ASTM C1909-21

Standard Test Method for Moisture Analysis of Plutonium Dioxide (PuO<inf>2</inf>) by Thermogravimetric Mass Spectrometry (TGA-MS)

SIGNIFICANCE AND USE
5.1 This test method is intended for use in quality control laboratories where a quantitative analysis of adsorbed moisture on a PuO2 sample is desired.  
5.2 The parameters described should be considered as guidelines. They may be altered to suit a particular analysis or type of analyzer, provided the changes are validated by the laboratory and noted in the report.  
5.3 The quantity of an adsorbed gas on a given PuO2 sample may indicate specific quality or end use performance characteristics. Specific limits on moisture content, for example, are required in cases where PuO2 will be packaged and stored for extended periods of time.
SCOPE
1.1 This test method provides necessary information to determine the total amount of moisture (physisorbed and chemisorbed water molecules) in a plutonium dioxide (PuO2) sample using a combination of thermogravimetric and mass spectrometric analyses. This test method is useful when performing analysis in cases where a maximum amount of moisture content in PuO2 samples has been agreed upon by interested parties. For example this method can be used to determine the moisture content of some types of PuO2 packaged to meet the requirements of DOE-STD-3013 (1),2 “Stabilization, Packaging, and Storage of Plutonium-Bearing Materials,” when such PuO2 meets the specifications given in this test method (2).  
1.2 This test method is applicable to PuO2 samples having the following characteristics: Plutonium mass fraction ≥ 83 % (the plutonium in the sample should be close to stoichiometric PuO2 which is approximately 88 wt% plutonium depending on the isotopic composition of the plutonium, but can have several weight percent impurities), moisture ≤1 %.  
1.3 The temperature range of test is typically room temperature to greater than 1000 °C. Typically the PuO2 is heated to 1100 °C.  
1.4 This test method utilizes an inert gas environment (argon, nitrogen, or helium).  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.7 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.

General Information

• Status: Published
• Publication Date: 31-May-2021
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

Standards Content (Sample)

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.
Designation: C1909 − 21
Standard Test Method for
Moisture Analysis of Plutonium Dioxide (PuO )by
2
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Thermogravimetric Mass Spectrometry (TGA-MS)
This standard is issued under the fixed designation C1909; 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 1.7 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 This test method provides necessary information to
ization established in the Decision on Principles for the
determine the total amount of moisture (physisorbed and
Development of International Standards, Guides and Recom-
chemisorbed water molecules) in a plutonium dioxide (PuO )
2
mendations issued by the World Trade Organization Technical
sample using a combination of thermogravimetric and mass
Barriers to Trade (TBT) Committee.
spectrometric analyses. This test method is useful when per-
forming analysis in cases where a maximum amount of
2. Referenced Documents
moisture content in PuO samples has been agreed upon by
2
3
2.1 ASTM Standards:
interested parties. For example this method can be used to
C859 Terminology Relating to Nuclear Materials
determine the moisture content of some types of PuO pack-
2
2 C1210 Guide for Establishing a Measurement System Qual-
aged to meet the requirements of DOE-STD-3013 (1),
ity Control Program for Analytical Chemistry Laborato-
“Stabilization, Packaging, and Storage of Plutonium-Bearing
ries Within Nuclear Industry
Materials,” when such PuO meets the specifications given in
2
E473 Terminology Relating to Thermal Analysis and Rhe-
this test method (2).
ology
1.2 This test method is applicable to PuO samples having
2
E967 Test Method for Temperature Calibration of Differen-
the following characteristics: Plutonium mass fraction ≥ 83 %
tial Scanning Calorimeters and Differential Thermal Ana-
(the plutonium in the sample should be close to stoichiometric
lyzers
PuO which is approximately 88 wt% plutonium depending on
2
E1142 Terminology Relating to Thermophysical Properties
theisotopiccompositionoftheplutonium,butcanhaveseveral
E1582 Test Method for Temperature Calibration of Thermo-
weight percent impurities), moisture ≤1%.
gravimetric Analyzers
1.3 Thetemperaturerangeoftestistypicallyroomtempera-
3. Terminology
ture to greater than 1000 °C. Typically the PuO is heated to
2
1100 °C.
3.1 Definitions:
3.1.1 Except as otherwise defined herein, definitions of
1.4 This test method utilizes an inert gas environment
terms are as given in Terminology C859, E473, and E1142.
(argon, nitrogen, or helium).
3.2 Definitions of Terms Specific to This Standard:
1.5 The values stated in SI units are to be regarded as
3.2.1 rotary riffler, n—a piece of laboratory equipment
standard. No other units of measurement are included in this
capable of subdividing large samples into smaller sub-samples
standard.
by means of vibration of the large sample into a rotating set of
1.6 This standard does not purport to address all of the
sub-sample containers.
safety concerns, if any, associated with its use. It is the
3.2.1.1 Discussion—This technique minimizes operator er-
responsibility of the user of this standard to establish appro-
ror and bias as compared with many other types of sample
priate safety, health, and environmental practices and deter-
dividing.
mine the applicability of regulatory limitations prior to use.
4. Summary of Test Method
4.1 This test method is an empirical technique using ther-
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This test method is under the jurisdiction ofASTM Committee C26 on Nuclear mogravimetry and mass spectrometry in which the mass of a
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
Test.
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Current edition approved June 1, 2021. Published July 2021. DOI: 10.1520/ For referenced ASTM standards, visit the ASTM website, www.astm.org, or
C1909-21. contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
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The boldface numbers in parentheses refer to a list of references at the end of Standards volume information, refer to the standard’s Document Summary page on
this standard. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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C1909 − 21
analyzer specific. Examples include heat rate, type of carrier gas, mass of
sample of PuO , heated at a controlled rate in a gaseous
2
sample,
...