Development of a microanalytical energy dispersive X-ray fluorescence method for compositional characterization of (U, Pu)O2 samples

Dhara, Sangita; Kumar, Sachin; Jayachandran, Kavitha; Kamat, J. V.; Kumar, Ashok; Radhakrishna, J.; Misra, Nilanjal

doi:10.1016/j.sab.2017.03.006

Cited by 12 publications

(3 citation statements)

References 17 publications

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“…A large number of destructive and nondestructive analytical techniques − are available in the arsenal of an analyst for determination of U and Pu in nuclear fuel samples, but redox titrimetric methods offer several advantages over other techniques if cost, time, precision, accuracy, space, and the analyst’s effort are all taken into account. Most of the methods involve expensive equipment, are time-consuming, and are not capable of giving results with accuracy and precision better than 1% .…”

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confidence: 99%

Poly(3,4-ethylenedioxythiophene)–Poly(styrenesulfonate)-Coated Glassy-Carbon Electrode for Simultaneous Voltammetric Determination of Uranium and Plutonium in Fast-Breeder-Test-Reactor Fuel

et al. 2018

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Uranium (U) and plutonium (Pu) contents in nuclear materials must be maintained to a definite level in order to get the desired performance of the fuel inside the reactor. Therefore, high accuracy and precision is an essential criterion for the determination of U and Pu. We already reported the voltammetric determination of Pu in the presence of U in fast-breeder-test-reactor (FBTR) fuel samples, but interfacial, coupled chemical reactions between U(IV) and Pu(IV) enhance the peak-current density of U(VI) reduction and thus make voltammetry unsuitable for the quantitative determination of U in the presence of Pu. Thus, developing a voltammetric method for the simultaneous determination of U and Pu is highly challenging. Herein, we report the simultaneous voltammetric determination of U and Pu in 1 M sulfuric acid (HSO) on a poly(3,4-ethylenedioxythiophene) (PEDOT)-poly(styrenesulfonate) (PSS)-modified glassy-carbon (GC) electrode (PEDOT-PSS/GC). The modified electrode shows enhanced performance compared with bare GC electrodes. The peak-current density for U(VI) reduction is enhanced in the presence of Pu(IV), but it attains saturation when [Pu]/[U] in solution is maintained ≥2. Hence, under these circumstances, the variation of Pu concentration no longer influences the U(VI)-reduction peak, and thus the quantitative determination of U in the presence of Pu is possible. No interference is observed from commonly encountered impurities present in FBTR fuel samples. This method shows accuracy and precision comparable to those of the biamperometry method. High robustness, fast analysis, simultaneous determination, reduced radiation exposure to the analyst, and ease of recovery of U and Pu from analytical waste makes it a suitable candidate to substitute the presently applied biamperometry method.

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Poly(3,4-ethylenedioxythiophene)–Poly(styrenesulfonate)-Coated Glassy-Carbon Electrode for Simultaneous Voltammetric Determination of Uranium and Plutonium in Fast-Breeder-Test-Reactor Fuel

et al. 2018

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“…It is being routinely used for the determination of elemental composition in environmental, biological and industrial samples. [8][9][10] The XRF technique has many advantages, like being fast and simple. X-ray spectra are less complex compared to other atomic spectra, i.e.…”

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Universal EDXRF Method for Multi-elemental Determinations Using Fused Bead Specimens

2019

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A systematic study on the EDXRF determination of multi-elements using fusion bead specimens and a universal calibration procedure was carried out. Beads of multi-elements were prepared by mixing MERCK multi-elemental standard solutions with the fusion flux. The elemental X-ray lines of K, Ca, Ba, Cr, Mn, Fe, Co, Ni, Cu and Zn were excited using a Ge secondary target and that of Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Pb, Bi and Sr using a Rh primary target. The relative sensitivities of the elemental X-ray lines obtained using different excitation modes were calculated using a single bead. Using this relative sensitivity, the concentration of elements in other bead samples was determined. The average precision obtained was 3% (1 s) and the average deviation from expected values, calculated on the basis of sample preparation, was 6%. In order to further countercheck the validity of this methodology, a standard soil sample received from IAEA was analyzed.

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“…In most of the cases, the ED-XRF quantification is only performed by semiquantitative methods based on Fundamental Parameters equations . There are other works in which different empirical calibration methodologies have been developed for elemental quantification in different matrixes, such as vegetables and rice, or in totally different samples such as nuclear fuels to quantify U and P . In the field of Cultural Heritage, the characterization of building materials is commonly carried out by means of ED-XRF following an in situ qualitative strategy. − There is an study where an empirical calibration based on standards was developed for the characterization of calcareous building materials with high Cultural Heritage value .…”

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Usefulness of a Dual Macro- and Micro-Energy-Dispersive X-Ray Fluorescence Spectrometer to Develop Quantitative Methodologies for Historic Mortar and Related Materials Characterization

et al. 2018

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Wavelength dispersive X-ray fluorescence (WD-XRF) spectrometry has been widely used for elemental quantification of mortars and cements. In this kind of instrument, samples are usually prepared as pellets or fused beads and the whole volume of sample is measured at once. In this work, the usefulness of a dual energy dispersive X-ray fluorescence spectrometer (ED-XRF), working at two lateral resolutions (1 mm and 25 μm) for macro and microanalysis respectively, to develop quantitative methods for the elemental characterization of mortars and concretes is demonstrated. A crucial step before developing any quantitative method with this kind of spectrometers is to verify the homogeneity of the standards at these two lateral resolutions. This new ED-XRF quantitative method also demonstrated the importance of matrix effects in the accuracy of the results being necessary to use Certified Reference Materials as standards. The results obtained with the ED-XRF quantitative method were compared with the ones obtained with two WD-XRF quantitative methods employing two different sample preparation strategies (pellets and fused beads). The selected ED-XRF and both WD-XRF quantitative methods were applied to the analysis of real mortars. The accuracy of the ED-XRF results turn out to be similar to the one achieved by WD-XRF, except for the lightest elements (Na and Mg). The results described in this work proved that μ-ED-XRF spectrometers can be used not only for acquiring high resolution elemental map distributions, but also to perform accurate quantitative studies avoiding the use of more sophisticated WD-XRF systems or the acid extraction/alkaline fusion required as destructive pretreatment in Inductively coupled plasma mass spectrometry based procedures.

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Development of a microanalytical energy dispersive X-ray fluorescence method for compositional characterization of (U, Pu)O2 samples

Cited by 12 publications

References 17 publications

Poly(3,4-ethylenedioxythiophene)–Poly(styrenesulfonate)-Coated Glassy-Carbon Electrode for Simultaneous Voltammetric Determination of Uranium and Plutonium in Fast-Breeder-Test-Reactor Fuel

Poly(3,4-ethylenedioxythiophene)–Poly(styrenesulfonate)-Coated Glassy-Carbon Electrode for Simultaneous Voltammetric Determination of Uranium and Plutonium in Fast-Breeder-Test-Reactor Fuel

Universal EDXRF Method for Multi-elemental Determinations Using Fused Bead Specimens

Usefulness of a Dual Macro- and Micro-Energy-Dispersive X-Ray Fluorescence Spectrometer to Develop Quantitative Methodologies for Historic Mortar and Related Materials Characterization

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