<p>Lead contamination of groundwater remains a serious environmental and public health concern, particularly in urban regions where borehole water serves as a major domestic water source. Conventional analytical techniques such as atomic absorption spectroscopy (AAS) and inductively coupled plasma-based methods provide excellent sensitivity for trace metal determination but are often limited by high cost, technical expertise requirements, and infrastructural constraints in many developing regions. In this study, a simple Schiff-base ligand derived from salicylaldehyde (0.01&#xa0;mol) and ethylenediamine (0.01&#xa0;mol) was synthesized under reflux for 2&#xa0;h and evaluated as a low-cost colorimetric sensor for Pb<sup>2+</sup> detection in borehole water collected from Kaduna metropolis, Nigeria. The ligand was obtained as a yellow crystalline product with a percentage yield of 78.4% and melting point of 189–191&#xa0;°C. FT-IR analysis confirmed successful azomethine formation with ν(C=N) band at 1624&#xa0;cm<sup>−1</sup>, while 1H NMR spectroscopy showed characteristic azomethine proton resonance at <i>δ</i> 8.31&#xa0;ppm, aromatic proton signals at <i>δ</i> 6.82–7.45&#xa0;ppm, methylene linker protons at <i>δ</i> 3.76&#xa0;ppm, and phenolic OH resonance at <i>δ</i> 12.94&#xa0;ppm, confirming ligand formation. Coordination of Pb<sup>2+</sup> through azomethine nitrogen and phenolic oxygen donor sites was accompanied by a shift of the ν(C=N) band to 1598&#xa0;cm<sup>−1</sup> and formation of a probable distorted hemidirected Pb(II) coordination geometry, producing a visible color change from pale-yellow to orange with the emergence of an absorption band at 445&#xa0;nm. Good linearity was obtained over the investigated concentration range with correlation coefficient (<i>R</i><sup>2</sup> = 0.995), slope-based sensitivity of 0.126 AU mg<sup>−1</sup> L, limit of detection (LOD) of 0.82&#xa0;mg/L, and limit of quantification (LOQ) of 2.49&#xa0;mg/L. Selectivity studies showed stronger response toward Pb<sup>2+</sup> relative to competing ions such as Cu<sup>2+</sup>, Zn<sup>2+</sup>, Ni<sup>2+</sup>, Fe<sup>3+</sup>, and Cd<sup>2+</sup> tested at 50&#xa0;mg/L under identical conditions. Application to twelve borehole water samples produced recovery values of 92–98% with relative standard deviations below 3.0%, indicating satisfactory precision and analytical applicability. Although not intended to replace ultra-trace instrumental methods, the developed sensor offers a simple, rapid, and affordable approach for preliminary groundwater lead monitoring and may serve as an early-warning screening tool for potentially contaminated water sources in resource-limited settings.</p>

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Development and application of a Schiff-base colorimetric sensor for lead (Pb2+) detection in borehole water from Kaduna metropolis, Nigeria

  • Adetutu Oluwakemi Aliyu,
  • Asmau Shehu,
  • Abdulafeez Olayinka Akorede

摘要

Lead contamination of groundwater remains a serious environmental and public health concern, particularly in urban regions where borehole water serves as a major domestic water source. Conventional analytical techniques such as atomic absorption spectroscopy (AAS) and inductively coupled plasma-based methods provide excellent sensitivity for trace metal determination but are often limited by high cost, technical expertise requirements, and infrastructural constraints in many developing regions. In this study, a simple Schiff-base ligand derived from salicylaldehyde (0.01 mol) and ethylenediamine (0.01 mol) was synthesized under reflux for 2 h and evaluated as a low-cost colorimetric sensor for Pb2+ detection in borehole water collected from Kaduna metropolis, Nigeria. The ligand was obtained as a yellow crystalline product with a percentage yield of 78.4% and melting point of 189–191 °C. FT-IR analysis confirmed successful azomethine formation with ν(C=N) band at 1624 cm−1, while 1H NMR spectroscopy showed characteristic azomethine proton resonance at δ 8.31 ppm, aromatic proton signals at δ 6.82–7.45 ppm, methylene linker protons at δ 3.76 ppm, and phenolic OH resonance at δ 12.94 ppm, confirming ligand formation. Coordination of Pb2+ through azomethine nitrogen and phenolic oxygen donor sites was accompanied by a shift of the ν(C=N) band to 1598 cm−1 and formation of a probable distorted hemidirected Pb(II) coordination geometry, producing a visible color change from pale-yellow to orange with the emergence of an absorption band at 445 nm. Good linearity was obtained over the investigated concentration range with correlation coefficient (R2 = 0.995), slope-based sensitivity of 0.126 AU mg−1 L, limit of detection (LOD) of 0.82 mg/L, and limit of quantification (LOQ) of 2.49 mg/L. Selectivity studies showed stronger response toward Pb2+ relative to competing ions such as Cu2+, Zn2+, Ni2+, Fe3+, and Cd2+ tested at 50 mg/L under identical conditions. Application to twelve borehole water samples produced recovery values of 92–98% with relative standard deviations below 3.0%, indicating satisfactory precision and analytical applicability. Although not intended to replace ultra-trace instrumental methods, the developed sensor offers a simple, rapid, and affordable approach for preliminary groundwater lead monitoring and may serve as an early-warning screening tool for potentially contaminated water sources in resource-limited settings.