Determination of iron in nuclear grade zirconium oxide by x-ray fluorescence spectrometry using an internal intensity reference

Krishna, Gautam; Ravindra, H.R.; Gopalan, B.; Syamsunder, S.

doi:10.1016/0003-2670(95)00061-4

Cited by 12 publications

(5 citation statements)

References 16 publications

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“…Natural zirconium comprises five stable isotopes (with mass numbers 90, 91, 92, 94, and 96), which could be considered a challenging case for LAMIS. Isotopic analysis of zirconium is important in nuclear science and forensics. , For example, zirconium, in the form of zircaloys, is used as a cladding material for nuclear reactor fuels because of its low neutron-capture cross-section. , In nuclear forensics, because the maxima of the yields of fission products from thermal neutron-induced fission of 235 U and 239 Pu are found in the ranges of mass numbers 90–100 and 95–105, respectively, , Zr isotopic analysis allows the determination of the contribution of fissions from these two radionuclides …”

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confidence: 99%

Femtosecond Laser Ablation Molecular Isotopic Spectrometry for Zirconium Isotope Analysis

et al. 2015

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Laser ablation molecular isotopic spectrometry (LAMIS) for rapid isotopic analysis of zirconium at atmospheric pressure was studied with a femtosecond-laser system operated under high repetition rate (1 kHz) and low pulse energy (160 μJ). The temporal evolution of zirconium neutral-atomic and ionic lines, as well as zirconium oxide molecular bands, were studied. Six molecular bands, belonging to the d(3)Δ-a(3)Δ (i.e., the α system) and E(1)Σ(+)-X(1)Σ(+) transitions, were observed with appreciable isotopic shifts. The assignments of the isotopic bandheads were first based on theoretical predictions of the band origins and the associated isotopic shifts of various dipole-allowed ZrO electronic transitions, followed by an experimental confirmation with a (94)Zr-enriched ZrO2 sample. In this work, the α(0,1) band from the d(3)Δ3-a(3)Δ3 subsystem was utilized for Zr isotope analysis based on a compromise between the magnitude of isotopic shifts in emission wavelengths, emission strengths, signal-to-background ratios, and spectral interferences. The analysis was performed in a standardless calibration approach; the isotopic information was extracted from the experimentally measured molecular spectra through theoretical spectral fitting. The results demonstrate the feasibility to obtain isotopic information for a spectrally complicated element like zirconium, without the need to use isotopically labeled calibration standards. The availability of comprehensive molecular constants will further improve the analytical accuracy of this standardless calibration approach.

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confidence: 99%

Femtosecond Laser Ablation Molecular Isotopic Spectrometry for Zirconium Isotope Analysis

et al. 2015

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“…This is mainly due to its many unique characteristics such as low thermal neutron absorption cross section (0.18barn), have good mechanical properties and corrosion resistance. In order to become suitable as nuclear material, one of the criteria is to conform to trace metal impurities as per the specifications laid down by fuel designer [16][17][18][19][20][21][22] . Using D.C. arc-AES technique based on carrier-distillation method, we have reported determination of trace common metallic elements in Zr matrix without chemical separation [23][24][25] .…”

Section: Introductionmentioning

confidence: 99%

Determination of Spectral Interference of Zirconium On Some Critical Analytes By CCD Based Inductively Coupled Plasma – Atomic Emission Spectrometric Technique

Adya¹

2023

J. ISAS

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Inductively coupled plasma atomic emission spectrometry (ICP-AES) is multi elemental, rapid, simple technique for the determination of trace level analytes, but suffers from spectral interference of matrix elements like U, Pu, Zr, Th etc. originating from their line rich emission spectra causing detrimental effect on the determination of analyte elements at trace levels in the nuclear materials. This can be overcome by using carrier distillation technique wherein carrier selectively distills analytes into D.C. arc-AES leaving behind the matrix into the electrode crater, being physical separation of the matrix. This technique is generally used to determine common metallic elements. For the determination of rare earth elements being refractory in nature like U, Th, etc. at sub-ppm levels, carrier distillation technique cannot be used. Hence, chemical separation of the matrix followed by their determination by AES technique is the usual practice, which may involve contamination of the sample during pre treatment. Charged Coupled Detector (CCD) with flexibility of the choices of additional analytical lines of analytes, e.g., for Ce, 413.38 nm, 413.765 nm, 418.66 nm and 448.691 nm lines were selected and studied which may have lesser interference from Zr, facilitating direct determination of analytes at trace levels without any type of separation. Present paper involves the detailed study of spectral interference of zirconium on different analytical lines of Ba, Bi, Ce, Er, La, Lu, Mo, Nd, Pr, Sb, Sc, Ti, Tl, U, W, Y, Yb to select suitable analytical lines based on contributions of Zr on each analytical line, detection limits and sensitivity. Zirconium being major matrix, it’s determination by ICP-AES was performed by identifying four suitable analytical lines, namely, 339.198 nm, 343.823 nm, 257.139 nm and 272.262 nm including monitoring of sensitivity, detection limits etc. Based on these interference studies, it is possible to determine 17 analytes under investigations in Zr matrix on ppm basis by ICP AES using their appropriate analytical lines without any chemical/physical separation.

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“…[14] The ability to perform not just elemental analysis but also isotopic analysis at a distance is important for some remote sensing applications, including nuclear non-proliferation and forensics. [15,16] Despite all the research on LIBS, the ability to provide isotopic information is limited to only a few studies (e.g., H, Li and U). [17][18][19] The recent development of Laser Ablation Molecular Isotopic Spectrometry (LAMIS) introduced a new way for direct isotopic analysis at atmospheric pressure.…”

Section: Introductionmentioning

confidence: 99%

Femtosecond filament-laser ablation molecular isotopic spectrometry

Hou

Chan

Mao

et al. 2015

Spectrochimica Acta Part B: Atomic Spectroscopy

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A new remote sensing technology for real-time isotopic analysis is introduced: Femtosecond Filament-Induced Laser Ablation Molecular Isotopic Spectrometry (F 2-LAMIS). The technique combines femtosecond (fs) laser filamentation and ablationbased molecular isotopic spectroscopy, thereby enabling isotopic analysis of samples at a distance, in ambient air and at ambient pressure conditions. Isotopic analysis of zirconium (Zr) samples by F 2-LAMIS is demonstrated, and the molecular and atomic emission intensity, and properties of the filament-induced plasma generated at different filament propagation distances were investigated. Spectral fitting of F 2-LAMIS spectra enabled semi-quantitative isotopic analysis without the use of calibration standards, which was independent of the filament propagation distance for the studied range. This technology provides new capabilities for direct isotopic ratio measurements at remote distances.

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Determination of iron in nuclear grade zirconium oxide by x-ray fluorescence spectrometry using an internal intensity reference

Cited by 12 publications

References 16 publications

Femtosecond Laser Ablation Molecular Isotopic Spectrometry for Zirconium Isotope Analysis

Femtosecond Laser Ablation Molecular Isotopic Spectrometry for Zirconium Isotope Analysis

Determination of Spectral Interference of Zirconium On Some Critical Analytes By CCD Based Inductively Coupled Plasma – Atomic Emission Spectrometric Technique

Femtosecond filament-laser ablation molecular isotopic spectrometry

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