Characterization of transplutonium orthophosphates and trimetaphosphates by Raman spectrophotometry

Hobart, David E.; Begun, G. M.; Haire, R.G.; Hellwege, H.E.

doi:10.1016/0022-5088(83)90186-8

Cited by 6 publications

(8 citation statements)

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“…Raman spectroscopy is an especially well adapted method for the investigation of nuclear materials, thanks to its flexibility permitting remote and in‐situ analyses and its relative ease of use which requires only limited effort for the sample preparation. Recently, it has been used particularly for the identification of different uranium oxides and oxygen defects and for the study of spent nuclear fuels and mixed actinide systems . The main challenge in the field of nuclear materials is of course the sample radioactivity, potentially exposing the user to significant radiation doses but also to the risk of ingestion or incorporation of radiotoxic nuclides.…”

Section: Introductionmentioning

confidence: 99%

“…In order to overcome these drawbacks, a sample encapsulation technique in a double quartz capillary surrounded by an external Pyrex test tube was developed in the 1990s at the Oak Ridge National Laboratory (ORNL) . However, with that approach it was only possible to collect Raman spectra on a 90° or 180° geometry through a curved quartz capsule, yielding a rather poor signal at the Raman detector.…”

Section: Introductionmentioning

confidence: 99%

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An original approach for Raman spectroscopy analysis of radioactive materials and its application to americium‐containing samples

Naji

Colle

Beneš

et al. 2015

J Raman Spectroscopy

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An approach for Raman measurements of highly radioactive samples is presented here. The innovative part of this approach lies in the fact that no single part of the Raman equipment is in direct contact with the radioactive sample, as the sample is sealed in an alphatight capsule. Raman analysis is effectively performed through the optical-grade quartz window closing the capsule. This allows performing micro-Raman measurements on radioactive samples with no limitations on the laser source wavelength, polarisation mode, spectrometer mode and microscope mode (provided the focal length of the microscope objective is greater than the thickness of the quartz window and with sub mg samples). Some example results are shown and discussed. In particular, some spectral features of americium-containing oxide nuclear fuel specimens are presented. Raman spectra clearly reveal in these specimens the presence of abundant oxygen defects induced in the fcc fluorite lattice by trivalent americium. In order to complete the analysis the Raman spectrum of pure americium dioxide was also measured with a lower energy excitation source compared with previous research. The current results seem to be consistent with the possible occurrence of a photolysis process induced by the Raman laser, resulting in the formation of hyperstoichiometric americium sesquioxide Am 2 O 3 + z . Such a photolytic process is deemed to be unavoidable when visible lasers are used as excitation sources for the Raman analysis of americium dioxide.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

An original approach for Raman spectroscopy analysis of radioactive materials and its application to americium‐containing samples

Naji

Colle

Beneš

et al. 2015

J Raman Spectroscopy

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“…In comparison with the method used at ORNL – USA 12 13 14 15 , microscopy can be applied in proper optical conditions (single optical window instead of tubes), reducing the sample quantity needed, as well as the requirements for laser power.…”

Section: Discussionmentioning

confidence: 99%

“…With its ease of use, limited sample preparation, and the possibility for remote measurement, Raman spectroscopy is of particular interest in the nuclear field. It has been used recently for applied studies of radiation damage (defect) in spent nuclear fuel 2 3 4 5 , as well as for fundamental studies on actinide compound systems 6 7 8 9 10 11 12 13 14 15 . The major challenge for Raman measurement of nuclear materials is the inherent risk of radiation exposure and incorporation.…”

Section: Introductionmentioning

confidence: 99%

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A Novel Technique for Raman Analysis of Highly Radioactive Samples Using Any Standard Micro-Raman Spectrometer

Colle

Naji

Sierig

et al. 2017

JoVE

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A novel approach for the Raman measurement of nuclear materials is reported in this paper. It consists of the enclosure of the radioactive sample in a tight capsule that isolates the material from the atmosphere. The capsule can optionally be filled with a chosen gas pressurized up to 20 bars. The micro-Raman measurement is performed through an optical-grade quartz window. This technique permits accurate Raman measurements with no need for the spectrometer to be enclosed in an alpha-tight containment. It therefore allows the use of all options of the Raman spectrometer, like multi-wavelength laser excitation, different polarizations, and single or triple spectrometer modes. Some examples of measurements are shown and discussed. First, some spectral features of a highly radioactive americium oxide sample (AmO2) are presented. Then, we report the Raman spectra of neptunium oxide (NpO2) samples, the interpretation of which is greatly improved by employing three different excitation wavelengths, 17O doping, and a triple mode configuration to measure the anti-stokes Raman lines. This last feature also allows the estimation of the sample surface temperature. Finally, data that were measured on a sample from Chernobyl lava, where phases are identified by Raman mapping, are shown.

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Raman Spectroscopy Coupled with Chemometric Analysis for Speciation and Quantitative Analysis of Aqueous Phosphoric Acid Systems

et al. 2021

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Complex chemical systems that exhibit varied and matrix-dependent speciation are notoriously difficult to monitor and characterize online and in real-time. Optical spectroscopy is an ideal tool for in situ characterization of chemical species that can enable quantification as well as species identification. Chemometric modeling, a multivariate method, has been successfully paired with optical spectroscopy to enable measurement of analyte concentrations even in complex solutions where univariate methods such as Beer’s law analysis fail. Here, Raman spectroscopy is used to quantify the concentration of phosphoric acid and its three deprotonated forms during a titration. In this system, univariate approaches would be difficult to apply due to multiple species being present simultaneously within the solution as the pH is varied. Locally weighted regression (LWR) modeling was used to determine phosphate concentration from spectral signature. LWR results, in tandem with multivariate curve resolution modeling, provide a direct measurement of the concentration of each phosphate species using only the Raman signal. Furthermore, results are presented within the context of fundamental solution chemistry, including Pitzer equations, to compensate for activity coefficients and nonidealities associated with high ionic strength systems.

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Characterization of transplutonium orthophosphates and trimetaphosphates by Raman spectrophotometry

Cited by 6 publications

References 0 publications

An original approach for Raman spectroscopy analysis of radioactive materials and its application to americium‐containing samples

An original approach for Raman spectroscopy analysis of radioactive materials and its application to americium‐containing samples

A Novel Technique for Raman Analysis of Highly Radioactive Samples Using Any Standard Micro-Raman Spectrometer

Raman Spectroscopy Coupled with Chemometric Analysis for Speciation and Quantitative Analysis of Aqueous Phosphoric Acid Systems

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