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Flow-injection interface for on-line coupling solid-phase extraction and X-ray fluorescence measurements.

J A Pérez-Serradilla1, M D Luque de Castro

  • 1Department of Analytical Chemistry, Annex Marie Curie Building, Campus of Rabanales, University of Córdoba, E-14071 Córdoba, Spain.

Analytica Chimica Acta
|June 15, 2007
PubMed
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This study introduces a novel online solid-phase extraction coupled with energy-dispersive X-ray fluorescence detection (SPE-EDXRFD) for analyzing lead (Pb) and cadmium (Cd). The method offers a fast, precise, and cost-effective approach for wastewater analysis with low detection limits.

Area of Science:

  • Analytical Chemistry
  • Environmental Science
  • Spectroscopy

Background:

  • Traditional methods for heavy metal analysis can be time-consuming and require complex sample preparation.
  • Solid-phase extraction (SPE) is effective for pre-concentrating analytes but often involves manual steps.
  • Energy-dispersive X-ray fluorescence detection (EDXRFD) is a sensitive technique for elemental analysis.

Purpose of the Study:

  • To develop and validate an online coupling of a flow-injection (FI) system with solid-phase extraction (SPE) and energy-dispersive X-ray fluorescence detection (EDXRFD).
  • To assess the performance of the integrated SPE-EDXRFD system for the determination of lead (Pb) and cadmium (Cd) in aqueous solutions.
  • To demonstrate the applicability of the method for wastewater analysis.

Main Methods:

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  • A flow-injection (FI) manifold was integrated with a solid-phase extraction (SPE) mini-column and an energy-dispersive X-ray fluorescence detector (EDXRFD).
  • A lab-modified flow-cell was positioned within the X-ray spectrometer chamber, directly connected to the SPE column.
  • Dowex 50 cation-exchange resin was used as the sorbent for Pb and Cd, with eluates flushed through the flow-cell for monitoring.

Main Results:

  • Achieved low limits of detection (LODs) and quantification (LOQs): 1 µg and 3.2 µg for Pb, and 1.8 µg and 4.8 µg for Cd, respectively.
  • Demonstrated linear dynamic ranges suitable for wastewater analysis (e.g., 1-4000 µg for Pb and 1.8-2000 µg for Cd with 20 mL sample volume).
  • Validated the method using standard addition with groundwater samples, confirming its accuracy and precision.

Conclusions:

  • The online SPE-EDXRFD coupling provides an automatic, cost-effective, fast, and precise method for analyzing heavy metals like Pb and Cd.
  • The system allows for efficient study of variables influencing the SPE process, such as sample volume, pH, and flow rates.
  • This integrated approach is well-suited for the routine analysis of trace metals in environmental samples, including wastewater.