Measuring Lanthanide Concentrations in Molten Salt Using Laser-Induced Breakdown Spectroscopy (LIBS)

Weisberg, Arel; Lakis, Rollin E.; Simpson, Michael F.; Horowitz, Leo; Craparo, Joseph

doi:10.1366/13-07390

Cited by 27 publications

(20 citation statements)

References 31 publications

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“…Weisberg et al also studied a molten LiCl-KCl salt with additives of EuCl 3 and PrCl 3 using the static surface approach. 7 In this work, a thin film was observed on the top surface of the salts containing Eu and Pr but not on blank LiCl-KCl samples. The composition of the film with respect to the bulk was not reported; however, the presence of the film influenced the shot-to-shot results since plasma formed on the liquid surface differed from those formed on the solid film surface.…”

Section: Introductionmentioning

confidence: 59%

Laser-Induced Breakdown Spectroscopy (LIBS) in a Novel Molten Salt Aerosol System

Williams

Phongikaroon

2016

Appl Spectrosc

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In the pyrochemical separation of used nuclear fuel (UNF), fission product, rare earth, and actinide chlorides accumulate in the molten salt electrolyte over time. Measuring this salt composition in near real-time is advantageous for operational efficiency, material accountability, and nuclear safeguards. Laser-induced breakdown spectroscopy (LIBS) has been proposed and demonstrated as a potential analytical approach for molten LiCl-KCl salts. However, all the studies conducted to date have used a static surface approach which can lead to issues with splashing, low repeatability, and poor sample homogeneity. In this initial study, a novel molten salt aerosol approach has been developed and explored to measure the composition of the salt via LIBS. The functionality of the system has been demonstrated as well as a basic optimization of the laser energy and nebulizer gas pressure used. Initial results have shown that this molten salt aerosol-LIBS system has a great potential as an analytical technique for measuring the molten salt electrolyte used in this UNF reprocessing technology.

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Section: Introductionmentioning

confidence: 59%

Laser-Induced Breakdown Spectroscopy (LIBS) in a Novel Molten Salt Aerosol System

Williams

Phongikaroon

2016

Appl Spectrosc

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“…A more direct approach has been used to monitor the molten salt by performing the analysis directly in the molten salt liquid. [17][18][19][20] In this approach, the laser is fired downwards onto the top surface of the salt to form the plasma on the liquid surface. The plasma formation creates a shock wave that splashes material that can be damaging to the optical equipment used.…”

Section: Introductionmentioning

confidence: 99%

“…In addition, surface inhomogeneity and bubble formation contribute to uncertainty in the results. However, with this approach, chromium (Cr), 17 cobalt (Co), 17 manganese (Mn), 17,18 Ce, 18 europium (Eu), 19 praseodymium (Pr), 19 neptunium (Np), 20 U, 20 and Pu 20 have been successfully measured in the molten salt phase.…”

Section: Introductionmentioning

confidence: 99%

Laser-Induced Breakdown Spectroscopy (LIBS) Measurement of Uranium in Molten Salt

Williams

Phongikaroon

2018

Appl Spectrosc

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In this current study, the molten salt aerosol-laser-induced breakdown spectroscopy (LIBS) system was used to measure the uranium (U) content in a ternary UCl-LiCl-KCl salt to investigate and assess a near real-time analytical approach for material safeguards and accountability. Experiments were conducted using five different U concentrations to determine the analytical figures of merit for the system with respect to U. In the analysis, three U lines were used to develop univariate calibration curves at the 367.01 nm, 385.96 nm, and 387.10 nm lines. The 367.01 nm line had the lowest limit of detection (LOD) of 0.065 wt% U. The 385.96 nm line had the best root mean square error of cross-validation (RMSECV) of 0.20 wt% U. In addition to the univariate calibration approach, a multivariate partial least squares (PLS) model was developed to further analyze the data. Using partial least squares (PLS) modeling, an RMSECV of 0.085 wt% U was determined. The RMSECV from the multivariate approach was significantly better than the univariate case and the PLS model is recommended for future LIBS analysis. Overall, the aerosol-LIBS system performed well in monitoring the U concentration and it is expected that the system could be used to quantitatively determine the U compositions within the normal operational concentrations of U in pyroprocessing molten salts.

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“…Researchers and industrial partners continue to join forces in large-scale investigations to measure, model, and determine if spectroscopy has potential in a wide range of application fields, 10,11 including pharmaceutical, [12][13][14][15] food, [16][17][18][19][20] waste sorting, [21][22][23] bioprocess monitoring, 24 and metallurgy. [25][26][27][28] The potential for inline measurements is ever-increasing as new, enabling technology is being developed, e.g., enhanced silicon and InGaAs detectors, 29,30 OEM spectrometers, [31][32][33] and light-emitting diode (LED) sources. 34 The objective of this review article is to approach inline spectroscopy from a solution design perspective.…”

Section: Introductionmentioning

confidence: 99%

Inline Spectroscopy: From Concept to Function

2018

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The field of applied spectroscopy is strongly dominated by publications presenting proof-of-concepts, lab set-ups, and demonstrations. In contrast, the corresponding number of commercial successes of inline spectroscopy is surprisingly lower. This article discusses inline spectroscopy from an instrumentation perspective. It is the authors' firm belief that the success of inline spectroscopy lies in the understanding of how the design and implementation of the optical instrumentation affects the data quality, and how this in turn will limit or enhance the performance of the prediction model. This article emphasizes the need for a strong, multidisciplinary design team, whose design process is rooted in first principles, to bridge the technology "valley of death" and convert research in applied spectroscopy into commercially successful solutions.

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Measuring Lanthanide Concentrations in Molten Salt Using Laser-Induced Breakdown Spectroscopy (LIBS)

Cited by 27 publications

References 31 publications

Laser-Induced Breakdown Spectroscopy (LIBS) in a Novel Molten Salt Aerosol System

Laser-Induced Breakdown Spectroscopy (LIBS) in a Novel Molten Salt Aerosol System

Laser-Induced Breakdown Spectroscopy (LIBS) Measurement of Uranium in Molten Salt

Inline Spectroscopy: From Concept to Function

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