ISO 8299:2019
Nuclear fuel technology — Determination of the isotopic and elemental uranium and plutonium concentrations of nuclear materials in nitric acid solutions by thermal-ionization mass spectrometry
This document specifies a method for the determination of the isotopic and elemental uranium and plutonium concentrations of nuclear materials in nitric acid solutions by thermal-ionization mass spectrometry.
The method applies to uranium and plutonium isotope composition and concentration measurement of irradiated Magnox and light water reactor fuels (boiling water reactor or pressurized water reactor), in final products at spent-fuel reprocessing plants, and in feed and products of MOX and uranium fuel fabrication. The method is applicable to other fuels, but the chemical separation and spike solution are, if necessary, adapted to suit each type of fuel.
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Foreword
1 Scope
2 Normative references
3 Terms and definitions
4 Principle
5 Reference materials and reagents
5.1 Spikes and reference materials
5.2 Other chemical reagents
5.3 Resin, applicable for separation/purification of Pu and U
5.3.1 General
5.3.2 Preparation of resin
6 Apparatus
7 Apparatus for mass spectrometry
8 Sample preparation
8.1 Subsampling and spiking
8.1.1 Pellet or powder samples
8.1.2 Concentrated nuclear fuel solution samples (such as reprocessing solution)
8.1.3 Plutonium nitrate solution samples (such as product solution from a reprocessing plant)
8.1.4 Dried nitrate samples
8.2 Chemical valency adjustment
8.2.1 Valence adjustment with ferrous solution
8.2.2 Valence adjustment with hydrogen peroxide
8.3 Sample separation/purification
8.3.1 Ion exchange with anion-exchange resin
8.3.2 Purification with extraction separation resins (see 5.3.1.2)
8.4 Replicate treatments
9 Filaments preparation
9.1 Degassing of filaments
9.2 Sample loading
9.2.1 Normal sample loading
9.2.2 Graphite loading technique
9.2.3 Resin-bead loading on single filaments for Pu samples
9.3 Filament mounting (filament assemblies preparation)
10 Instrument calibration
10.1 Mass calibration
10.2 Gain calibration for Faraday multi-detectors
10.3 Faraday detector calibration
10.4 Mass discrimination calibration
11 Isotopic mass spectrometric measurements
11.1 Total evaporation measurements using a single or double filament assembly and a multi-Faraday collector system
11.2 Bias correction method using a double filament assembly and a multi-Faraday collector system
12 Calculation of the results
12.1 Calculation of ion current intensities
12.2 Calculation of mean, weighted mean and standard deviation on a set of ratios xi, (i = 1…N)
12.3 Mass discrimination correction
12.4 Calculation of the atomic percent abundance Ai
12.5 Calculation of the isotopic mass percent Wj
12.6 Calculation of concentration
12.7 Isotope decay correction
13 Blanks
14 Quality control
15 Measurement uncertainty
15.1 Elemental assay
15.2 Isotopic analysis
16 Interferences
Annex A (normative) Preparation and standardization of spike solutions
Bibliography
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Foreword
1 Scope
2 Normative references
3 Terms and definitions
4 Principle
5 Reference materials and reagents
5.1 Spikes and reference materials
5.2 Other chemical reagents
5.3 Resin, applicable for separation/purification of Pu and U
5.3.1 General
5.3.2 Preparation of resin
6 Apparatus
7 Apparatus for mass spectrometry
8 Sample preparation
8.1 Subsampling and spiking
8.1.1 Pellet or powder samples
8.1.2 Concentrated nuclear fuel solution samples (such as reprocessing solution)
8.1.3 Plutonium nitrate solution samples (such as product solution from a reprocessing plant)
8.1.4 Dried nitrate samples
8.2 Chemical valency adjustment
8.2.1 Valence adjustment with ferrous solution
8.2.2 Valence adjustment with hydrogen peroxide
8.3 Sample separation/purification
8.3.1 Ion exchange with anion-exchange resin
8.3.2 Purification with extraction separation resins (see 5.3.1.2)
8.4 Replicate treatments
9 Filaments preparation
9.1 Degassing of filaments
9.2 Sample loading
9.2.1 Normal sample loading
9.2.2 Graphite loading technique
9.2.3 Resin-bead loading on single filaments for Pu samples
9.3 Filament mounting (filament assemblies preparation)
10 Instrument calibration
10.1 Mass calibration
10.2 Gain calibration for Faraday multi-detectors
10.3 Faraday detector calibration
10.4 Mass discrimination calibration
11 Isotopic mass spectrometric measurements
11.1 Total evaporation measurements using a single or double filament assembly and a multi-Faraday collector system
11.2 Bias correction method using a double filament assembly and a multi-Faraday collector system
12 Calculation of the results
12.1 Calculation of ion current intensities
12.2 Calculation of mean, weighted mean and standard deviation on a set of ratios xi, (i = 1…N)
12.3 Mass discrimination correction
12.4 Calculation of the atomic percent abundance Ai
12.5 Calculation of the isotopic mass percent Wj
12.6 Calculation of concentration
12.7 Isotope decay correction
13 Blanks
14 Quality control
15 Measurement uncertainty
15.1 Elemental assay
15.2 Isotopic analysis
16 Interferences
Annex A (normative) Preparation and standardization of spike solutions
Bibliography