developed mesoporous structure expediting effective eco-toxicants removal. • Cooperative static and dynamic adsorption of pollutants in situ. • The adsorbents with high adsorption capacity and very fast eluted. • Broad applicability to diverse cationic and anionic forms of eco-pollutants in real waters. A simple methodology was proposed for the separation and quantitation of toxic heavy metals (Pb 2+ , Cr 3+ , Cu 2+ , Mn 2+ , Cd 2+ , CrO 4 2- and MnO 4 - ) in the fixed-bed column and batch adsorption experiments using functionalised mesoporous silicas. For this reason, SBA-15 silica with covalently immobilized ethylenediaminetriacetic acid (referred to as MS/EDTA) and quaternary ammonium groups (labelled to as MS/QAS) has been successfully prepared using a post-synthesis approach. The MS/EDTA and MS/QAS samples were characterized by N 2 adsorption/desorption isotherms, FTIR, XPS, SEM and TEM measurements, elemental and titrimetric analysis. Functionalized materials of the SBA-15 type was shown to have a specific surface area of approximately 715-745 m 2 /g. This kind of materials was applied for the adsorption process at static and dynamic conditions after corresponding optimizations with respect to pH values, amount of adsorbent, contact time, interfering compounds on the removal of target ions. All adsorbents exhibit fast adsorption rate and high adsorption capacity. Excellent maximum adsorption capacity of MS/EDTA sample was observed for Pb(II) and Cr(III) ions (until 1.55 mmol/g) at pH 6.5. The K d values of target cations was reached up to 1.8×10 4 mL/g. Interfering effects caused by the presence of alkali metal ions, earth alkali metal ions and some anions were negligible. To reused of adsorbents during four-five cycles with high adsorption capacity using HNO 3 solution (1 M). At the same time, the surface area and concentration (∼4 %) of functional groups on the surface of the adsorbents unchanged after four regeneration cycles. The MS/QAS sample was applied to the selective and efficient removal of Cr(VI) and Mn(VII) ions. The extraction of CrO 4 2- ions at pH 7.5 by the MS/QAS adsorbent is practically unchanged in the presence of other divalent anions such as CO 3 2- and SO 4 2- . The results indicated that the adsorption capacity of the column was lower than that of the batch system. The synthesized mesoporous materials are used as effective energy-efficient adsorbents for simultaneous removal of heavy metal ions in various forms from natural water samples.

Chemical Engineering Journal AdvancesVol. 22
A.V. Dumansky Institute of Colloid and Water Chemistry (UA)
Ministerio de Economía y Competitividad
Clean water and sanitation
Openalex Percentile: Top 21%
Analytical chemistry methods development
1.50
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