ASTM C1432-03

Standard Test Method for Determination of Impurities in Plutonium: Acid Dissolution, Ion Exchange Matrix Separation, and Inductively Coupled Plasma-Atomic Emission Spectroscopic (ICP/AES) Analysis

SCOPE
1.1 This test method covers the determination of 25 elements in plutonium (Pu) materials. The Pu is dissolved in acid, the Pu matrix is separated from the target impurities by an ion exchange separation, and the concentrations of the impurities are determined by inductively coupled plasma-atomic emission spectroscopy (ICP-AES).
1.2 This test method is specific for the determination of impurities in 8 M HNO3 solutions. Impurities in other plutonium materials, including plutonium oxide samples, may be determined if they are appropriately dissolved (see Practice C 1168) and converted to 8 M HNO3 solutions.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 09-Feb-2003
• ICS: 27.120.30 - Fissile materials and nuclear fuel technology
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

Relations

• Replaces: ASTM C1432-99 - Standard Test Method for Determination of Impurities in Plutonium: Acid Dissolution, Ion Exchange Matrix Separation, and Inductively Coupled Plasma-Atomic Emission Spectroscopic (ICP/AES) Analysis
• Effective Date: 10-Feb-2003
• Replaced By: ASTM C1432-03(2008) - Standard Test Method for Determination of Impurities in Plutonium: Acid Dissolution, Ion Exchange Matrix Separation, and Inductively Coupled Plasma-Atomic Emission Spectroscopic (ICP/AES) Analysis
• Effective Date: 01-Dec-2008
• Referred By: ASTM C697-16 - Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium Dioxide Powders and Pellets
• Effective Date: 10-Feb-2003
• Referred By: ASTM C1647-20 - Standard Practice for Removal of Uranium or Plutonium, or both, for Impurity Assay in Uranium or Plutonium Materials
• Effective Date: 10-Feb-2003
• Referred By: ASTM C1637-21 - Standard Test Method for Determination of Impurities in Plutonium Materials—Acid Digestion and Inductively Coupled Plasma-Mass Spectroscopy (ICP-MS) Analysis
• Effective Date: 10-Feb-2003
• Referred By: ASTM C698-16 - Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Mixed Oxides ((U, Pu)O<inf>2</inf>)
• Effective Date: 10-Feb-2003
• Referred By: ASTM C759-18 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Plutonium Nitrate Solutions
• Effective Date: 10-Feb-2003
• Referred By: ASTM C758-18 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Plutonium Metal
• Effective Date: 10-Feb-2003

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: C 1432 – 03
Standard Test Method for
Determination of Impurities in Plutonium: Acid Dissolution,
Ion Exchange Matrix Separation, and Inductively Coupled
1
Plasma-Atomic Emission Spectroscopic (ICP/AES) Analysis
This standard is issued under the fixed designation C 1432; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 0.03 M hydrofluoric acid (HF) is added to the dissolved
plutonium to oxidize the plutonium to the Pu (IV) state. The
1.1 This test method covers the determination of 25 ele-
sample solution is loaded onto a nitrate anion exchange resin
ments in plutonium (Pu) materials.The Pu is dissolved in acid,
and eluted with8MHNO /0.006 M HF.The rinses contain the
the Pu matrix is separated from the target impurities by an ion 3
target metallic impurities and less than 15 µg/mL Pu. The
exchange separation, and the concentrations of the impurities
plutonium is stripped from the anion exchange resin with 0.1
aredeterminedbyinductivelycoupledplasma-atomicemission
M HCl. The rinses containing the metallic impurities are
spectroscopy (ICP-AES).
analyzed by ICP-AES.
1.2 This test method is specific for the determination of
impurities in8MHNO solutions. Impurities in other pluto-
3
4. Significance and Use
nium materials, including plutonium oxide samples, may be
4.1 This test method can be used on plutonium matrices in
determined if they are appropriately dissolved (see Practice
nitrate solutions.
C 1168) and converted to8MHNO solutions.
3
4.2 This test method has been validated for all elements
1.3 This standard does not purport to address all of the
listed in Test Methods C 757 except sulfur (S) and tantalum
safety concerns, if any, associated with its use. It is the
(Ta).
responsibility of the user of this standard to establish appro-
4.3 This test method has been validated for all of the cation
priate safety and health practices and determine the applica-
elements measured in Table 1. Phosphorus (P) requires a
bility of regulatory limitations prior to use.
vacuum or an inert gas purged optical path instrument.
2. Referenced Documents
5. Interferences
2.1 ASTM Standards:
5.1 Plutonium concentrations of less than 50 µg/mL in the
C 757 Specification for Nuclear-Grade Plutonium Dioxide
2 final aqueous phase do not significantly affect the analytical
Powder, Sinterable
results for most elements. Interference studies should be made
C 758 Test Methods for Chemical, Mass Spectrometric,
todeterminethedegreeofPuandotherelementalinterferences
Spectrochemical, Nuclear, and Radiochemical Analysis of
2 onthetargetanalytes;backgroundandinterelementcorrections
Nuclear-Grade Plutonium Metal
may be required.
C 759 Test Methods for Chemical, Mass Spectrometric,
Spectrochemical, Nuclear, and Radiochemical Analysis of
6. Apparatus
2
Nuclear-Grade Plutonium Nitrate Solutions
6.1 An ICP-AES equipped with a Charge Injection Device
C 1168 Practice for Preparation and Dissolution of Pluto-
(CID) detector or an ICP-AES with a spectral bandpass of 0.05
2
nium Materials for Analysis
3 nm or less is required to provide the necessary spectral
D 1193 Specification for Reagent Water
4
resolution. The spectrometer may be either a simultaneous
3. Summary of Test Method multielement or a sequential spectrometer. The spectrometer
may be either an inert gas-path or vacuum instrument; the
3.1 A sample of plutonium metal is dissolved in a small
appropriate spectral lines should be selected for each specific
volume of 6 M hydrochloric acid (HCl). Then, 10 M (HNO )/
3
instrument. Either an analog or digital readout system may be
used.
1
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
Test.
Current edition approved Feb. 10, 2003. Published April 2003. Originally
4
approved in 1999. Last previous edition approved in 1999 as C 1432 – 99. A Thermo Jarrell Ash PolyScan Iris spectrometer (Thermo Electron Spectros-
2
Annual Book of ASTM Standards, Vol 12.01. copy, Franklin, MA), or an Applied Research Laboratories 3580 ICP-AES instru-
3
Annual Book of ASTM Standards, Vol 11.01. ment (Dearborn, MI) have been found to be acceptable.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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C1432–03
TABLE 1 Percent Recovery and Repeatability Standard Deviation for Sixteen Spiked Samples
Wavelength/Order Actual Conc Mean Conc Average R.S.D.
Element
(nm) (µg/mL) (µg/mL) (%R) (%)
Aluminum Al 396.152 {67} 2.5 2.4 95 6
...