ASTM C1432-23
(Test Method)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
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
SIGNIFICANCE AND USE
5.1 This test method can be used on plutonium matrices in nitrate solutions.
5.2 This test method has been validated for all elements listed in Test Methods C757 except sulfur (S) and tantalum (Ta).
5.3 This test method has been validated for all of the cation elements measured in Table 1. Phosphorus (P) requires a vacuum or an inert gas purged optical path instrument.
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 C1168) and converted to 8 M HNO3 solutions.
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses are mathematical conversions that are provided for information only and are not considered standard. Additionally, the non-SI units of molarity and centimeters of mercury are to be regarded as standard.
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Some specific hazards statements are given in Section 9 on Hazards.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: C1432 − 23
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 C1432; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
2
1.1 This test method covers the determination of 25 ele- 2.1 ASTM Standards:
ments in plutonium (Pu) materials. The Pu is dissolved in acid, C757 Specification for Nuclear-Grade Plutonium Dioxide
the Pu matrix is separated from the target impurities by an ion Powder for Light Water Reactors
exchange separation, and the concentrations of the impurities C859 Terminology Relating to Nuclear Materials
are determined by inductively coupled plasma-atomic emission C1128 Guide for Preparation of Working Reference Materi-
spectroscopy (ICP-AES). als for Use in Analysis of Nuclear Fuel Cycle Materials
C1168 Practice for Preparation and Dissolution of Plutonium
1.2 This test method is specific for the determination of
Materials for Analysis
impurities in 8 M HNO solutions. Impurities in other pluto-
3
C1215 Guide for Preparing and Interpreting Precision and
nium materials, including plutonium oxide samples, may be
Bias Statements in Test Method Standards Used in the
determined if they are appropriately dissolved (see Practice
Nuclear Industry
C1168) and converted to 8 M HNO solutions.
3
D1193 Specification for Reagent Water
1.3 The values stated in SI units are to be regarded as
standard. The values given in parentheses are mathematical 3. Terminology
conversions that are provided for information only and are not
3.1 Except as otherwise defined herein, definitions of terms
considered standard. Additionally, the non-SI units of molarity
are as given in Terminology C859.
and centimeters of mercury are to be regarded as standard.
4. Summary of Test Method
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4.1 A sample of plutonium metal is dissolved in a small
responsibility of the user of this standard to establish appro-
volume of 6 M hydrochloric acid (HCl). Then, 10 M (HNO )/
3
priate safety, health, and environmental practices and deter-
0.03 M hydrofluoric acid (HF) is added to the dissolved
mine the applicability of regulatory limitations prior to use.
plutonium to oxidize the plutonium to the Pu (IV) state. The
Some specific hazards statements are given in Section 9 on
sample solution is loaded onto a nitrate anion exchange resin
Hazards.
and eluted with 8 M HNO /0.006 M HF. The rinses contain the
3
1.5 This international standard was developed in accor-
target metallic impurities and less than 15 μg/mL Pu. The
dance with internationally recognized principles on standard-
plutonium is stripped from the anion exchange resin with 0.1
ization established in the Decision on Principles for the
M HCl. The rinses containing the metallic impurities are
Development of International Standards, Guides and Recom-
analyzed by ICP-AES.
mendations issued by the World Trade Organization Technical
5. Significance and Use
Barriers to Trade (TBT) Committee.
5.1 This test method can be used on plutonium matrices in
nitrate solutions.
1
This test method is under the jurisdiction of ASTM Committee C26 on Nuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
2
Test. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Dec. 1, 2023. Published January 2024. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1999. Last previous edition approved in 2015 as C1432 – 15. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/C1432-23. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C1432 − 23
5.2 This test method has been validated for all elements 7.3 Vacuum manifold set at approximately 23 cm Hg (9 in.
listed in Test Methods C757 except sulfur (S) and tantalum Hg) is optional. A gravity system is also acceptable.
(Ta).
7.4 15 mL plastic disposable ion exchange columns.
5.3 This test method has been validated for all of the cation
7.5 50 mL plastic vials.
eleme
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: C1432 − 15 C1432 − 23
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 C1432; 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 (´) indicates an editorial change since the last revision or reapproval.
1. 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 HNO solutions. Impurities in other plutonium materials,
3
including plutonium oxide samples, may be determined if they are appropriately dissolved (see Practice C1168) and converted to
8 M HNO solutions.
3
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses are mathematical conversions that
are provided for information only and are not considered standard. Additionally, the non-SI units of molarity and centimeters of
mercury are to be regarded as standard.
1.4 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 healthsafety, health, and environmental practices and determine
the applicability of regulatory limitations prior to use. Some specific hazards statements are given in Section 9 on Hazards.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
C757 Specification for Nuclear-Grade Plutonium Dioxide Powder for Light Water Reactors
C758 Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-
Grade Plutonium Metal
C759 Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-
Grade Plutonium Nitrate Solutions
C859 Terminology Relating to Nuclear Materials
C1128 Guide for Preparation of Working Reference Materials for Use in Analysis of Nuclear Fuel Cycle Materials
C1168 Practice for Preparation and Dissolution of Plutonium Materials for Analysis
1
This test method is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test.
Current edition approved June 1, 2015Dec. 1, 2023. Published July 2015January 2024. Originally approved in 1999. Last previous edition approved in 20082015 as
C1432 – 03 (2008).C1432 – 15. DOI: 10.1520/C1432-15.10.1520/C1432-23.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C1432 − 23
C1215 Guide for Preparing and Interpreting Precision and Bias Statements in Test Method Standards Used in the Nuclear
Industry
D1193 Specification for Reagent Water
3. Terminology
3.1 Except as otherwise defined herein, definitions of terms are as given in Terminology C859.
4. Summary of Test Method
4.1 A sample of plutonium metal is dissolved in a small volume of 6 M hydrochloric acid (HCl). Then, 10 M (HNO )/0.03 M
3
)/0.03 M hydrofluoric acid (HF) is added to the dissolved plutonium to oxidize the plutonium to the Pu (IV) state. The sample
solution is loaded onto a nitrate anion exchange resin and eluted with 8 M HNO /0.006 M HF. The rinses contain the target metallic
3
impurities and less than 15 μg/mL Pu. The plutonium is stripped from the anion exchange resin with 0.1 M HCl. The rinses
containing the metallic impurities are analy
...
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