ASTM C1411-99

Standard Practice for the Ion Exchange Separation of Uranium and Plutonium Prior to Isotopic Analysis

SCOPE
1.1 This practice is for the ion exchange separation of uranium and plutonium from each other and from other impurities for subsequent isotopic analysis by thermal ionization mass spectrometry. Plutonium-238 and uranium-238, and plutonium-241 and americium-241, will appear as the same mass peak and must be chemically separated prior to analysis. Only high purity solutions can be analyzed reliably using thermal ionization mass spectrometry.
1.2 This standard may involve hazardous material, operations, and equipment. 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.

General Information

• Status: Historical
• Publication Date: 09-Jan-2001
• ICS: 27.120.30 - Fissile materials and nuclear fuel technology
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

Relations

• Replaced By: ASTM C1411-01 - Standard Practice for the Ion Exchange Separation of Uranium and Plutonium Prior to Isotopic Analysis
• Effective Date: 10-Jan-2001

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or
withdrawn. Contact ASTM International (www.astm.org) for the latest information.
Designation: C 1411 – 99
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Practice for
The Ion Exchange Separation of Uranium and Plutonium
1
Prior to Isotopic Analysis
This standard is issued under the fixed designation C 1411; 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.
1. Scope to provide up to 1 mg of plutonium on the ion exchange
column to be separated from 10 mg or less of uranium. Valence
1.1 This practice is for the ion exchange separation of
adjustment is attained by using one of two procedures.
uranium and plutonium from each other and from other
3.1.1 For any sample type, especially those containing large
impurities for subsequent isotopic analysis by thermal ioniza-
amounts of impurities, ferrous sulfate may be used for reduc-
tion mass spectrometry. Plutonium–238 and uranium–238, and
tion. The aliquant is dissolved in 3 M HNO . Ferrous sulfate is
3
plutonium–241 and americium–241, will appear as the same
added to reduce all plutonium (VI) to plutonium (III), then 16
mass peak and must be chemically separated prior to analysis.
M HNO is added to oxidize plutonium (III) to plutonium (IV),
3
Only high purity solutions can be analyzed reliably using
and to adjust the final acid concentration to 8M HNO .
3
thermal ionization mass spectrometry.
3.1.2 A hydrogen peroxide reduction may be used for
1.2 This standard may involve hazardous material, opera-
relatively pure samples which do not contain excessive
tions, and equipment. This standard does not purport to
amounts of oxidizing impurities. The aliquant is dissolved in 8
address all of the safety concerns, if any, associated with its
M HNO . Hydrogen peroxide is added to the aliquant prior to
3
use. It is the responsibility of the user of this standard to
fuming to reduce plutonium (VI) to the lower oxidation states.
consult and establish appropriate safety and health practices
The solution is warmed on a hot plate to destroy excess
and determine the applicability of regulatory limitations prior
,
4 5
hydrogen peroxide and stabilize plutonium (IV) in solution.
to use.
3.2 After valence adjustment, the resulting solution is
2. Referenced Documents passed through an anion exchange column in the nitrate form
which retains the plutonium; uranium and americium are not
2.1 ASTM Standards:
absorbed. The adsorbed plutonium is washed with additional 8
C 698 Standard Test Method for Chemical, Mass Spectro-
M nitric acid (HNO ) to remove impurities and then stripped
metric, and Spectrochemical Analysis of Nuclear-Grade 3
2
from the column with 0.36 M hydrochloric acid (HCl) and 0.01
Mixed Oxides ((U, Pu)O ), Sections 141-149.
2
M hydrofluoric acid (HF). The effluent containing the uranium
C 833 Standard Specification for Sintered (Uranium, Pluto-
2
and americium is converted to a HCl medium, and this solution
nium) Dioxide Pellets.
is passed through an anion exchange column in the chloride
C 1008 Standard Specification for Sintered (Uranium, Plu-
2
form which retains the uranium. The adsorbed uranium is
tonium) Dioxide Pellets - Fast Reactor Fuel.
washed with additional concentrated HCl to remove the
C 1168 Standard Practice for Preparation and Dissolution of
2
impurities and then stripped from the column with 0.1 M HCl.
Plutonium Materials for Analysis.
E 267 Standard Test Method for Uranium and Plutonium
4. Significance and Use
3
Concentrations and Isotopic Abundances.
4.1 Uranium and plutonium are used in nuclear reactor fuel
3. Summary of Practice and must be analyzed to insure that they meet certain criteria
for isotopic composition as described in Specification C 833
3.1 Solid samples are dissolved according to Practice
and Specification C 1008. This standard practice is used to
C 1168 or other appropriate methods. The resulting solution is
chemically separate the same mass peak interferences from
processed by this practice to prepare separate solutions of
uranium and plutonium and from other impurities prior to
plutonium and uranium for mass spectrometric isotopic analy-
isotopic abundance determination by thermal ionization mass
sis using Method C 698, see Sec. 144 through 145 and 147.4
spectrometry.
through 149 or its replacement. Appropriate aliquants are taken
4.2 In those facilities where perchloric acid use is tolerated,
the ion exchange separation procedure in Test Method E 267
1
This practice is under the jurisdiction of ASTM Committee C-26 on Nuclear
may be used prior to isotopic abundance determination. Also,
Fuel Cycle
...