ASTM C1108-99
(Test Method)Standard Test Method for Plutonium by Controlled-Potential Coulometry
Standard Test Method for Plutonium by Controlled-Potential Coulometry
SCOPE
1.1 This test method describes the determination of plutonium in solutions of unirradiated nuclear-grade (that is, high-purity) materials by controlled-potential coulometry. Controlled-potential coulometry may be performed in a choice of supporting electrolytes, such as 0.9 HNO 3 , 1 HClO 4 , 1 HCl, 5 HCl, and 0.5 H 2 SO 4 . Limitations on the use of selected supporting electrolytes are discussed in Section 5. Optimum quantities of plutonium for this procedure are 5 to 10 mg.
1.2 Plutonium-bearing materials are radioactive and toxic. Adequate laboratory facilities, such as gloved boxes, fume hoods, controlled ventilation, etc., along with safe techniques must be used in handling specimens containing these materials.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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 1108 – 99
Standard Test Method for
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Plutonium by Controlled-Potential Coulometry
This standard is issued under the fixed designation C1108; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope C1168 Practice for Preparation and Dissolution of Pluto-
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nium Materials for Analysis
1.1 This test method describes the determination of pluto-
C1210 Guide for Establishing a Measurement System
nium in solutions of unirradiated nuclear-grade (that is, high-
Quality Control Program for Analytical Chemistry Labo-
purity) materials by controlled-potential coulometry.
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ratories Within the Nuclear Industry
Controlled-potential coulometry may be performed in a choice
C1297 Guide for Qualification of Laboratory Analysts for
of supporting electrolytes, such as 0.9 M HNO,1 M HClO,1
3 4
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the Analysis of Nuclear Fuel Cycle Materials
M HCl, 5 M HCl, and 0.5 M H SO . Limitations on the use of
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E691 Practice for Conducting an Interlaboratory Study to
selected supporting electrolytes are discussed in Section 5.
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Determine the Precision of a Test Method
Optimumquantitiesofplutoniumforthisprocedureare5to10
mg.
3. Summary of Test Method
1.2 Plutonium-bearing materials are radioactive and toxic.
3.1 In a controlled-potential coulometric measurement, the
Adequate laboratory facilities, such as gloved boxes, fume
substancebeingdeterminedreactsatanelectrode,thepotential
hoods, controlled ventilation, etc., along with safe techniques
of which is maintained at such a value that unwanted electrode
mustbeusedinhandlingspecimenscontainingthesematerials.
reactions are precluded under the prevailing experimental
1.3 The values stated in SI units are to be regarded as the
conditions. Those substances which have reduction-oxidation
standard. The values given in parentheses are for information
(redox) potentials near that of the ion being determined
only.
constitute interferences. Electrolysis current decreases expo-
1.4 This standard does not purport to address all of the
nentially as the reaction proceeds, until constant background
safety concerns, if any, associated with its use. It is the
current is obtained. Detailed discussions of the theory and
responsibility of the user of this standard to establish appro-
applications of this technique have been published (1, 2, 3, 4,
priate safety and health practices and determine the applica-
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5, 6). The control-potential adjustment technique (7) can be
bility of regulatory limitations prior to use.
used to terminate the electrolysis of the specimen at constant
2. Referenced Documents background current without exhaustive electrolysis with con-
siderable reduction in operating time. Use of the control-
2.1 ASTM Standards:
potential adjustment technique requires that the coulometer
C1009 Guide for Establishing a Quality Assurance Pro-
integrator be capable of operations in a bipolar mode and that
gram for Analytical Chemistry Laboratories Within the
2 the plutonium-containing solution be of high purity, that is,
Nuclear Industry
nuclear grade.
C1068 Guide for Qualification of Measurement Methods
3 3.2 Plutonium(IV) is reduced to Pu(III) at a working elec-
by a Laboratory Within the Nuclear Industry
trode maintained at a potential more negative than the formal
C1128 Guide for Preparation of Working Reference Mate-
redox potential. Plutonium(III) is oxidized to Pu(IV) at a
rials for Use in the Analysis of Nuclear fuel Cycle
3
potential more positive than the formal redox potential. The
Materials
quantity of plutonium electrolyzed is calculated from the net
C1156 Guide for Establishing Calibration for a Measure-
number of coulombs required for the electrolysis, according to
ment Method Used to Analyze Nuclear Fuel Cycle Mate-
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Faraday’s law. Corrections for incomplete reaction, derived
rials
from the Nernst equation, must be applied for electrolysis of
the sample aliquot (7, 8).
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~Q 2 Q ! M
ThistestmethodisunderthejurisdictionofASTMCommitteeC-26onNuclear s b
W 5 (1)
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of nFf
Test.
Current edition approved Jan. 10, 1999. Published February 1999. Originally
published as C1108–88. Last previous edition C1108–93.
2 4
A Julie 100-V precision resistor number NB102A, accurate to 0.0015%, has Annual Book of ASTM Standards, Vol 14.02.
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been found satisfactory. Theboldfacenumbersinparenthesesrefertothelistofreferencesattheendof
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Annual Book of ASTM Standards, Vol 12.01. this test method.
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