Synthesis and Characterization of Mesoporous Silica Modified with Purpald and Its Application in the Preconcentration of Cu<sup>2+</sup> and Cd<sup>2+</sup> from Aqueous Samples through Solid-Phase Extraction
The synthesis of an organofunctionalized mesoporous silica was accomplished by a two-step process involving (1) the co-condensation of a silylant agent at the surface of silica, followed by (2) the immobilization of Purpald (ligand) at the organic termination of the silytant agent. The characterizat...
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MDPI AG
2023-02-01
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| author | Marcos Henrique Pereira Wondracek Alexandre de Oliveira Jorgetto Adrielli Cristina Peres da Silva José Fabián Schneider Valber de Albuquerque Pedrosa Margarida Juri Saeki Gustavo Rocha de Castro |
| author_facet | Marcos Henrique Pereira Wondracek Alexandre de Oliveira Jorgetto Adrielli Cristina Peres da Silva José Fabián Schneider Valber de Albuquerque Pedrosa Margarida Juri Saeki Gustavo Rocha de Castro |
| author_sort | Marcos Henrique Pereira Wondracek |
| collection | DOAJ |
| description | The synthesis of an organofunctionalized mesoporous silica was accomplished by a two-step process involving (1) the co-condensation of a silylant agent at the surface of silica, followed by (2) the immobilization of Purpald (ligand) at the organic termination of the silytant agent. The characterization of the organofunctionalized material indicated the presence of NH<sub>2</sub> groups, and the immobilization of the ligand was confirmed by <sup>29</sup>Si- and <sup>13</sup>C-nuclear magnetic resonance. The material’s surface area was determined as 370 m<sup>2</sup> g<sup>−1</sup>. Batch adsorption experiments enabled the determination of optimum pH conditions for the adsorption of Cu(II) and Cd(II). Under optimal pH, the pseudo-second-order kinetic model and Langmuir model provided the best correlations to describe the materials adsorption behavior, suggesting a chemisorption mechanism. When tested in continuous-flow preconcentration experiments, the flow rate and eluent concentration demonstrated to affect the removal of Cu(II) and Cd(II), while the buffer concentration had an effect only over the adsorption of Cu(II). Under optimized preconcentration conditions, it was possible both to determine the concentrations of Cu(II) and Cd(II) in samples such as mineral water, ground water, tap water and river water. Ions commonly found in drinking and natural waters (Na<sup>+</sup>, K<sup>+</sup>, Ca<sup>2+</sup>, Mg<sup>2+</sup>, Fe<sup>3+</sup>, Ba<sup>2+</sup>, Cl<sup>−</sup>, SO<sub>4</sub><sup>2−</sup>, HCO<sub>3</sub><sup>−</sup>, and H2PO<sub>4</sub><sup>−</sup>) did not affect the preconcentration of any of the studied analytes. Reutilization experiments indicated that the adsorbent material can withstand at least 40 adsorption/desorption preconcentration cycles with no efficiency loss. |
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| spelling | doaj.art-0d3e188ceaf645ceab6bc65d89884bdb2023-11-16T23:14:27ZengMDPI AGSeparations2297-87392023-02-0110210810.3390/separations10020108Synthesis and Characterization of Mesoporous Silica Modified with Purpald and Its Application in the Preconcentration of Cu<sup>2+</sup> and Cd<sup>2+</sup> from Aqueous Samples through Solid-Phase ExtractionMarcos Henrique Pereira Wondracek0Alexandre de Oliveira Jorgetto1Adrielli Cristina Peres da Silva2José Fabián Schneider3Valber de Albuquerque Pedrosa4Margarida Juri Saeki5Gustavo Rocha de Castro6Faculty of Science and Technology, University of Grande Dourados, Rodovia Dourados-Itahum, km 12, Dourados 79804-970, MS, BrazilInterdisciplinary Laboratory of Nanostructures and Semiconductors (LINSE-IQ-UNESP), Rua Francisco Degni, 55, Araraquara 14800-060, SP, BrazilChemistry and Biochemistry Department, Institute of Biosciences of Botucatu-UNESP, C.P. 510, Botucatu 18618-000, SP, BrazilInstituto de Física de São Carlos (IFSC), Universidade de São Paulo (USP), São Carlos 13566-590, SP, BrazilChemistry and Biochemistry Department, Institute of Biosciences of Botucatu-UNESP, C.P. 510, Botucatu 18618-000, SP, BrazilChemistry and Biochemistry Department, Institute of Biosciences of Botucatu-UNESP, C.P. 510, Botucatu 18618-000, SP, BrazilChemistry and Biochemistry Department, Institute of Biosciences of Botucatu-UNESP, C.P. 510, Botucatu 18618-000, SP, BrazilThe synthesis of an organofunctionalized mesoporous silica was accomplished by a two-step process involving (1) the co-condensation of a silylant agent at the surface of silica, followed by (2) the immobilization of Purpald (ligand) at the organic termination of the silytant agent. The characterization of the organofunctionalized material indicated the presence of NH<sub>2</sub> groups, and the immobilization of the ligand was confirmed by <sup>29</sup>Si- and <sup>13</sup>C-nuclear magnetic resonance. The material’s surface area was determined as 370 m<sup>2</sup> g<sup>−1</sup>. Batch adsorption experiments enabled the determination of optimum pH conditions for the adsorption of Cu(II) and Cd(II). Under optimal pH, the pseudo-second-order kinetic model and Langmuir model provided the best correlations to describe the materials adsorption behavior, suggesting a chemisorption mechanism. When tested in continuous-flow preconcentration experiments, the flow rate and eluent concentration demonstrated to affect the removal of Cu(II) and Cd(II), while the buffer concentration had an effect only over the adsorption of Cu(II). Under optimized preconcentration conditions, it was possible both to determine the concentrations of Cu(II) and Cd(II) in samples such as mineral water, ground water, tap water and river water. Ions commonly found in drinking and natural waters (Na<sup>+</sup>, K<sup>+</sup>, Ca<sup>2+</sup>, Mg<sup>2+</sup>, Fe<sup>3+</sup>, Ba<sup>2+</sup>, Cl<sup>−</sup>, SO<sub>4</sub><sup>2−</sup>, HCO<sub>3</sub><sup>−</sup>, and H2PO<sub>4</sub><sup>−</sup>) did not affect the preconcentration of any of the studied analytes. Reutilization experiments indicated that the adsorbent material can withstand at least 40 adsorption/desorption preconcentration cycles with no efficiency loss.https://www.mdpi.com/2297-8739/10/2/108adsorptionsolid-phase extractionpreconcentrationtoxic metals |
| spellingShingle | Marcos Henrique Pereira Wondracek Alexandre de Oliveira Jorgetto Adrielli Cristina Peres da Silva José Fabián Schneider Valber de Albuquerque Pedrosa Margarida Juri Saeki Gustavo Rocha de Castro Synthesis and Characterization of Mesoporous Silica Modified with Purpald and Its Application in the Preconcentration of Cu<sup>2+</sup> and Cd<sup>2+</sup> from Aqueous Samples through Solid-Phase Extraction Separations adsorption solid-phase extraction preconcentration toxic metals |
| title | Synthesis and Characterization of Mesoporous Silica Modified with Purpald and Its Application in the Preconcentration of Cu<sup>2+</sup> and Cd<sup>2+</sup> from Aqueous Samples through Solid-Phase Extraction |
| title_full | Synthesis and Characterization of Mesoporous Silica Modified with Purpald and Its Application in the Preconcentration of Cu<sup>2+</sup> and Cd<sup>2+</sup> from Aqueous Samples through Solid-Phase Extraction |
| title_fullStr | Synthesis and Characterization of Mesoporous Silica Modified with Purpald and Its Application in the Preconcentration of Cu<sup>2+</sup> and Cd<sup>2+</sup> from Aqueous Samples through Solid-Phase Extraction |
| title_full_unstemmed | Synthesis and Characterization of Mesoporous Silica Modified with Purpald and Its Application in the Preconcentration of Cu<sup>2+</sup> and Cd<sup>2+</sup> from Aqueous Samples through Solid-Phase Extraction |
| title_short | Synthesis and Characterization of Mesoporous Silica Modified with Purpald and Its Application in the Preconcentration of Cu<sup>2+</sup> and Cd<sup>2+</sup> from Aqueous Samples through Solid-Phase Extraction |
| title_sort | synthesis and characterization of mesoporous silica modified with purpald and its application in the preconcentration of cu sup 2 sup and cd sup 2 sup from aqueous samples through solid phase extraction |
| topic | adsorption solid-phase extraction preconcentration toxic metals |
| url | https://www.mdpi.com/2297-8739/10/2/108 |
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