Standard Active Last Updated: Dec 27, 2016
ASTM C697-16

Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium Dioxide Powders and Pellets

Significance and Use

4.1 Plutonium dioxide is used in mixtures with uranium dioxide as a nuclear-reactor fuel. In order to be suitable for this purpose, the material must meet certain criteria for plutonium content, isotopic composition, and impurity content. These test methods are designed to show whether or not a given material meets the specifications for these items as described in Specification C757.

4.1.1 An assay is performed to determine whether the material has the minimum plutonium content specified on a dry weight basis.

4.1.2 Determination of the isotopic content of the plutonium in the plutonium dioxide powder is made to establish whether the effective fissile content is in compliance with the purchaser's specifications.

4.1.3 Impurity content is determined to ensure that the maximum concentration limit of certain impurity elements is not exceeded. Determination of impurities is also required for calculation of the equivalent boron content (EBC) as described in Practice C1233.

4.2 Fitness for Purpose of Safeguards and Nuclear Safety Applications—Methods intended for use in safeguards and nuclear safety applications shall meet the requirements specified by Guide C1068 for use in such applications.


1.1 These test methods cover procedures for the chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade plutonium dioxide powders and pellets to determine compliance with specifications.

1.2 The analytical procedures appear in the following order:



Plutonium Sample Handling

  8 to 10

Plutonium by Controlled-Potential Coulometry


Plutonium by Ceric Sulfate Titration


Plutonium by Amperometric Titration with Iron(II)


Plutonium by Diode Array Spectrophotometry


Nitrogen by Distillation Spectrophotometry Using Nessler

11 to 18

Carbon (Total) by Direct Combustion–Thermal Conductivity

19 to 29

Total Chlorine and Fluorine by Pyrohydrolysis

30 to 37

Sulfur by Distillation Spectrophotometry

38 to 46

Plutonium Isotopic Analysis by Mass Spectrometry


Rare Earth Elements by Spectroscopy

47 to 54

Trace Elements by Carrier–Distillation Spectroscopy

55 to 62

(Alternative: Impurities by ICP-AES or ICP-MS)


Impurity Elements by Spark-Source Mass Spectrography

63 to 69

Moisture by the Coulometric Electrolytic Moisture Analyzer

70 to 77

Total Gas in Reactor-Grade Plutonium Dioxide Pellets


Plutonium-238 Isotopic Abundance by Alpha Spectrometry


Americium-241 in Plutonium by Gamma-Ray Spectrometry


Rare Earths By Copper Spark-Spectroscopy

78 to 87

Plutonium Isotopic Analysis by Mass Spectrometry

88 to 96

Oxygen-To-Metal Atom Ratio by Gravimetry

97 to 104

1.3 The values stated in SI units are to be regarded as 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. For specific precautionary statements, see Sections 6, 16.2.5, 44.7, 51.9 and 92.5.1.

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Book of Standards Volume: 12.01
Developed by Subcommittee: C26.05
Pages: 25
DOI: 10.1520/C0697-16
ICS Code: 27.120.30