Efficient Isotope Ratio Analysis of Uranium Particles in Swipe Samples by Total-Reflection X-ray Fluorescence Spectrometry and Secondary Ion Mass Spectrometry

Esaka, Fumitaka; Watanabe, Kazuo; Fukuyama, Hiroyasu; Onodera, Takashi; Esaka, Konomi T.; Magara, Masaaki; Sakurai, S.; Usuda, Shigekazu

doi:10.3327/jnst.41.1027

Cited by 27 publications

(23 citation statements)

References 6 publications

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“…Particles in the sample were recovered onto a glassy carbon planchet (25 mm φ, Hitachi Chemical Co. Ltd., Japan) by a vacuum impaction technique. 10 The planchet was then introduced into the main chamber of SEM. After the identification of individual uranium particles with SEM-EDX, each uranium particle was manipulated with a glass needle attached to a manipulator and transferred onto another glassy carbon planchet.…”

Section: Methodsmentioning

confidence: 99%

Uranium Particle Identification with SEM-EDX for Isotopic Analysis by Secondary Ion Mass Spectrometry

Esaka¹,

Magara²

2016

Mass Spectrometry Letters

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: Secondary ion mass spectrometry (SIMS) is a promising tool to measure isotope ratios of individual uranium particles in environmental samples for nuclear safeguards. However, the analysis requires prior identification of a small number of uranium particles that coexist with a large number of other particles without uranium. In the present study, this identification was performed by scanning electron microscopy -energy dispersive X-ray analysis with automated particle search mode. The analytical results for an environmental sample taken at a nuclear facility indicated that the observation of backscattered electron images with × 1000 magnification was appropriate to efficiently identify uranium particles. Lower magnification (less than × 500) made it difficult to detect smaller particles of approximately 1 µm diameter. After identification, each particle was manipulated and transferred for subsequent isotope ratio analysis by SIMS. Consequently, the isotope ratios of individual uranium particles were successfully determined without any molecular ion interference. It was demonstrated that the proposed technique provides a powerful tool to measure individual particles not only for nuclear safeguards but also for environmental sciences.

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Section: Methodsmentioning

confidence: 99%

Uranium Particle Identification with SEM-EDX for Isotopic Analysis by Secondary Ion Mass Spectrometry

Esaka¹,

Magara²

2016

Mass Spectrometry Letters

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“…[8][9][10][11][12][13][14][15][16][17][18][19][20][21][22][23][24][25][26][27] The methods and procedures were validated, for example, by the use of reference materials certified by NBL (New Brunswick Laboratory) such as CRM111A ( 233 U 29 for validation of the developed bulk and particle analytical methods. The JAEA's measurement results and capabilities were proved to be excellent in the comparisons.…”

Section: Validation Of Methodsmentioning

confidence: 99%

QA/QC Activities and Estimation of Uncertainty for Ultra-trace Analysis of Uranium and Plutonium in Safeguards Environmental Samples

Usuda

Magara

Esaka

et al. 2010

Journal of Nuclear and Radiochemical Sciences

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Japan Atomic Energy Agency (JAEA) has been conducting the environmental sample analysis, which is one of the IAEA's safeguards measures. In the analysis, isotope ratios of ultra-trace amounts of uranium and plutonium in samples taken from nuclear facilities are determined to detect undeclared nuclear materials and activities. In order to keep and enhance the reliability of the measurement results, validation of analytical methods and estimation of measurement uncertainty in such ultra-trace analysis should be properly done in accordance with worldwide standards. In this paper, the current activities on achievement of QA/QC (quality assurance and quality control) and estimation of measurement uncertainty in the ultra-trace analysis at a clean chemistry laboratory (CLEAR) of JAEA are reported.

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“…The sample was prepared in a clean room by transferring the particles onto a planchet (SPI Pyrolytic Graphite Planchet, 25.4 Â 3.2 mm, #428GP-AB) using a vacuum impactor. 10 Additional analyses were performed on CRM U100 deposed also with the vacuum impactor technique, but this time on a 25.4 Â 5.0 mm silicon planchet from company Si-Mat.…”

Section: B Reference Materialsmentioning

confidence: 99%

“…Good detection limits for 236 U can be reached by SIMS on low enriched material but to a lesser extent on high 235 U enriched or weapon grade materials due to the higher hydride ( 235 U 1 H) contribution that interferes with the 236 U isotope. 6,10 In this paper, we present some of the latest developments that were implemented in order to increase the precision in the uranium isotopic measurements as well as to improve the detection limits of 236 U. This includes the optimization of the analytical protocol and new capabilities now available in the CAMECA acquisition and data processing software.…”

Section: Introductionmentioning

confidence: 99%

Latest improvements in isotopic uranium particle analysis by large geometry–secondary ion mass spectrometry for nuclear safeguards purposes

Hedberg

Peres

Fernandes

et al. 2018

Journal of Vacuum Science &Amp; Technology B, Nanotechnology and Microelectronics: Materials, Processing, Measurement, and Phen

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Large geometry secondary ion mass spectrometry can be efficiently used to analyze uranium aerosol particles from dust samples in the search for undeclared nuclear activities. Automated sample screening measurements are followed by more precise and accurate microbeam measurements of both the major and minor uranium isotopes on selected individual particles. The quality of this work is essential in order to be able to draw valuable safeguards conclusions. This paper describes the latest developments that have been undertaken to enhance the detection limits and to reduce the uranium isotope measurement uncertainty. It includes improvements in the analytical protocol as well as in the instrument acquisition software and data reduction method. Recent useful yield measurements have been performed on uranium monodispersed particles using different primary bombardment conditions to compare to previously obtained data. Comparison of uranium isotope measurements when using pyrolytic graphite or silica planchets as a sample substrate will also be presented.

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Efficient Isotope Ratio Analysis of Uranium Particles in Swipe Samples by Total-Reflection X-ray Fluorescence Spectrometry and Secondary Ion Mass Spectrometry

Cited by 27 publications

References 6 publications

Uranium Particle Identification with SEM-EDX for Isotopic Analysis by Secondary Ion Mass Spectrometry

Uranium Particle Identification with SEM-EDX for Isotopic Analysis by Secondary Ion Mass Spectrometry

QA/QC Activities and Estimation of Uncertainty for Ultra-trace Analysis of Uranium and Plutonium in Safeguards Environmental Samples

Latest improvements in isotopic uranium particle analysis by large geometry–secondary ion mass spectrometry for nuclear safeguards purposes

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