ASTM C1432-15

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 − 15
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 Spectrochemical, Nuclear, and RadiochemicalAnalysis of
Nuclear-Grade Plutonium Nitrate Solutions
1.1 This test method covers the determination of 25 ele-
C859 Terminology Relating to Nuclear Materials
ments in plutonium (Pu) materials.The Pu is dissolved in acid,
C1168 PracticeforPreparationandDissolutionofPlutonium
the Pu matrix is separated from the target impurities by an ion
Materials for Analysis
exchange separation, and the concentrations of the impurities
D1193 Specification for Reagent Water
aredeterminedbyinductivelycoupledplasma-atomicemission
spectroscopy (ICP-AES).
3. Terminology
1.2 This test method is specific for the determination of
3.1 Except as otherwise defined herein, definitions of terms
impurities in8MHNO solutions. Impurities in other pluto-
3
are as given in Terminology C859.
nium materials, including plutonium oxide samples, may be
determined if they are appropriately dissolved (see Practice
4. Summary of Test Method
C1168) and converted to8MHNO solutions.
3
4.1 A sample of plutonium metal is dissolved in a small
1.3 The values stated in SI units are to be regarded as
volume of 6 M hydrochloric acid (HCl). Then, 10 M (HNO )/
3
standard. The values given in parentheses are mathematical
0.03 M hydrofluoric acid (HF) is added to the dissolved
conversions that are provided for information only and are not
plutonium to oxidize the plutonium to the Pu (IV) state. The
considered standard.
sample solution is loaded onto a nitrate anion exchange resin
1.4 This standard does not purport to address all of the
and eluted with8MHNO /0.006 M HF.The rinses contain the
3
safety concerns, if any, associated with its use. It is the
target metallic impurities and less than 15 µg/mL Pu. The
responsibility of the user of this standard to establish appro-
plutonium is stripped from the anion exchange resin with 0.1
priate safety and health practices and determine the applica-
M HCl. The rinses containing the metallic impurities are
bility of regulatory limitations prior to use.
analyzed by ICP-AES.
2. Referenced Documents
5. Significance and Use
2
2.1 ASTM Standards:
5.1 This test method can be used on plutonium matrices in
C757 Specification for Nuclear-Grade Plutonium Dioxide
nitrate solutions.
Powder, Sinterable
5.2 This test method has been validated for all elements
C758 Test Methods for Chemical, Mass Spectrometric,
listed in Test Methods C757 except sulfur (S) and tantalum
Spectrochemical, Nuclear, and RadiochemicalAnalysis of
(Ta).
Nuclear-Grade Plutonium Metal
5.3 This test method has been validated for all of the cation
C759 Test Methods for Chemical, Mass Spectrometric,
elements measured in Table 1. Phosphorus (P) requires a
vacuum or an inert gas purged optical path instrument.
1
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear
6. Interferences
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
Test.
6.1 Plutonium concentrations of less than 50 µg/mL in the
CurrenteditionapprovedJune1,2015.PublishedJuly2015.Originallyapproved
final aqueous phase do not significantly affect the analytical
in 1999. Last previous edition approved in 2008 as C1432 – 03 (2008). DOI:
10.1520/C1432-15.
results for most elements. Interference studies should be made
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
todeterminethedegreeofPuandotherelementalinterferences
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
onthetargetanalytes;backgroundandinterelementcorrections
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. may be required.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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C1432 − 15
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
Barium Ba 455.403 {58} 2.5 2.4 95 5
Beryllium
...