ISO 15366-2:2014 PDF

Nuclear fuel technology — Chemical separation and purification of uranium and plutonium in nitric acid solutions for isotopic and isotopic dilution analysis by solvent extraction chromatography — Part 2: Samples containing plutonium and uranium in the nanogram range and below

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Title (English):

ISO 15366-2:2014

Document status:: Active
Format:: Electronic (PDF)
Number of pages:: 10
Publication date:: June 17, 2014
Edition:: ISO IS 15366 edition 1 version 1
ICS:: 27.120.30

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Description (English):

ISO 15366-2:2014 describes procedures to chemically separate and purify uranium and plutonium in dissolved solutions of irradiated light water reactor fuels and in samples of high active liquid waste of spent fuel reprocessing plants, prior to their isotopic analysis by e.g. mass spectrometric method or alpha spectrometry. ISO 15366-2:2014 describes a slightly different separation technique from ISO 15366-1, based on the same chemistry, using smaller columns, different support material and special purification steps, applicable to samples containing plutonium and uranium amounts in the nanogram range and below. The detection limits were found to be 500 pg plutonium and 500 pg uranium.

Technical details

Technical committee: ISO/TC 85/SC 5 - Nuclear installations, processes and technologies
SKU: ISO 15366-2:2014

Abstract

Overview

ISO 15366-2:2014 - part of the ISO 15366 series on nuclear fuel technology - specifies a chemical separation and purification method for uranium and plutonium in nitric acid solutions prior to isotopic or isotope-dilution analysis (e.g., mass spectrometry or alpha spectrometry). This Part 2 procedure is tailored for extremely small analyte amounts (nanogram range and below), using solvent extraction chromatography on disposable mini-columns with TOPO-coated supports. The method is applicable to dissolved irradiated light water reactor (LWR) fuels and high active liquid waste from spent fuel reprocessing. Reported detection limits: 500 pg plutonium and 500 pg uranium.

Key technical topics and requirements

Separation principle: Extraction chromatography using tri-n-octylphosphine-oxide (TOPO) coated on polyethylene or silica supports to retain Pu(IV) and U(VI) from 3 mol·L−1 HNO3.
Valency control: Redox valency cycle (Fe(II) reduction, NaNO2 re-oxidation) to ensure plutonium is in the tetravalent state before loading.
Elution strategy:
- Plutonium eluted after reduction to Pu(III) (ascorbic acid/formic acid eluent).
- Uranium eluted with ammonium carbamate and optionally purified further by anion exchange or fuming with 14 mol·L−1 HNO3.
Mini-columns and support: Smaller disposable columns and specific support materials (polyethylene powder or silica gel) and column preparation procedures are detailed in the annex.
Analytical performance: Flow-rate control for favourable kinetics (gravity flow ≤ 0.4 mL·min−1) and parallel blanks/controls to monitor cross-contamination and separation efficiency.
Quality & safety: Use of suprapure reagents, laminar-flow clean conditions (shielded glove box or fume hood), and radioactive waste disposal of used columns.

Practical applications and users

Radiochemistry and nuclear fuel laboratories performing isotopic analysis of uranium and plutonium at ultra-trace levels.
Spent-fuel reprocessing plants analyzing dissolved samples and high active liquid waste.
Safeguards and forensic laboratories requiring reliable chemical purification prior to mass spectrometry (ISO 8299) or alpha spectrometry (ISO 11483).
Method supports ultra-trace isotopic dilution workflows and contamination-controlled sample prep for nuclear safeguards and material accountancy.

Related standards

ISO 15366-1 (Part 1: procedures for larger sample amounts - same chemistry, different column/support)
ISO 8299 (mass spectrometric isotopic analysis guidance)
ISO 11483 (alpha spectrometry for plutonium/uranium)

Keywords: ISO 15366-2:2014, nuclear fuel technology, chemical separation, purification, uranium, plutonium, nitric acid, solvent extraction chromatography, TOPO, mini-column, isotopic analysis, mass spectrometry, nanogram range.

Related standards

Standards mentioned in the description

Abstract

Overview

Key technical topics and requirements

Separation principle: Extraction chromatography using tri-n-octylphosphine-oxide (TOPO) coated on polyethylene or silica supports to retain Pu(IV) and U(VI) from 3 mol·L−1 HNO3.
Valency control: Redox valency cycle (Fe(II) reduction, NaNO2 re-oxidation) to ensure plutonium is in the tetravalent state before loading.
Elution strategy:
- Plutonium eluted after reduction to Pu(III) (ascorbic acid/formic acid eluent).
- Uranium eluted with ammonium carbamate and optionally purified further by anion exchange or fuming with 14 mol·L−1 HNO3.
Mini-columns and support: Smaller disposable columns and specific support materials (polyethylene powder or silica gel) and column preparation procedures are detailed in the annex.
Analytical performance: Flow-rate control for favourable kinetics (gravity flow ≤ 0.4 mL·min−1) and parallel blanks/controls to monitor cross-contamination and separation efficiency.
Quality & safety: Use of suprapure reagents, laminar-flow clean conditions (shielded glove box or fume hood), and radioactive waste disposal of used columns.

Practical applications and users

Radiochemistry and nuclear fuel laboratories performing isotopic analysis of uranium and plutonium at ultra-trace levels.
Spent-fuel reprocessing plants analyzing dissolved samples and high active liquid waste.
Safeguards and forensic laboratories requiring reliable chemical purification prior to mass spectrometry (ISO 8299) or alpha spectrometry (ISO 11483).
Method supports ultra-trace isotopic dilution workflows and contamination-controlled sample prep for nuclear safeguards and material accountancy.

Related standards

ISO 15366-1 (Part 1: procedures for larger sample amounts - same chemistry, different column/support)
ISO 8299 (mass spectrometric isotopic analysis guidance)
ISO 11483 (alpha spectrometry for plutonium/uranium)

ISO 15366-2:2014 PDF

Technical details

Abstract

Overview

Key technical topics and requirements

Practical applications and users

Related standards

Related standards

Abstract

Overview

Key technical topics and requirements

Practical applications and users

Related standards

Related standards

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