ASTM C1637-21

Standard Test Method for Determination of Impurities in Plutonium Materials—Acid Digestion and Inductively Coupled Plasma-Mass Spectroscopy (ICP-MS) Analysis

SIGNIFICANCE AND USE
5.1 This test method may be run together with Test Method C1432 to analyze for trace impurities in Pu metal. Using the technique described in this test method and the technique described in Test Method C1432 will provide the analyst with a more thorough verification of the impurity concentrations contained in the Pu metal sample. In addition, Test Method C1432 can be used to determine impurity concentrations for analytes such as Ca, Fe, Na, and Si, which have not been determined using this test method.  
5.2 This test method can be used on Pu matrices in nitrate solutions.  
5.3 This test method has been validated for use on materials that meet the specifications described in Specification C757 and Test Methods C758 and C759.  
5.4 This test method has been validated for all elements listed in Table 1. (A) Without outlying value.
SCOPE
1.1 This test method covers the determination of trace elements in plutonium (Pu) materials such as Pu metal, Pu oxides, and Pu/uranium (U) mixed oxides. The Pu sample is dissolved in acid, and the concentration of the trace impurities are determined by Inductively Coupled Plasma-Mass Spectroscopy (ICP-MS).  
1.2 This test method is specific for the determination of trace impurities where the samples are dissolved and the oxidation state is adjusted to the Pu(IV) and, if applicable, the U(VI) state. It may be applied to other matrices; however, it is the responsibility of the user to evaluate the performance of other matrices.  
1.3 The use of a quadrupole ICP-MS or a high resolution ICP-MS (HR-ICP-MS) can be employed in all applications relevant to this test method. HR-ICP-MS is a better option in many cases since it can reduce or potentially eliminate interferences encountered in the following complex sample matrices.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 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.  
1.6 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.

General Information

• Status: Published
• Publication Date: 31-May-2021
• ICS: 71.060.10 - Chemical elements
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

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: C1637 − 21
Standard Test Method for
Determination of Impurities in Plutonium Materials—Acid
Digestion and Inductively Coupled Plasma-Mass
1
Spectroscopy (ICP-MS) Analysis
This standard is issued under the fixed designation C1637; 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 trace
2.1 ASTM Standards:
elements in plutonium (Pu) materials such as Pu metal, Pu
C757 Specification for Nuclear-Grade Plutonium Dioxide
oxides, and Pu/uranium (U) mixed oxides. The Pu sample is
Powder for Light Water Reactors
dissolved in acid, and the concentration of the trace impurities
C758 Test Methods for Chemical, Mass Spectrometric,
aredeterminedbyInductivelyCoupledPlasma-MassSpectros-
Spectrochemical, Nuclear, and RadiochemicalAnalysis of
copy (ICP-MS).
Nuclear-Grade Plutonium Metal
C759 Test Methods for Chemical, Mass Spectrometric,
1.2 This test method is specific for the determination of
Spectrochemical, Nuclear, and RadiochemicalAnalysis of
trace impurities where the samples are dissolved and the
Nuclear-Grade Plutonium Nitrate Solutions
oxidation state is adjusted to the Pu(IV) and, if applicable, the
C859 Terminology Relating to Nuclear Materials
U(VI) state. It may be applied to other matrices; however, it is
C1168 PracticeforPreparationandDissolutionofPlutonium
the responsibility of the user to evaluate the performance of
Materials for Analysis
other matrices.
C1432 Test Method for Determination of Impurities in
1.3 The use of a quadrupole ICP-MS or a high resolution
Plutonium: Acid Dissolution, Ion Exchange Matrix
ICP-MS (HR-ICP-MS) can be employed in all applications
Separation, and Inductively Coupled Plasma-Atomic
relevant to this test method. HR-ICP-MS is a better option in
Emission Spectroscopic (ICP/AES) Analysis
many cases since it can reduce or potentially eliminate inter-
D1193 Specification for Reagent Water
ferences encountered in the following complex sample matri-
E1154 Specification for Piston or Plunger Operated Volu-
ces.
metric Apparatus
1.4 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
3. Terminology
standard.
3.1 Except as otherwise defined herein, definitions of terms
1.5 This standard does not purport to address all of the
are as given in Terminology C859.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety, health, and environmental practices and deter-
4.1 Samples of plutonium materials are prepared and dis-
mine the applicability of regulatory limitations prior to use.
solved in accordance with an appropriate procedure in Practice
1.6 This international standard was developed in accor-
C1168.These procedures adjust the dissolved Pu to the Pu(IV)
dance with internationally recognized principles on standard-
oxidation state.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
4.2 A sample of Pu metal is weighed and dissolved as
mendations issued by the World Trade Organization Technical
described in Practice C1168.An aliquot of the original sample
Barriers to Trade (TBT) Committee.
is then taken and diluted with 1 % HNO by volume to a
3
prescribed volume. Aliquots from a second dilution of the
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
2
Test. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
CurrenteditionapprovedJune1,2021.PublishedJuly2021.Originallyapproved contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
in 2006. Last previous edition approved in 2013 as D1637 – 13. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
C1637-21. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
C1637 − 21
TABLE 1 Impurity Elements, Mean Percent Recoveries and
original sample are used to prepare run batch dilutions that are
3 Percent Relative Standard Deviations
analyzed for trace impurities by ICP-MS (Section 10).
Element N Mean R, % RSD, %
4.3 Plutonium oxide powders are we
...

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: C1637 − 13 C1637 − 21
Standard Test Method for
the Determination of Impurities in Plutonium Metal: Acid
Materials—Acid Digestion and Inductively Coupled Plasma-
1
Mass Spectroscopy (ICP-MS) Analysis
This standard is issued under the fixed designation C1637; 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 Methodtest method covers the determination of 58 trace elements in plutonium (Pu) metal. materials such as Pu
metal, Pu oxides, and Pu/uranium (U) mixed oxides. The Pu sample is dissolved in acid, and the concentration of the trace
impurities are determined by Inductively Coupled Plasma-Mass Spectroscopy (ICP-MS).
1.2 This Test Methodtest method is specific for the determination of trace impurities in Pu metal. It may be applied to other types
of Pu materials, such as Pu oxides, if the samples are dissolved and oxidized to the Pu(IV) state. However, where the samples are
dissolved and the oxidation state is adjusted to the Pu(IV) and, if applicable, the U(VI) state. It may be applied to other matrices;
however, it is the responsibility of the user to evaluate the performance of other matrices.
1.3 The use of a quadrupole ICP-MS or a high resolution ICP-MS (HR-ICP-MS) can be employed in all applications relevant to
this test method. HR-ICP-MS is a better option in many cases since it can reduce or potentially eliminate interferences encountered
in the following complex sample matrices.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all of the safety concerns concerns, if any, associated with its use. It is the
responsibility of the user of this methodstandard to establish appropriate safety safety, health, and healthenvironmental practices
and to determine the applicability of regulatory limitations prior to use of this standard.use.
1.6 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
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 Jan. 1, 2013June 1, 2021. Published January 2013July 2021. Originally approved in 2006. Last previous edition approveapproved in 20062013
as D1637 – 06.13. DOI: 10.1520/C1637-13.10.1520/C1637-21.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. 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 ----------------------
C1637 − 21
C759 Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-
Grade Plutonium Nitrate Solutions
C859 Terminology Relating to Nuclear Materials
C1168 Practice for Preparation and Dissolution of Plutonium Materials for Analysis
C1432 Test Method for Determination of Impurities in Plutonium: Acid Dissolution, Ion Exchange Matrix Separation, and
Inductively Coupled Plasma-Atomic Emission Spectroscopic (ICP/AES) Analysis
D1193 Specification for Reagent Water
E1154 Specification for Piston or Plunger Operated Volumetric Apparatus
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 Samples of plutonium materials are prepared and dissolved in accordance with an appropriate procedure in Practice C1168.
These procedures adjust the dissolved Pu to the Pu(IV) oxidation state.
4.2 A sample of Pu metal is weighed and dissolved as
...