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<p>Heavy metal contamination in water remains a major environmental concern. In this work, ZSM-5 zeolites were synthesized by a microwave-assisted route and optimized by Design of Experiments to enhance adsorption performance. Structural and textural characterization by XRD, N₂-physisorption, and SEM confirmed the formation of crystalline micro–mesoporous ZSM-5 with hierarchical features. The zeolite synthesized under the optimized conditions (Si/Al ratio of 25, tetrapropylammonium bromide concentration of 0.08&#xa0;mol, and crystallization time of 8&#xa0;h) demonstrated a strong ability to selectively remove Cd<sup>2</sup>⁺ at 10&#xa0;µg L<sup>−1</sup> from aqueous solution even in the presence of a ten-fold excess of competing Ca<sup>2</sup>⁺ ions. The zeolite was further integrated into a pipette-tip microextraction format for Co<sup>2</sup>⁺ preconcentration, and the extraction procedure was independently optimized by a second DoE, assessing aspiration/dispensing strokes, sample volume, and temperature. Extraction consisted of a single procedure in which the same solution was repeatedly aspirated and dispensed through the zeolite bed to maximize contact. The regression model for tip extraction achieved <i>R</i><sup>2</sup> = 0.958 and <i>Q</i><sup>2</sup> = 0.892, confirming strong predictive performance and methodological robustness. These results support the use of engineered ZSM-5 as a reusable and low-impact material for monitoring and mitigating heavy-metal pollution in water.</p>

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Optimized microwave-assisted synthesis and application of ZSM-5 zeolites for Cd2⁺ and Co2⁺ adsorption in the presence of competing Ca2⁺

  • 期刊论文

  • 出版模式：

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  • 发表日期：

    2026年2月24日

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  • Fabrizio Ruggieri,
  • Mariagiovanna Accili,
  • Ilenia Di Giuseppe,
  • Alessia Marino,
  • Alfredo Aloise

摘要

Heavy metal contamination in water remains a major environmental concern. In this work, ZSM-5 zeolites were synthesized by a microwave-assisted route and optimized by Design of Experiments to enhance adsorption performance. Structural and textural characterization by XRD, N₂-physisorption, and SEM confirmed the formation of crystalline micro–mesoporous ZSM-5 with hierarchical features. The zeolite synthesized under the optimized conditions (Si/Al ratio of 25, tetrapropylammonium bromide concentration of 0.08 mol, and crystallization time of 8 h) demonstrated a strong ability to selectively remove Cd2⁺ at 10 µg L−1 from aqueous solution even in the presence of a ten-fold excess of competing Ca2⁺ ions. The zeolite was further integrated into a pipette-tip microextraction format for Co2⁺ preconcentration, and the extraction procedure was independently optimized by a second DoE, assessing aspiration/dispensing strokes, sample volume, and temperature. Extraction consisted of a single procedure in which the same solution was repeatedly aspirated and dispensed through the zeolite bed to maximize contact. The regression model for tip extraction achieved R2 = 0.958 and Q2 = 0.892, confirming strong predictive performance and methodological robustness. These results support the use of engineered ZSM-5 as a reusable and low-impact material for monitoring and mitigating heavy-metal pollution in water.