Direct uranium isotope ratio analysis of single micrometer-sized glass particles

Kappel, Stefanie; Boulyga, Sergei F.; Prohaska, Thomas

doi:10.1016/j.jenvrad.2012.03.017

Cited by 43 publications

(42 citation statements)

References 26 publications

(47 reference statements)

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“…) was identified as the main contributor to the uncertainty. This is also in good accordance to previous work [6]. However, an exception from this was observed for the RU of the 235 U/ 238 U isotope ratio with the lowest maximal 238 U signal intensity of the ‘PBP’ method.…”

Section: Resultssupporting

confidence: 92%

“…These ratios are equally important in nuclear safeguards and forensics for verifying the absence of undeclared nuclear activities. The applicability of LA-MC-ICPMS for the determination of the minor U isotopes was demonstrated in a recent study [6], as well as within the NUSIMEP-7 ILC [38]. …”

Section: Discussionmentioning

confidence: 99%

“…IRMM-184, U030-A and U500, respectively, were measured before and after the particle analyses for the determination of the external correction factor , which corrects primarily for mass bias in the case of 235 U/ 238 U measurements [6]. …”

Section: Data Treatmentmentioning

confidence: 99%

“…A promising technique for U isotope ratio analyses of single particles is laser ablation–multi-collector–inductively coupled plasma mass spectrometry (LA-MC-ICPMS) [6–11]. LA of single particles with sizes in the low micrometer range typically yields transient signals lasting less than 1 s.…”

Section: Introductionmentioning

confidence: 99%

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Evaluation strategies for isotope ratio measurements of single particles by LA-MC-ICPMS

et al. 2013

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Data evaluation is a crucial step when it comes to the determination of accurate and precise isotope ratios computed from transient signals measured by multi-collector–inductively coupled plasma mass spectrometry (MC-ICPMS) coupled to, for example, laser ablation (LA). In the present study, the applicability of different data evaluation strategies (i.e. ‘point-by-point’, ‘integration’ and ‘linear regression slope’ method) for the computation of 235U/238U isotope ratios measured in single particles by LA-MC-ICPMS was investigated. The analyzed uranium oxide particles (i.e. 9073-01-B, CRM U010 and NUSIMEP-7 test samples), having sizes down to the sub-micrometre range, are certified with respect to their 235U/238U isotopic signature, which enabled evaluation of the applied strategies with respect to precision and accuracy. The different strategies were also compared with respect to their expanded uncertainties. Even though the ‘point-by-point’ method proved to be superior, the other methods are advantageous, as they take weighted signal intensities into account. For the first time, the use of a ‘finite mixture model’ is presented for the determination of an unknown number of different U isotopic compositions of single particles present on the same planchet. The model uses an algorithm that determines the number of isotopic signatures by attributing individual data points to computed clusters. The 235U/238U isotope ratios are then determined by means of the slopes of linear regressions estimated for each cluster. The model was successfully applied for the accurate determination of different 235U/238U isotope ratios of particles deposited on the NUSIMEP-7 test samples.Electronic supplementary materialThe online version of this article (doi:10.1007/s00216-012-6674-3) contains supplementary material, which is available to authorized users.

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Section: Resultssupporting

confidence: 92%

Section: Discussionmentioning

confidence: 99%

Section: Data Treatmentmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Evaluation strategies for isotope ratio measurements of single particles by LA-MC-ICPMS

et al. 2013

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“…In ICP-MS, the mass bias per mass unit usually ranges from 0.5-1.5% for heavier masses (e.g. Pb, U) 6 and up to 25% for light masses (e.g. Li, B).…”

mentioning

confidence: 99%

Instrumental Isotopic Fractionation

Irrgeher

Prohaska

2014

Sector Field Mass Spectrometry for Elemental and Isotopic Analysis

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In mass spectrometry, the term ‘instrumental isotopic fractionation’ is recommended to describe the sum of the effects in a mass spectrometer occurring during sample introduction, ion formation, ion extraction, ion separation and ion detection leading to a difference of the measured isotope ratio from the true isotope ratio in a sample. Instrumental isotopic fractionation (IIF) describes the instrumental fractionation between nuclides of the same element resulting in erroneous results of isotope ratios. The major aspects of IIF for the different techniques (i.e. (LA)-ICP-MS, GDMS, TIMS, SIMS and IRMS) based on magnetic sector field analysers are presented. A special focus is set on the description of the major causes of IIF, the areas of occurrence in the respective instrumentations as well as the impact of IIF on the final measurement result and the related measurement uncertainty. The described techniques differ strongly in the extent of IIF, mainly due to the different ionization sources as well as vacuum conditions.

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Determination of minor isotope ratios of individual uranium particles by accelerator mass spectrometry

Gao

Zhao

et al. 2021

J Mass Spectrom

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The determination of uranium isotope ratios in uranium particle is an essential technique in the analysis of environmental samples for nuclear safeguards. At present, mass spectrometry has been widely used to measure isotope ratios of uranium particles. We developed a new analytical method for measuring minor isotope ratios of individual uranium particles directly. The technique includes single particle identification by energy dispersive X‐ray spectrometer (EDX), transfer by scanning electron microscope (SEM) combined with micromanipulator and isotope ratios analysis with accelerator mass spectrometry (AMS). The minor isotope ratios of individual uranium particles with four isotopic abundances and different sizes from certified reference materials were measured by AMS. The results show that the relative error (RE, i.e., the deviation of measured value from the certified value) of 234U/235U and 234U/236U isotope ratios was 9.0% and 19.3%, respectively, and the relative standard deviation (RSD) was within 9.9% and 16%, respectively. The minimum particle determined was about 2 μm. The method was found to be an alternative analytical means for nuclear safeguards.

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Direct uranium isotope ratio analysis of single micrometer-sized glass particles

Cited by 43 publications

References 26 publications

Evaluation strategies for isotope ratio measurements of single particles by LA-MC-ICPMS

Evaluation strategies for isotope ratio measurements of single particles by LA-MC-ICPMS

Instrumental Isotopic Fractionation

Determination of minor isotope ratios of individual uranium particles by accelerator mass spectrometry

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