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

Williams, Ammon N.; Phongikaroon, Supathorn

doi:10.1177/0003702816648965

Cited by 30 publications

(26 citation statements)

References 18 publications

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“…In this work, the aerosol-LIBS system used in previous molten salt studies was implemented and a full description of the system can be found in the literature. 21,22 In brief, the system consists of a stainless-steel Collison nebulizer, a sealed sampling chamber (with sapphire windows), and a series of filters to remove the aerosol from the gas stream as shown in Fig. 1.…”

Section: Methodsmentioning

confidence: 99%

“…Recently, a novel molten salt aerosol approach has been demonstrated using Ce. 21,22 In this approach, a nebulizer with an argon gas carrier was used to generate a molten salt aerosol into which the laser light was focused to create the plasma. The advantages of this system are that splashing is reduced and the optics are isolated from the salt system.…”

Section: Introductionmentioning

confidence: 99%

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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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Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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

Williams

Phongikaroon

2018

Appl Spectrosc

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“…Laser-induced breakdown spectroscopy was first proposed for electrochemical sampling measurements because it can be performed at significant distance from its intended target, potentially simplifying its implementation and potentially allowing for deployment above the electrorefiner vessel. [62][63][64][65] LIBS has been considered for both in situ 63 and ex situ 65 deployment. The deployment scenario would drive latency of measurement (low for in situ measurements and medium to high for ex situ).…”

Section: Iiib2 Laser-induced Breakdown Spectroscopymentioning

confidence: 99%

Review of Candidate Techniques for Material Accountancy Measurements in Electrochemical Separations Facilities

et al. 2020

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Electrochemical reprocessing (also commonly known as pyroprocessing) of used nuclear fuel is an alternative to aqueous reprocessing that confers a number of advantages, including the ability to process more recently discharged fuel, smaller resultant waste volumes, and the lack of isolation of plutonium in the product stream. While electrochemical reprocessing systems have seen a significant research and development effort, nuclear safeguards and the security of these systems remain underdeveloped, particularly given the significant differences in operating environment and process flow sheet compared with established aqueous methods. In this paper we present an overview of the current state of the art for several of the most promising candidate techniques for material accountancy and process monitoring measurements for electrochemical separations facilities for used nuclear fuel, specifically passive radiation signatures (gamma spectroscopy, neutron spectroscopy, alpha spectrometry, calorimetry, and microcalorimetry), active radiation signatures (X-ray interrogation and its derivatives, high-resolution X-ray, k-edge densitometry, and hybrid k-edge densitometry; laser-induced breakdown spectroscopy; active neutron interrogation and neutron coincidence counting; inductively coupled plasma mass spectrometry; and optical measurements such as ultraviolet visible spectroscopy, near-infrared spectroscopy, and Raman spectroscopy), and control and process state variable monitoring (cyclic voltammetry and bulk measurements such as level and density, load cell forces, and off-gas monitors). This assessment includes an evaluation of each measurement's respective modality (i.e., whether the measurement relates to elemental, isotopic, or other properties), published best estimates of measurement precision, measurement latency, and an overall evaluation of each technique's level of technical maturity. Additionally, this study assesses the most likely locations within the pyroprocessing flow sheet where measurements may be deployed, the physical information required to properly capture the behavior of such measurements, and potential modeling strategies for such measurements. This latter component thus serves to inform future development of process monitoring models in existing and proposed electrochemical separations simulation models.

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“…There are some examples of the practical application of LIBS to characterize materials specifically from the nuclear arena in published literature. To date, the successful identification of fission products, actinides, radionuclides, and activated corrosion products has been reported within a range of supporting materials that include mixed oxide fuels [29], vitrified high level waste [30], and molten salt electrolytes [31]. These include the use of LIBS to analyse specific radioactive materials such as uranium or plutonium, and radionuclides such as 90 In this new study, we undertake a range of LIBS analyses to explore the use of multivariate statistical analysis techniques for discriminating between graphite and charcoal, which is used to represent other carbon-bearing materials and represents a challenging test case.…”

Section: Minor Comments 55mentioning

confidence: 99%

A new analysis workflow for discrimination of nuclear grade graphite using laser-induced breakdown spectroscopy

Horsfall

Trivedi

Smith

et al. 2019

Journal of Environmental Radioactivity

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Stand-off, in-situ, laser induced breakdown spectroscopy (LIBS) offers a rapid, safe, and cost-effective method for discrimination of radioactive waste materials arising during the operation of nuclear plants and from decommissioning activities. Characterisation of waste materials is a critical activity in understanding the nature of the waste, ensuring hazardous material is managed safely and that waste can be segregated for reuse, recycle or sentenced for appropriate disposal. Characterisation of materials, often in hostile environments, requires the ability to remotely differentiate between materials in terms of their chemical composition and radioactivity. This proposition was tested using a case study on nuclear grade graphite. Graphite has been used extensively as a moderator material in many nuclear reactors. Internationally, over 250,000 tons of various nuclear-grade graphite, and graphite-bearing, materials exist and are a major issue for nuclear decommissioning and radioactive waste management, due to the long half-lives of the associated 14C and 36Cl isotopes. LIBS offers a method for discrimination of nuclear grade graphites and other carbon and non-carbon-bearing wastes. This paper describes the development of a workflow method, including LIBS measurement analysis, for the discrimination of pre-irradiated nuclear 'Pile Grade A' (PGA) graphite moderator rod and domestic lumpwood charcoal, which act as surrogates for nuclear grade graphite and other carbon-bearing wastes. A new analysis workflow comprising the examination of spectral characteristics, multivariate analysis and molecular isotopic spectroscopy is proposed to enable rapid segregation of graphite from a heterogeneous waste stream. Enhanced characterisation techniques have the potential to significantly reduce the cost of decommissioning large parts of legacy nuclear generation plants.

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

Cited by 30 publications

References 18 publications

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

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

Review of Candidate Techniques for Material Accountancy Measurements in Electrochemical Separations Facilities

A new analysis workflow for discrimination of nuclear grade graphite using laser-induced breakdown spectroscopy

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