Inter-Element Interference Studies in the Determination of Trace Amounts of Plutonium by Inductively Coupled Plasma - Atomic Emission Spectrometry

Kulkarni, Madhuri J.; Thulasidas, S. K.; Goyal, Neelam; Page, A.G.; Sastry, M. D.

doi:10.1080/00032719008052552

Cited by 7 publications

(10 citation statements)

References 5 publications

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“…Already at a 10-fold excess of either U or Th, the Pu emission signal at l ¼ 300.06 nm yielded distinctly elevated Pu concentrations. 9 The Pu emission signal at l ¼ 453.62 nm, in turn, was found to be free from these spectral interferences. 9 More recently, the spectral performance of the two above mentioned Pu emission wavelengths was tested using a high resolution (HR-)ICP-OES instrument.…”

Section: Introductionmentioning

confidence: 97%

“…9 The Pu emission signal at l ¼ 453.62 nm, in turn, was found to be free from these spectral interferences. 9 More recently, the spectral performance of the two above mentioned Pu emission wavelengths was tested using a high resolution (HR-)ICP-OES instrument. 10 Employing experimentally established inter-elemental correction factors, the potential impact of a 10-fold excess of U, Th and selected rare earth elements was limited to an increase of 8% with respect to the target Pu concentration.…”

Section: Introductionmentioning

confidence: 97%

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Improved plutonium concentration analysis in specimens originating from the nuclear fuel cycle using high resolution ICP-OES

Krachler

Alvarez‐Sarandes

2015

J. Anal. At. Spectrom.

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An accurate and robust ICP-OES procedure for the reliable determination of the Pu concentration in radioactive samples was developed and subsequently cross-validated using ICP-MS. Method optimisation focused on identifying Pu emission wavelengths that are spectrally not interfered by the occurrence of emission signals of concomitant elements (e.g. Am, Np, Th, and U) in the analyte solution, thereby avoiding an otherwise necessary chemical separation of Pu from the matrix elements. To this end, a total of 43 Pu emission wavelengths were tested for their selectivity and sensitivity. The signal to background ratio of the 27 most prominent Pu emission lines ranged from $2 to 20, while relative sensitivities varied only within a factor of two. Peak widths of ICP-OES Pu signals extended from $5 pm to $11 pm, with the majority remaining <6 pm. Using a desolvating nebuliser, instrumental detection limits (LOD) were lowered by an order of magnitude compared to all previous studies. Among the finally selected, seven worthwhile Pu emission wavelengths, LODs of 2.3 mg L À1 , 3.1 mg L À1 , and 3.2 mg L À1 were obtained at l ¼ 299.649 nm, l ¼ 299.409 nm, and l ¼ 297.251 nm. Applying external calibration, several radioactive samples originating from pyrochemical separation experiments were analysed for their Pu concentration. Typical relative standard deviations of replicate Pu measurements amounted to $1% to 2%. The complementary employment of the standard addition approach confirmed the accuracy of this data as well did comparative in-house sector field ICP-MS analysis. Preliminary experiments with spent fuel solutions revealed promising Pu data highlighting the potential of ICP-OES for reliable Pu analysis in the nuclear field.

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Section: Introductionmentioning

confidence: 97%

Section: Introductionmentioning

confidence: 97%

Improved plutonium concentration analysis in specimens originating from the nuclear fuel cycle using high resolution ICP-OES

Krachler

Alvarez‐Sarandes

2015

J. Anal. At. Spectrom.

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“…In order to decrease the radiation burden for personnel and to ensure appropriate functioning of the analytical instrumentation, the samples taken from PUREX are normally diluted multiple times. The methods currently in use for plutonium quantification in process streams are mainly inductively coupled plasma atomic emission spectrometry (ICP-AES) [2] and mass spectrometry (ICP-MS) [3]. While providing perfect sensitivity and selectivity, these methods are rather time-consuming and can hardly be implemented in on-line mode.…”

Section: Introductionmentioning

confidence: 99%

Plutonium (IV) Quantification in Technologically Relevant Media Using Potentiometric Sensor Array

Savosina

Agafonova-Moroz

Yaroshenko

et al. 2020

Sensors

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The quantification of plutonium in technological streams during spent nuclear fuel (SNF) reprocessing is an important practical task that has to be solved to ensure the safety of the process. Currently applied methods are tedious, time-consuming and can hardly be implemented in on-line mode. A fast and simple quantitative plutonium (IV) analysis using a potentiometric sensor array based on extracting agents is suggested in this study. The response of the set of specially designed PVC-plasticized membrane sensors can be related to plutonium content in solutions simulating real SNF-reprocessing media through multivariate regression modeling, providing 30% higher precision of plutonium quantification than optical spectroscopy.

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“…Of these, ICP-AES has been widely selected as the technique of choice to perform the analysis of metallic constituents owing to its simultaneous measurement capability, wide dynamic analytical range, high sensitivity and relative freedom from matrix interferences [3,4]. A number of studies have been reported on the application of ICP-AES to the determination of the trace or minor metal constituents in nuclear materials such as uranium, plutonium, oxides/carbides of uranium and plutonium, high-level radioactive waste glass and simulated nuclear waste solutions after the prior chemical separation of the major matrix [5][6][7][8][9][10][11][12].…”

Section: Introductionmentioning

confidence: 99%

Determination of In and Ga in plutonium oxide matrix by ICP-AES after chemical separation

et al. 2011

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An analytical method was developed for the determination of indium and gallium in plutonium samples. A solvent extraction technique was employed by using 30% TBP in CCl 4 for the quantitative separation of plutonium from the sample solution and subsequent determination by radial inductively coupled plasma atomic emission spectrometry (ICP-AES). The quantitative recovery of In and Ga in the separated samples was confirmed from radiometric/tracer studies. Recording of spectral profile at 303.396 nm for In and 403.298 nm for Ga has clearly indicated that the determination of Ga and In at lower concentrations will be affected by the presence of significant amounts of residual Pu in the aqueous phase due to spectral interference. These elements can be determined from ppm to % levels by proper dilution with 1 M HNO 3 and appropriate (100 mg and 1 g) sample size. The analytical range obtained for Ga and In was 0.1-1000 µg/mL and 0.05-500 µg/mL respectively by ICP-AES. Synthetic samples of plutonium containing indium and gallium in the range of 50-20 000 ppm were analyzed.

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Inter-Element Interference Studies in the Determination of Trace Amounts of Plutonium by Inductively Coupled Plasma - Atomic Emission Spectrometry

Cited by 7 publications

References 5 publications

Improved plutonium concentration analysis in specimens originating from the nuclear fuel cycle using high resolution ICP-OES

Improved plutonium concentration analysis in specimens originating from the nuclear fuel cycle using high resolution ICP-OES

Plutonium (IV) Quantification in Technologically Relevant Media Using Potentiometric Sensor Array

Determination of In and Ga in plutonium oxide matrix by ICP-AES after chemical separation

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