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<p>Heavy metal ions (HMIs) contamination in the fertilizers industry is a global concern, with strict export limits. Moroccan fertilizers, sensitive to these restrictions, could benefit from advanced detection methods. In this study, we synthesized analcime/nepheline (ANA/NEPH) composite from clay-rich illite mineral using a 1.5 M NaOH pre-fusion (800 °C for 1 h) pretreatment and hydrothermal route (150–200&#xa0;°C for 12–24&#xa0;h). The resulting material, with high crystallinity of 167%, a surface area of 19.62 m<sup>2</sup>/g, and a significant CEC of 447&#xa0;meq/100&#xa0;g, was used to modify graphite electrodes (ZeoMGE) for HMIs detection in crude phosphoric acid (CPA). A series of tests, including Fc<sup>+</sup>/Fc probe validation analysis, varying scan rates, and analyte concentration studies, were performed to analyze the ZeoMGE’s potentiometric responses using CV, SWV, and EIS techniques. Results revealed that ANA/NEPH integration improved both the interfacial phenomena and mass transport, enhancing redox peak resolution and significantly reducing impedance <i>R</i><sub>ct</sub> from 184.041 to 16.653 Kohm cm<sup>2</sup>, indicating faster electron transfer and improved accessibility of diffusive species at the electrode interface. The zeolite’s microporous structure facilitated selective adsorption and pre-concentration of HMIs. Specifically, the ZeoMGE detects Zn, Cd, Pb, Cu, As, Cr, and V at low concentrations, with detection limits ranging from 0.143&#xa0;μM (for Cr<sup>6+</sup>) to 13.121&#xa0;nM (for V<sup>2+</sup>) using standard deviation criteria, and sensitivities ranging from 2.923&#xa0;mA/μM cm<sup>2</sup> (for Pb<sup>2+</sup>) to 0.035&#xa0;mA/μM cm<sup>2</sup> (for Cr<sup>6+</sup>), demonstrating high responsiveness and precision in detecting HMIs. This zeolite-based electrode offers a portable solution for HMIs detection in CPA and fertilizers, meeting environmental and regulatory standards.</p> Graphical abstract <p></p>

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Emerging analcime/nepheline-modified graphite sensor for the electroanalysis of heavy metals in crude phosphoric acid samples

  • 期刊论文

  • 发表日期：

    2025年4月28日

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  • Abdellah Ait Baha,
  • Mohammed Lasri,
  • Rachid Idouhli,
  • Kamal Tabit,
  • Abdelmaula Aboulaich,
  • Mohy Eddine Khadiri,
  • Abdesselam Abouelfida

摘要

Heavy metal ions (HMIs) contamination in the fertilizers industry is a global concern, with strict export limits. Moroccan fertilizers, sensitive to these restrictions, could benefit from advanced detection methods. In this study, we synthesized analcime/nepheline (ANA/NEPH) composite from clay-rich illite mineral using a 1.5 M NaOH pre-fusion (800 °C for 1 h) pretreatment and hydrothermal route (150–200 °C for 12–24 h). The resulting material, with high crystallinity of 167%, a surface area of 19.62 m2/g, and a significant CEC of 447 meq/100 g, was used to modify graphite electrodes (ZeoMGE) for HMIs detection in crude phosphoric acid (CPA). A series of tests, including Fc+/Fc probe validation analysis, varying scan rates, and analyte concentration studies, were performed to analyze the ZeoMGE’s potentiometric responses using CV, SWV, and EIS techniques. Results revealed that ANA/NEPH integration improved both the interfacial phenomena and mass transport, enhancing redox peak resolution and significantly reducing impedance Rct from 184.041 to 16.653 Kohm cm2, indicating faster electron transfer and improved accessibility of diffusive species at the electrode interface. The zeolite’s microporous structure facilitated selective adsorption and pre-concentration of HMIs. Specifically, the ZeoMGE detects Zn, Cd, Pb, Cu, As, Cr, and V at low concentrations, with detection limits ranging from 0.143 μM (for Cr6+) to 13.121 nM (for V2+) using standard deviation criteria, and sensitivities ranging from 2.923 mA/μM cm2 (for Pb2+) to 0.035 mA/μM cm2 (for Cr6+), demonstrating high responsiveness and precision in detecting HMIs. This zeolite-based electrode offers a portable solution for HMIs detection in CPA and fertilizers, meeting environmental and regulatory standards.

Graphical abstract