ASTM C1432-99
(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
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). The elements determined are listed in Table 2.
1.2 This test method is specific for the determination of impurities in Pu in 8 M nitric acid (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 Plutonium bearing materials are radioactive and toxic. Adequate laboratory facilities, glove boxes, and fume hoods, along with safe techniques, must be used in handling samples containing these materials. A detailed discussion of all the precautions necessary is beyond the scope of this test method; however, personnel who handle these materials should be familiar with such safe handling practices.
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 health practices and determine the applicability of regulatory limitations prior to use.
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Designation: C 1432 – 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
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.
A
TABLE 1 ICP-AES Operating Conditions
1. Scope
Parameter Value
1.1 This test method covers the determination of 25 ele-
Forward rf power 1.4 kW
ments in plutonium (Pu) materials. The Pu is dissolved in acid,
Reflected rf power <10 W
the Pu matrix is separated from the target impurities by an ion
Outer argon flow 15 L/min
exchange separation, and the concentrations of the impurities
Auxiliary argon flow 0.8 L/min
Carrier argon flow 0.7 L/min
are determined by inductively coupled plasma-atomic emission
Observation height 15 mm above load coil
spectroscopy (ICP-AES). The elements determined are listed
Nebulizer Cross flow type
in Table 2.
Solution uptake rate 1.4 mL/min
1.2 This test method is specific for the determination of A
These conditions are typical for an ARL #3580.
impurities in Pu in 8 M nitric acid (HNO ) solutions. Impuri-
ties in other plutonium materials, including plutonium oxide
C 759 Test Methods for Chemical, Mass Spectrometric,
samples, may be determined if they are appropriately dissolved
Spectrochemical, Nuclear, and Radiochemical Analysis of
(see Practices C 1168) and converted to8MHNO solutions.
Nuclear-Grade Plutonium Nitrate Solutions
1.3 Plutonium bearing materials are radioactive and toxic.
Adequate laboratory facilities, glove boxes, and fume hoods,
along with safe techniques, must be used in handling samples
TABLE 2 Repeatability Standard Deviation for Three Spike
containing these materials. A detailed discussion of all the
Recovery Experiments
precautions necessary is beyond the scope of this test method;
Experimental
Determinations
however, personnel who handle these materials should be
Element Wavelength Actual Mean Avg % Recovery RSD %
familiar with such safe handling practices.
(nm) Conc Conc
1.4 This standard does not purport to address all of the
(μg/g) (μg/g)
safety concerns, if any, associated with its use. It is the
Aluminum 308.22 6.0 6.9 114 2.7
responsibility of the user of this method to establish appropri-
Barium 493.41 3.0 3.3 109 1.7
Beryllium 313.04 1.5 1.7 112 1.7
ate safety and health practices and determine the applicability
Cadmium 226.5 6.0 6.5 109 4.6
of regulatory limitations prior to use of this standard.
Calcium 393.37 3.0 3.3 109 1.8
Chromium 267.72 6.0 7.0 117 5.1
2. Referenced Documents
Cobalt 237.86 6.0 6.9 115 1.6
Copper 324.75 3.0 3.5 118 2.0
2.1 ASTM Standards:
Hafnium 232.25 6.0 6.4 106 1.1
C 697 Test Methods for Chemical, Mass Spectrometric, and
Iron 259.94 6.0 6.8 113 1.6
Lead 220.35 6.0 6.9 114 3.6
Spectrochemical Analysis of Nuclear-Grade Plutonium
Lithium 670.78 3.0 3.4 112 1.8
Dioxide Powers and Pellets
Magnesium 279.55 3.0 3.5 116 1.8
C 757 Specification for Nuclear-Grade Plutonium Dioxide
Manganese 257.61 3.0 3.4 112 1.8
Molybdenum 202.03 6.0 4.5 75 22
Powder, Sinterable
Nickel 231.6 6.0 6.8 114 1.6
C 758 Test Methods for Chemical, Mass Spectrometric,
Niobium 316.34 6.0 5.9 98.9 2.2
Spectrochemical, Nuclear, and Radiochemical Analysis of
Phosphorus 178.29 6.0 6.4 106 2.3
Potassium 766.49 30.0 33 110 1.8
Nuclear-Grade Plutonium Metal
Strontium 421.55 3.0 3.3 109 1.7
Titanium 368.52 3.0 3.3 111 1.1
Vanadium 292.4 6.0 6.8 113 1.9
This guide is under the jurisdiction of ASTM Committee C-26 on Nuclear Fuel
Yttrium 371.03 3.0 3.3 109 1.7
Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test.
Zinc 206.2 3.0 2.3 75.4 7.5
Current edition approved June 10, 1999. Published August 1999. Zirconium 349.62 6.0 6.5 109 1.5
Annual Book of ASTM Standards, Vol 12.01.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
C 1432
C 1168 Practice for Preparation and Dissolution of Pluto- 6.3 Vacuum manifold set at approximately 9 in. Hg (op-
2 6
nium Materials for Analysis tional). A gravity system is acceptable.
3 7
D 1193 Specification for Reagent Water 6.4 15-mL plastic disposable ion exchange columns.
6.5 30-mL plastic vials.
3. Summary of Test Method
6.6 Plastic micro and macro pipettes.
6.7 A 500-mL fritted column.
3.1 A sample of Pu metal is dissolved in a small volume of
6 M hydrochloric acid (HCl). Then, 1 mL of 10 M (HNO )/0.2
7. Reagents and Materials
M hydrofluoric acid (HF) is added to the dissolved Pu to
7.1 Purity of Reagents—Reagent grade chemicals shall be
oxidize the Pu to the Pu (IV) state. The sample solution is
used in all tests. Unless otherwise indicated, it is intended that
loaded onto a nitrate anion exchange resin and eluted with 8 M
all reagents shall conform to the specifications of the Commit-
HNO /0.2 M HF. The rinses contain the target metallic
tee on Analytical Reagents of the American Chemical Society
impurities and less than 15 μg/mL Pu. The Pu is stripped from
where such specifications are available. Other grades should
the anion exchange resin with 0.1 M HCl. The rinses contain-
be used, provided it is first ascertained that the reagent is of
ing the metallic impurities are analyzed by ICP-AES.
sufficiently high purity to permit its use without lessening the
4. Significance and Use accuracy of the determination.
7.2 Purity of Water—Unless otherwise indicated, references
4.1 This test method measures all elements listed in Speci-
to water shall be understood to mean laboratory accepted
fication C 757, except sulfur (S) and tantalum (Ta).
demineralized or deionized water as describe by Type 1 of
4.2 This test method measures all of the cation elements
Specification D 1193.
measured in Test Methods C 697, except silver (Ag), gold
7.3 Ultra high purity acids shall be used for sample disso-
(Au), and bismuth (Bi). Phosphorus (P) requires a vacuum
lution and calibration standards preparation unless otherwise
instrument.
noted.
5. Interferences
NOTE 1—All reagents are prepared and stored in polytetrafluoroethyl-
5.1 Plutonium concentrations of less than 50 μg/mL in the ene (PTFE) containers.
final aqueous phase do not significantly affect the analytical
7.4 Hydrochloric Acid ((HCl) (sp gr 1.18)), concentrated
results for most elements. Interference studies should be made 9
ultra high purity HCl.
to determine the degree of Pu and other elemental interferences
7.5 Hydrochloric Acid (HCl, 6 M)—Add 500 mL of con-
on the target analytes; background and interelement corrections
centrated ultra high purity HCl (sp gr 1.18) to less than 500 mL
may be required.
of water and dilute to 1 L with water.
7.6 Hydrochloric Acid (HCl, 0.1 M)—Add 8.3 mL of
6. Apparatus
concentrated ultra high purity HCl (sp gr 1.18) to water, while
6.1 An ICP-AES with a spectral bandpass of 0.05 nm or less
stirring, and dilute to 1 L with water. (Reagent grade HCl can
is required to provide the necessary spectral resolution. The
be used in preparing this reagent.)
spectrometer may be either a simultaneous multielement or a
7.7 Hydrofluoric Acid ((HF) (sp gr 1.15)), concentrated ultra
sequential spectrometer. The spectrometer may be either an
high purity HF.
inert gas-path or vacuum instrument; the appropriate spectral
7.8 Nitric Acid ((HNO ) (sp gr 1.42)), concentrated ultra
lines should be selected for each specific instrument. Either an
high purity HNO .
analog or digital readout system may be used.
7.9 Nitric Acid-Hydrofluoric Acid Mixture,10MHNO /0.2
6.2 The ICP-AES is interfaced to a glovebox. The torchbox
M HF—Add 7.2 mL of concentrated ultra high purity HF (sp
is glovebox enclosed since Pu containing materials come in
gr 1.15) to water, using a plastic pipet, while stirring; add
direct contact with the torch. The torchbox offers several safety
637-mL concentrated ultra high purity HNO (sp gr 1.42); and
features, such as a shielded window for observing the plasma,
dilute to 1 L with water.
which allows the operator to view the plasma without risking
7.10 Nitric Acid-Hydrofluoric Acid Mixture,8MHNO /0.2
damage to the eyes. The torchbox is equipped with an interlock
M HF—Add 7.2 mL of concentrated ultra high purity HF (sp
that shuts off high voltage power to the torchbox when the
gr 1.15) to water, using a plastic pipet, while stirring; add 510
torchbox door is open. The interlock prevents the operator
mL of concentrated ultra high purity HNO (sp gr 1.42); and
from being exposed to high voltages during routine cleaning.
This setup is described in ASTM STP 951.
Speed Mate 10 Vacuum Extraction System, Applied Separations, Bethlehem,
PA, has been found to be acceptable.
Ion exchange columns from either Applied Separation or Bio-Rad Inc. have
Annual Book of ASTM Standards, Vol 11.01. been found to be acceptable.
4 8
An Applied Research Laboratories 3580 ICP-AES instrument (Fisons Instru- Reagent Chemicals, American Chemical Society Specifications, American
ments, Dearborn, MI) has been found to be acceptable. The ARL 3580 is a Chemical Society, Washington, D.C. For suggestions on the testing of reagents not
combination Pashen-Runge type spectrometer containing a 58 channel simultaneous listed by the American Chemical Society, see Analar Standards for Laboratory
spectrometer and a sequential spectrometer, both with a 1-m focal length and Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
capable of operating in the 165 to 800-nm range. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Edelson, M. C., and Daniel, J. Leland, “Plasma Spectroscopy of the Analysis of MD.
Hazardous Materials: Design and Application of Enclosed Plasma Sources,” The Ultrex (J. T. Baker, Inc.) and Seastar brands of ultra high purity acids have
Conference Proceedings, ASTM STP 951, ASTM, 1986. been found to be acceptable.
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