Real-time elemental analysis of liquids for process monitoring using laser-induced breakdown spectroscopy with a liquid wheel sampling approach

Andrews, Hunter B.; Kitzhaber, Zechariah B.; Manard, Benjamin T.; Martin, Madhavi Z.; Sadergaski, Luke R.

doi:10.1039/d4ja00393d

Title: Real-time elemental analysis of liquids for process monitoring using laser-induced breakdown spectroscopy with a liquid wheel sampling approach

Journal Article · 06 February 2025 · Journal of Analytical Atomic Spectrometry

DOI: https://doi.org/10.1039/d4ja00393d · OSTI ID:2514502

^[1];

^[1]

Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)

This article presents an engineered sampling system that used a rotating wheel to form a thin liquid layer, permitting the use of laser-induced breakdown spectroscopy (LIBS) for in situ, real-time elemental impurity quantification during liquid processing. The sampling approach was demonstrated on eight elements from across the periodic table (Na, Al, K, Ca, Ti, Sr, Mo, and Yb). Univariate and multivariate calibrations were presented for each element. The average value for percent root mean square errors of cross-validation for the multivariate models was 3.64%, highlighting the method's strong prediction accuracy. Additionally, the limits of detection for each analyte were estimated from their univariate models: Na = 0.0532, Al = 18.5, K = 0.105, Ca = 0.273, Ti = 67.7, Sr = 0.640, Mo = 22.4, and Yb = 22.9 μg mL^–1. Finally, a test in which multivariate models were used to monitor a liquid system for 80 min was performed to investigate the real-time monitoring capabilities of this liquid LIBS sampling approach. Rigorous measurements were performed to effectively predict the absence and concentrations of multiple analytes as they were spiked and diluted. This demonstration showed the feasibility of using LIBS for real-time liquid quantification models with estimated precision ≤ 8.1%. Finally, the limitations of this approach and potential future improvements are discussed.

View Journal Article

Cite

Export

Save

Research Organization:: Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)

Sponsoring Organization:: USDOE; USDOE Office of Science (SC), Nuclear Physics (NP)

Grant/Contract Number:: AC05-00OR22725

OSTI ID:: 2514502

Journal Information:: Journal of Analytical Atomic Spectrometry, Journal Name: Journal of Analytical Atomic Spectrometry Journal Issue: 3 Vol. 40; ISSN 0267-9477

Publisher:: Royal Society of ChemistryCopyright Statement

Country of Publication:: United States

Language:: English

References (47)

Comparisons between LIBS and ICP/OES Fichet, P.; Tabarant, M.; Salle, B. Analytical and Bioanalytical Chemistry, Vol. 385, Issue 2 https://doi.org/10.1007/s00216-006-0384-7	journal	April 2006
Laser induced breakdown spectroscopy (LIBS) as an analytical tool for the detection of metal ions in aqueous solutions Knopp, R.; Scherbaum, F. J.; Kim, J. I. Fresenius Journal of Analytical Chemistry, Vol. 355, Issue 1 https://doi.org/10.1007/s0021663550016	journal	May 1996
Single Pulse-Laser Induced Breakdown Spectroscopy in aqueous solution De Giacomo, A.; Dell’Aglio, M.; De Pascale, O. Applied Physics A, Vol. 79, Issue 4-6 https://doi.org/10.1007/s00339-004-2622-1	journal	September 2004
Determination of As, Hg, S, and Se in liquid jets by laser-based optical diagnostic technique Bhatt, Chet R.; Hartzler, Daniel; Jain, Jinesh Applied Physics B, Vol. 127, Issue 1 https://doi.org/10.1007/s00340-020-07560-y	journal	January 2021
Partial least-squares regression: a tutorial Geladi, Paul; Kowalski, Bruce R. Analytica Chimica Acta, Vol. 185 https://doi.org/10.1016/0003-2670(86)80028-9	journal	January 1986
Panoramic laser-induced breakdown spectrometry of water Charfi, B.; Harith, M. A. Spectrochimica Acta Part B: Atomic Spectroscopy, Vol. 57, Issue 7 https://doi.org/10.1016/S0584-8547(02)00059-9	journal	July 2002
Data preprocessing for multiblock modelling – A systematization with new methods Campos, Maria P.; Reis, Marco S. Chemometrics and Intelligent Laboratory Systems, Vol. 199 https://doi.org/10.1016/j.chemolab.2020.103959	journal	April 2020
Direct analysis of calcium in liquid infant formula via laser-induced breakdown spectroscopy (LIBS) Cama-Moncunill, Xavier; Markiewicz-Keszycka, Maria; Cullen, Patrick J. Food Chemistry, Vol. 309 https://doi.org/10.1016/j.foodchem.2019.125754	journal	March 2020
Radiative transition probabilities of neutral and singly ionized rare earth elements (La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) estimated by laser-induced breakdown spectroscopy Irvine, Sawyer; Andrews, Hunter; Myhre, Kristian Journal of Quantitative Spectroscopy and Radiative Transfer, Vol. 297 https://doi.org/10.1016/j.jqsrt.2023.108486	journal	March 2023
Elemental analysis of liquid samples by laser induced breakdown spectroscopy (LIBS): Challenges and potential experimental strategies Keerthi, K.; George, Sajan D.; Kulkarni, Suresh D. Optics & Laser Technology, Vol. 147 https://doi.org/10.1016/j.optlastec.2021.107622	journal	March 2022
Quantitative determination of wear metals in engine oils using laser-induced breakdown spectroscopy: A comparison between liquid jets and static liquids Yaroshchyk, Pavel; Morrison, Richard J. S.; Body, Doug Spectrochimica Acta Part B: Atomic Spectroscopy, Vol. 60, Issue 7-8 https://doi.org/10.1016/j.sab.2005.03.011	journal	August 2005
Measurement of Eu and Yb in aqueous solutions by underwater laser induced breakdown spectroscopy Bhatt, Chet R.; Jain, Jinesh C.; Goueguel, Christian L. Spectrochimica Acta Part B: Atomic Spectroscopy, Vol. 137 https://doi.org/10.1016/j.sab.2017.09.009	journal	November 2017
Nanoparticle enhanced laser induced breakdown spectroscopy of liquid samples by using modified surface-enhanced Raman scattering substrates Palásti, Dávid J.; Albrycht, Paweł; Janovszky, Patrick Spectrochimica Acta Part B: Atomic Spectroscopy, Vol. 166 https://doi.org/10.1016/j.sab.2020.105793	journal	April 2020
Sub-ppb detection limit of Cr, Pb, and Cu in water by surface-enhanced LIBS with femtosecond laser Chen, Yutong; Si, Jiarui; Wan, Xiangtong Spectrochimica Acta Part B: Atomic Spectroscopy, Vol. 213 https://doi.org/10.1016/j.sab.2024.106880	journal	March 2024
Laser-induced breakdown spectroscopy for simultaneous determination of Sm, Eu and Gd in aqueous solution Alamelu, D.; Sarkar, A.; Aggarwal, S. K. Talanta, Vol. 77, Issue 1 https://doi.org/10.1016/j.talanta.2008.06.021	journal	October 2008
High-Throughput Elemental Analysis of Small Aqueous Samples by Emission Spectrometry with a Compact, Atmospheric-Pressure Solution-Cathode Glow Discharge Webb, Michael R.; Andrade, Francisco J.; Hieftje, Gary M. Analytical Chemistry, Vol. 79, Issue 20 https://doi.org/10.1021/ac0707885	journal	October 2007
Compact Glow Discharge for the Elemental Analysis of Aqueous Samples Webb, Michael R.; Andrade, Francisco J.; Hieftje, Gary M. Analytical Chemistry, Vol. 79, Issue 20 https://doi.org/10.1021/ac070789x	journal	October 2007
Quantitative Analysis of Liquids from Aerosols and Microdrops Using Laser Induced Breakdown Spectroscopy Cahoon, Erica M.; Almirall, Jose R. Analytical Chemistry, Vol. 84, Issue 5 https://doi.org/10.1021/ac202834j	journal	February 2012
Automated Calibration for Rapid Optical Spectroscopy Sensor Development for Online Monitoring Andrews, Hunter B.; Sadergaski, Luke R. ACS Sensors, Vol. 9, Issue 11 https://doi.org/10.1021/acssensors.4c02211	journal	September 2024
Rapid, direct determination of strontium in natural waters by laser-induced breakdown spectroscopy Popov, Andrey M.; Drozdova, Anastasiya N.; Zaytsev, Sergey M. Journal of Analytical Atomic Spectrometry, Vol. 31, Issue 5 https://doi.org/10.1039/C5JA00468C	journal	January 2016
Determination of lead in aqueous solutions using resonant surface-enhanced LIBS Liu, Kun; Tang, Zhiyang; Zhou, Ran Journal of Analytical Atomic Spectrometry, Vol. 36, Issue 11 https://doi.org/10.1039/D1JA00250C	journal	January 2021
Neptunium transition probabilities estimated through laser induced breakdown spectroscopy (LIBS) measurements Andrews, H. B.; Sadergaski, L. R.; Myhre, K. G. Journal of Analytical Atomic Spectrometry, Vol. 37, Issue 4 https://doi.org/10.1039/D1JA00423A	journal	January 2022
Simultaneous quantification of uranium(vi), samarium, nitric acid, and temperature with combined ensemble learning, laser fluorescence, and Raman scattering for real-time monitoring Sadergaski, Luke R.; Andrews, Hunter B. The Analyst, Vol. 147, Issue 18 https://doi.org/10.1039/D2AN00998F	journal	January 2022
Effect of liquid aerosol temperature on the detection performance of LIBS for analysis of phosphorus element in water Yang, Xinyan; Wang, Xin; Li, Dongdong Journal of Analytical Atomic Spectrometry, Vol. 39, Issue 2 https://doi.org/10.1039/D3JA00286A	journal	January 2024
Automated on-line monitoring of a lithium hydroxide production process using micro-discharge OES Wiggershaus, Bastian; Jeskanen, Miisamari; Roos, Aappo Journal of Analytical Atomic Spectrometry, Vol. 40, Issue 2 https://doi.org/10.1039/D4JA00330F	journal	January 2025
Optimization of liquid jet system for laser-induced breakdown spectroscopy analysis Skočovská, Katarína; Novotný, Jan; Prochazka, David Review of Scientific Instruments, Vol. 87, Issue 4 https://doi.org/10.1063/1.4947233	journal	April 2016
Review of aerosol analysis by laser-induced breakdown spectroscopy Ji, Huiwen; Ding, Yu; Zhang, Liwen Applied Spectroscopy Reviews, Vol. 56, Issue 3 https://doi.org/10.1080/05704928.2020.1780604	journal	June 2020
A Review of Online Monitoring within Used Nuclear Fuel Recycling Processes Tse, Poki; Bessen, Nathan P.; Hall, Gabriel B. Solvent Extraction and Ion Exchange, Vol. 42, Issue 5 https://doi.org/10.1080/07366299.2024.2395917	journal	July 2024
Application of laser-induced breakdown spectroscopy to in situ analysis of liquid samples Beddows, Dave C. S. Optical Engineering, Vol. 39, Issue 8 https://doi.org/10.1117/1.1304855	journal	August 2000
Laser-induced breakdown spectroscopy measurement for liquids: Experimental configurations and sample preparations Harun, Hanin Athirah; Zainal, Roslinda Journal of Nonlinear Optical Physics & Materials, Vol. 27, Issue 02 https://doi.org/10.1142/S0218863518500236	journal	June 2018
Quantification of Lanthanides in a Molten Salt Reactor Surrogate Off-Gas Stream Using Laser-Induced Breakdown Spectroscopy Andrews, Hunter B.; Myhre, Kristian G. Applied Spectroscopy https://doi.org/10.1177/00037028211070323	journal	March 2022
Monitoring Noble Gases (Xe and Kr) and Aerosols (Cs and Rb) in a Molten Salt Reactor Surrogate Off-Gas Stream Using Laser-Induced Breakdown Spectroscopy (LIBS) Andrews, Hunter B.; McFarlane, Joanna; Myhre, Kristian G. Applied Spectroscopy, Vol. 76, Issue 8 https://doi.org/10.1177/00037028221088625	journal	May 2022
Laser Ablation Plasmas and Spectroscopy for Nuclear Applications Kwapis, Emily H.; Borrero, Justin; Latty, Kyle S. Applied Spectroscopy, Vol. 78, Issue 1 https://doi.org/10.1177/00037028231211559	journal	December 2023
Study of laser-induced breakdown emission from liquid under double-pulse excitation Rai, Virendra N.; Yueh, Fang-Yu; Singh, Jagdish P. Applied Optics, Vol. 42, Issue 12 https://doi.org/10.1364/AO.42.002094	journal	January 2003
Double-pulse laser-induced breakdown spectroscopy with liquid jets of different thicknesses Kumar, Akshaya; Yueh, Fang Y.; Singh, Jagdish P. Applied Optics, Vol. 42, Issue 30 https://doi.org/10.1364/AO.42.006047	journal	January 2003
Determination of thorium and uranium in solution by laser-induced breakdown spectrometry Sarkar, Arnab; Alamelu, Devanathan; Aggarwal, Suresh Kumar Applied Optics, Vol. 47, Issue 31 https://doi.org/10.1364/AO.47.000G58	journal	January 2008
Investigation of laser-induced breakdown spectroscopy of a liquid jet Feng, Yuan; Yang, Jiajun; Fan, Jianmei Applied Optics, Vol. 49, Issue 13 https://doi.org/10.1364/AO.49.000C70	journal	January 2010
Determination of Ca and Mg in aqueous solution by laser-induced breakdown spectroscopy using absorbent paper substrates Zhu, Dehua; Wu, Lizhi; Wang, Bin Applied Optics, Vol. 50, Issue 29 https://doi.org/10.1364/AO.50.005695	journal	October 2011
Simple method for liquid analysis by laser-induced breakdown spectroscopy (LIBS) Zhang, D. C.; Hu, Z. Q.; Su, Y. B. Optics Express, Vol. 26, Issue 14, 18794-18802 https://doi.org/10.1364/OE.26.018794	journal	July 2018
Highly sensitive detection of sodium in aqueous solutions using laser-induced breakdown spectroscopy with liquid sheet jets Nakanishi, Ryuzo; Ohba, Hironori; Saeki, Morihisa Optics Express, Vol. 29, Issue 4 https://doi.org/10.1364/OE.415308	journal	February 2021
Optimal Choice of Baseline Correction for Multivariate Calibration of Spectra Liland, Kristian Hovde; Almøy, Trygve; Mevik, Bjørn-Helge Applied Spectroscopy, Vol. 64, Issue 9 https://doi.org/10.1366/000370210792434350	journal	September 2010
Laser-Induced Breakdown Spectroscopy (LIBS), Part I: Review of Basic Diagnostics and Plasma—Particle Interactions: Still-Challenging Issues within the Analytical Plasma Community Hahn, David W.; Omenetto, Nicoló Applied Spectroscopy, Vol. 64, Issue 12 https://doi.org/10.1366/000370210793561691	journal	December 2010
Spectrochemical Analysis of Liquids Using the Laser Spark Cremers, David A.; Radziemski, Leon J.; Loree, Thomas R. Applied Spectroscopy, Vol. 38, Issue 5 https://doi.org/10.1366/0003702844555034	journal	September 1984
Laser-Induced Breakdown Spectroscopy (LIBS), Part II: Review of Instrumental and Methodological Approaches to Material Analysis and Applications to Different Fields Hahn, David W.; Omenetto, Nicoló Applied Spectroscopy, Vol. 66, Issue 4 https://doi.org/10.1366/11-06574	journal	April 2012
Raman Spectroscopy Based On-Line, Real-Time Monitoring to Reduce Composition Uncertainties: Enhanced sensitivity through optimization of Raman Parameters Lines, Amanda; Felmy, Heather; Bryan, Samuel https://doi.org/10.2172/1989700	report	August 2021
Investigation of Laser-Induced Cavity and Plasma Formation in Water Using Double-Pulse LIBS Siemens, Michelle; Emde, Benjamin; Henkel, Marion Physics, Vol. 6, Issue 1 https://doi.org/10.3390/physics6010008	journal	January 2024
Nonlinear Partial Least Squares An Overview Rosipal, Roman Chemoinformatics and Advanced Machine Learning Perspectives: Complex Computational Methods and Collaborative Techniques https://doi.org/10.4018/978-1-61520-911-8.ch009	book	January 2011

Similar Records

Determination of elemental composition of shale rocks by laser induced breakdown spectroscopy

Journal Article · 2016 · Spectrochimica Acta. Part B, Atomic Spectroscopy · OSTI ID:1480827

Sanghapi, Hervé K.; Jain, Jinesh; Bol'shakov, Alexander; +3 more

Chapter 12 - Laser-Induced Breakdown Spectroscopy: Advanced Analytical Technique

Book · 2017 · Molecular and Laser Spectroscopy Advances and Applications 2018 · OSTI ID:1462357

Bhatt, Chet R.; Ghany, Charles T.; Yueh, Fang Y.; +2 more

Analysis of slags using laser-induced breakdown spectroscopy

Journal Article · 2015 · Spectrochimica Acta. Part B, Atomic Spectroscopy · OSTI ID:1480841

Sanghapi, Hervé K.; Ayyalasomayajula, Krishna K.; Yueh, Fang Y.; +4 more

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

Title: Real-time elemental analysis of liquids for process monitoring using laser-induced breakdown spectroscopy with a liquid wheel sampling approach

Citation Formats

References (47)

Similar Records

Related Subjects