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Published on: July 25, 2014
Handling complex effects in slurry-sampling-electrothermal atomic absorption spectrometry by multivariate
M Felipe-Sotelo1, M J Cal-Prieto, M P Gómez-Carracedo
1Dept. Analytical Chemistry. University of A Coruña, Campus da Zapateira s/n, E-15071 A Coruña, Spain.
This study introduces a new multivariate calibration method for slurry-sampling electrothermal atomic absorption spectrometry (SS-ETAAS). It effectively resolves spectral and chemical interferences from sample concomitants, enabling accurate antimony (Sb) determination in solid matrices.
Area of Science:
- Analytical Chemistry
- Environmental Science
Background:
- Slurry-sampling electrothermal atomic absorption spectrometry (SS-ETAAS) analysis of solid samples faces challenges from spectral and chemical interferences.
- Concomitants in solid matrices can cause interferences that are difficult to resolve with traditional methods like stabilized temperature platform furnace (STPF) conditions or sample ashing.
Purpose of the Study:
- To present a novel approach for managing interferences in SS-ETAAS using multivariate calibration techniques.
- To determine antimony (Sb) concentrations in solid matrices (soils, sediments, coal fly ash) as slurries by ETAAS, overcoming common analytical challenges.
Main Methods:
- Application of multivariate calibration methods, specifically partial least squares (PLS) and artificial neural networks (ANN).
- Utilized experimental designs to develop calibration models and identify key interfering ions (Na+, Ca2+).
- Validated the method by analyzing certified reference materials (CRMs) and assessing robustness.
Main Results:
- Demonstrated that PLS and ANN can effectively handle complex interferences (displacement, depletion, broadening) caused by Na+ and Ca2+ in SS-ETAAS.
- Achieved reliable, fast, and cost-effective prediction of Sb concentrations in diverse solid matrices.
- Showed that linear PLS models are comparable to more complex non-linear ANN models in performance.
Conclusions:
- Multivariate calibration offers a robust and efficient solution for interference management in SS-ETAAS analysis of solid samples.
- The developed method provides accurate and reliable determination of Sb in environmental and industrial solid matrices.
- This approach offers a cost-effective alternative to traditional, time-consuming interference mitigation techniques.
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