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LIBS sensing for in-situ iron detection and quantification in wastewater outfall

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Abstract

Iron measurement in water is important to ensure its quality. Although iron is essential for good health, when its level in water exceeds the permitted limit, it can cause health- and environmental-related issues. In this study, a spectroscopic methodology based on laser-induced breakdown spectroscopy (LIBS) has been developed for in situ detection and quantification of iron in water. Wastewater from the foundation of a historic building at the National Energy Technology Laboratory (NETL) Morgantown site was collected for ten continuous days and analyzed with the LIBS benchtop system and NETL’s LIBS probe. Spectral signatures of iron in the LIBS spectra were identified which demonstrated the significant presence of iron in the test samples. Chemometric tools, principal component analysis (PCA) and linear discriminant analysis (LDA) were used to distinguish the ten liquid samples. For quantitative study, univariate and multivariate analyses were performed. While two strong emission lines of iron, Fe I 371.9 nm and Fe I 373 nm, were used to develop the calibration curve for univariate analysis, whole spectra in the selected wavelength range were utilized to plot the partial least square regression (PLS-R) curve. These calibration curves were then used to estimate the iron content in water samples, and the estimated values were compared to inductively coupled plasma-mass spectrometry (ICP-MS) measurements. The relative difference was found to be less than 15%, which shows that the iron content in liquid can be reliably detected and quantified by the LIBS-based spectroscopic technique.

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Funding

This project was funded by the U.S. Department of Energy, National Energy Technology Laboratory, in part, through a site support contract. Neither the US Government nor any agency thereof, nor any of their employees, nor the support contractor, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the US Government or any agency thereof.

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CRB performed the experiment and data analysis and wrote the manuscript text. DH contributed to perform experiment and data analysis, and DM oversaw the whole project and managed the funding. All authors reviewed the manuscript.

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Correspondence to Chet Raj Bhatt.

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Bhatt, C.R., Hartzler, D. & McIntyre, D. LIBS sensing for in-situ iron detection and quantification in wastewater outfall. Appl. Phys. B 130, 18 (2024). https://doi.org/10.1007/s00340-023-08156-y

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