Development of an improved method to perform single particle analysis by TIMS for nuclear safeguards

Kraiem, M.; Stephan, Richter; Kühn, He; Yetunde, Aregbe

doi:10.1016/j.aca.2010.12.003

Cited by 38 publications

(38 citation statements)

References 19 publications

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“…The safeguard authorities requirement for 235 U abundance measurement uncertainty by TIMS is set to 0.28% [8]. The isotopic abundance of 234 U provides information about the type of activities conducted in the nuclear installations: enrichment or reprocessing [3,9]. However, 234 U stays a minor isotope with an isotopic abundance below 0.1% whatever its origins: enriched uranium, spent nuclear fuel, reprocessed uranium or depleted uranium.…”

Section: Introductionmentioning

confidence: 99%

“…The major development for the low quantities measurements is the use the electron multipliers [9,[13][14][15]18,19]. They are used to further extend the sensitivity of the instrument by several orders of magnitude.…”

Section: Introductionmentioning

confidence: 99%

“…Thermal ionization mass spectrometry (TIMS) is a reference technique for uranium isotope measurement [9][10][11][12][13][14][15]. TIMS allows measurement of isotope ratio with high trueness and precision, allowing the knowledge of isotope ratio with an uncertainty sometimes lower than 0.1% [10,11,13,[16][17][18].…”

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Development of an analysis method of minor uranium isotope ratio measurements using electron multipliers in Thermal Ionization Mass Spectrometry

Quemet

Maloubier

Dalier

et al. 2014

International Journal of Mass Spectrometry

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a b s t r a c tA simple analytical procedure was developed to measure with high accuracy the isotope ratio of minor isotope of natural uranium present in small quantities using a thermal ionization mass spectrometer (TIMS). The reduction of quantities used for analysis and the measurement of non-abundant isotopes are of prime interest in the nuclear industry. Indeed it is necessary to reduce the analyst received dose and the effluent released, as well as realizing measurement at trace level. The new generation of TIMS is equipped with a multicollection system of electron multipliers: discrete dynode electron multiplier (SEM) and continuous dynode electron multiplier (MIC), that improve the sensitivity compared to faraday cups. The procedure developed was verified using Certified Reference Material IRMM 052. Results were evaluated relying on NF T 90-210 norm regarding method validation. First, the isotope ratio 234 U/ 238 U was examined by total evaporation using the SEM and MIC to measure 234 U and the faraday cup to measure 238 U. In a second approach, the isotope ratio 235 U/ 238 U was studied by total evaporation using the SEM to measure 235 U and the faraday cup to measure 238 U. The classical method with peak-jumping SEM measurement was also used. Total evaporation method employing only the faraday cup was used to confront the results obtained. The analyzable quantity was reduced from 250 ng to 50 ng for the 235 U/ 238 U isotope ratio and from 1270 ng to 50 ng for the 234 U/ 238 U isotope ratio with acceptable uncertainties thanks to the use of electron multipliers. For all experiments were the accuracy was achieved, the calculated uncertainties were below to 0.28% for the 235 U/ 238 U isotope ratio and 5% for the 234 U/ 238 U isotope ratio.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Development of an analysis method of minor uranium isotope ratio measurements using electron multipliers in Thermal Ionization Mass Spectrometry

Quemet

Maloubier

Dalier

et al. 2014

International Journal of Mass Spectrometry

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“…Rhenium is the preferred material in these analyses for its high work function and melting point that is well above ionization temperatures for plutonium [3]. Rhenium also has been employed as an ionization surface for a variety of other analytes [4, 5, 6, 7, 8]. The use of rhenium in other high-temperature applications has been limited by its oxidation characteristics [9].…”

Section: Introductionmentioning

confidence: 99%

Ambient aging of rhenium filaments used in thermal ionization mass spectrometry: Growth of oxo-rhenium crystallites and anti-aging strategies

Mannion

Wellons

Shick

et al. 2017

Heliyon

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Degassing is a common preparation technique for rhenium filaments used for thermal ionization mass spectrometric analysis of actinides, including plutonium. Although optimization studies regarding degassing conditions have been reported, little work has been done to characterize filament aging after degassing. In this study, the effects of filament aging after degassing were explored to determine a “shelf-life” for degassed rhenium filaments, and methods to limit filament aging were investigated. Zone-refined rhenium filaments were degassed by resistance heating under high vacuum before exposure to ambient atmosphere for up to 2 months. After degassing the nucleation and preferential growth of oxo-rhenium crystallites on the surface of polycrystalline rhenium filaments was observed by atomic force microscopy and scanning electron microscopy (SEM). Compositional analysis of the crystallites was conducted using SEM-Raman spectroscopy and SEM energy dispersive X-ray spectroscopy, and grain orientation at the metal surface was investigated by electron back-scatter diffraction mapping. Spectra collected by SEM-Raman suggest crystallites are composed primarily of perrhenic acid. The relative extent of growth and crystallite morphology were found to be grain dependent and affected by the dissolution of carbon into filaments during annealing (often referred to as carbonization or carburization). Crystallites were observed to nucleate in region specific modes and grow over time through transfer of material from the surface. Factors most likely to affect the rates of crystallite growth include rhenium substrate properties such as grain size, orientation, levels of dissolved carbon, and relative abundance of defect sites; as well as environmental factors such as length of exposure to oxygen and relative humidity. Thin (∼180 nm) hydrophobic films of poly(vinylbenzyl chloride) were found to slow the growth of oxo-rhenium crystallites on the filament surfaces and may serve as an alternative carbon source for filament carburization.

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“…[1][2][3][4][5][6][7][8] The high precision of the isotope ratio measurements is ensured by utilizing state-of-the-art instruments, such as the thermal ionization mass spectrometer (TIMS) 2-4,7-14 and the multi collector inductively coupled plasma mass spectrometer (MC-ICP-MS). [15][16][17][18] On the other hand, high precision itself does not necessarily guarantee that the measurement is accurate.…”

Section: Introductionmentioning

confidence: 99%

A Correction Method for the Peak Tailing Backgrounds for Accurate Isotope Ratio Measurements of Uranium in Ultra Trace Levels using Thermal Ionization Mass Spectrometry

Park¹,

Choi²,

Park

et al. 2011

Bulletin of the Korean Chemical Society

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A new method in thermal ionization mass spectrometry (TIMS) was developed to correct peak tailing backgrounds in the isotope ratio measurements of uranium in ultra trace levels for higher accuracy. Two different uranium standard reference materials (U005 and U030) were used to construct databases of signal intensities at mass 234 u and mass 236 u, which correspond to the two uranium minor isotopes, and signal intensity of 238 U. Correlations between peak tailing backgrounds and 238 U were obtained by least-squares regression on calculated backgrounds at mass 234 u and mass 236 u with respect to the signal intensity of 238 U followed by separation of the peak tails of the two major isotopes of uranium ( 235 U and 238 U), which enables us to obtain a master equation for peak tailing background correction on all kinds of samples. Verification of the correction method was carried out using U010 and IRMM-040a.

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Development of an improved method to perform single particle analysis by TIMS for nuclear safeguards

Cited by 38 publications

References 19 publications

Development of an analysis method of minor uranium isotope ratio measurements using electron multipliers in Thermal Ionization Mass Spectrometry

Development of an analysis method of minor uranium isotope ratio measurements using electron multipliers in Thermal Ionization Mass Spectrometry

Ambient aging of rhenium filaments used in thermal ionization mass spectrometry: Growth of oxo-rhenium crystallites and anti-aging strategies

A Correction Method for the Peak Tailing Backgrounds for Accurate Isotope Ratio Measurements of Uranium in Ultra Trace Levels using Thermal Ionization Mass Spectrometry

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