ASTM C1432-23

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Designation: C1432 − 15 C1432 − 23
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
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,
including plutonium oxide samples, may be determined if they are appropriately dissolved (see Practice C1168) and converted to
8 M HNO 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 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
2.1 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
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.
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
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
)/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
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 analyzed by ICP-AES.
5. 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.
6. Interferences
6.1 Plutonium concentrations of less than 50 μg/mL in the final aqueous phase do not significantly affect the analytical results for
most elements. Interference studies should be made to determine the degree of Pu and other elemental interferences on the target
analytes; background and interelement corrections may be required.
7. Apparatus
7.1 An ICP-AES equipped with a Charge Injection Device (CID) detector or an ICP-AES with a spectral bandpass of 0.05 nm
TABLE 1 Percent Recovery and Repeatability Standard Deviation for Sixteen Spiked Samples
Wavelength/Order Actual Conc Mean Conc Average R.S.D.RSD
Element
(nm) (μg/mL) (μg/mL) (%R) R % (%) %
Aluminum Al 396.152 {67} 2.5 2.4 95 6
Barium Ba 455.403 {58} 2.5 2.4 95 5
Beryllium Be 313.042 {84} 2.5 2.3 94 6
Boron B 249.773 {106} 2.5 2.5 100 7
Cadmium Cd 226.502 {116} 2.5 2.5 101 12
Calcium Ca 396.847 {66} 2.5 2.6 104 20
Chromium Cr 283.563 {93} 2.5 2.3 92 8
Cobalt Co 228.616 {115} 2.5 2.5 101 6
Copper Cu 324.754 {81} 2.5 2.4 97 6
Iron Fe 259.940 {101} 2.5 2.5 101 12
Lead Pb 220.353 {120} 2.5 3.1 122 12
Lithium Li 670.784 {39} 2.5 2.2 87 6
Magnesium Mg 280.270 {94} 2.5 2.4 95 6
Manganese Mn 257.610 {102} 2.5 2.5 98 5
Molybdenum Mo 202.030 {130} 2.5 2.6 103 10
Nickel Ni 231.604 {114} 2.5 2.5 100 11
Silicon Si 251.612 {104} 2.5 2.3 92 16
Sodium Na 588.995 {45} 25.0 24.7 97 16
Strontium Sr 421.552 {62} 2.5 2.4 95 5
Tin Sn 189.989 {139} 2.5 2.7 109 19
Titanium Ti 334.941 {79} 2.5 2.5 102 8
Tungsten W 207.911 {127} 2.5 2.5 99 11
Vanadium V 292.402 {90} 2.5 2.0 82 7
Zinc Zn 213.856 {123} 2.5 2.5 100 8
Zirconium Zr 339.198 {78} 2.5 2.5 101 10
C1432 − 23
0.05 nm or less is required to provide the necessary spectral resolution. The spectrometer may be either a simultaneous
multielement or a sequential spectrometer. The spectrometer may be either an inert gas-path or vacuum instrument; the appropriate
spectral lines should be selected for each specific instrument. Either an analog or digital readout system may be used.
7.2 The ICP-AES is interfaced to an enclosure. The torch box is contained with an enclosure, since plutonium containing materials
may come in direct contact with the torch despite the substantial removal by ion exchange in 10.3. A possible setup is described
in ASTM STP 951.
7.3 Vacuum manifold set at approximately 23 cm Hg (9 in. Hg) is optional. A gravity system is also acceptable.
7.4 15 mL plastic disposable ion exchange columns.
7.5 50 mL plastic vials.
7.6 Plastic micro and macro pipettes.
7.7 1000 mL plastic volumetric flasks.
8. Reagents and Materials
8.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society (ACS),
where such specifications are available. Other grades could be used, provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of the determination.
8.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean laboratory accepted
demineralized or deionized water as described by Type 1 of Specification D1193.
8.3 Ultra high Ultra-high purity acids shall be used for sample dissolution and calibration standards preparation unless otherwise
noted.
NOTE 1—The molarity of ultra high ultra-high purity acids may vary from standard ACS specifications for concentrated acids.
NOTE 2—All reagents are prepared and stored in polytetrafluoroethylene (PTFE) containers.
8.4 Hydrochloric Acid (HCl, 11.3 M),concentrated ultra high ultra-high purity HCl.
8.5 Hydrochloric Acid (HCl, 6 M)—Add 531 mL of concentrated ultra high ultra-high purity HCl (11.3 M) to less than 450 mL
of water and dilute to 1 L with water.
8.6 Hydrochloric Acid (HCl, 0.1 M)—Add 8.8 mL of concentrated ultra high ultra-high purity HCl (11.3 M) to water, while
stirring, and dilute to 1 L with water. (Reagent grade HCl can be used in preparing this reagent.)
8.7 Hydrofluoric Acid (HF, 28.3 M),concentrated ultra high ultra-high purity HF.
8.8 Nitric Acid (HNO , 15.8 M),concentrated ultra high ultra-high purity nitric acid.
Edellson, M. C., and Daniel, J. Leland, “Plasma Spectroscopy of the Analysis of Hazardous Materials: Design and Application of Enclosed Plasma Sources,” Conference
Proceedings, ASTM STP 951, ASTM, 1986.
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
C1432 − 23
8.9 Nitric Acid-Hydrofluoric Acid Mixture, 10 M HNO /0.03 M HF—Add 1 mL of concentrated ultra high ultra-high purity HF
(28.3 M) (28.3 M) to water; using a plastic pipette, while stirring, add 633 mL concentrated ultra high ultra-high purity HNO (15.8
M) and dilute to 1 L 1 L with water.
8.10 Nitric Acid-Hydrofluoric Acid Mixture, 8 M HNO /0.006 M HF—Add 0.21 mL of concentrated ultra high ultra-high purity
HF (28.3 M) to water; using a plastic pipette, while stirring, add 506 mL of concentrated ultra high ultra-high purity HNO (15.8
M) and dilute to 1 L with water.
8.11 Nitric Acid (HNO , 4 M)—Add 253 mL of concentrated ultra high ultra-high purity nitric acid (15.8 M) to water, while
stirring, and dilute to 1 L with water.
8.12 Anion Exchange Resin, macroporous-1 (MP-1), 200-400 200 mesh - 400 mesh, either nitrate form or chloride form, high
purity.
8.13 Stock Solutions, traceable to a national standard, of multielement spike solutions are available from a commercial vendor. The
stock solutions of multielement spike solutions can also be prepared in-house.
8.13.1 Spike Solution 1 (SS-1), contains 500 μg/mL of Al, Ba, Be, Ca, Li, Mg, Sr, and Na in 0.8 M HNO .
8.13.2 Spike Solution 2 (SS-2), contains 500 μg/mL of B, Mo, Si, Sn, Ti, W, and Zr in 0.8 M HNO .
8.13.3 Spike Solution 3 (SS-3), contains 500 μg/mL of Cd, Cr, Co, Cu, Fe, Pb, Mn, Ni, V, and Zn in 0.8 M HNO .
8.14 Stock Solutions, traceable to a national standard, of multielement impurity standards are available from a commercial vendor.
The stock solutions of multielement standards can also be prepared in-house.
8.14.1 Calibration Stock Solution-2 (CSS-2), contains 5000 μg/mL of Na in 0.8 M HNO .
8.14.2 Calibration Stock Solution-3 (CSS-3), contains 500 μg/mL of Mo, Si, Sn, Ti, W, and Zr in 0.3 M HNO /0.1 M HF.
8.14.3 Calibration Stock Solution-5 (CSS-5), contains 500 μg/mL of Al, Ba, and Sr in 0.8 M HNO .
8.14.4 Calibration Stock Solution-6 (CSS-6), contains 500 μg/mL of Be, B, Cd, Ca, Cr, Co, Cu, Fe, Li, Mg, Mn, Ni, Pb, V, and
Zn in 0.8 M HNO .
8.15 Prepare the multielement impurity standards and blanks as described in 8.15.1 – 8.15.5. All calibration standard solutions are
stored in PTFE containers.
8.15.1 Calibration Standard One High (CAL 1 HI)—Pipette 20 mL each, of stock solutions CSS-3, and CSS-5 into a 1 L
volumetric flask. Dilute to 1 L with 8 M HNO /0.006 M HF. This standard solution contains the target analytes at a concentration
of 10 μg/mL.
8.15.2 Calibration Standard One Low (CAL 1 LO)—Pipette 10 mL each, of stock solutions CSS-3, and CSS-5 into a 1 L
volumetric flask. Dilute to 1 L with 8 M HNO /0.006 M HF. This standard solution contains the target analytes at a concentration
of 5 μg/mL.
8.15.3 Calibration Standard Two High (CAL 2 HI)—Pipette 20 mL each, of stock solutions CCS-2, and CSS-6 into a 1 L
volumetric flask. Dilute to 1 L with 8 M HNO /0.006 M HF. This standard solution contains the ta
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