ASTM C1408-16

Standard Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method

SIGNIFICANCE AND USE
5.1 Uranium dioxide is used as a nuclear-reactor fuel. Gadolinium oxide is used as an additive to uranium dioxide. In order to be suitable for this purpose, these materials must meet certain criteria for impurity content. This test method is designed to determine whether the carbon content meets Specifications C753, C776, C888, and C922.
SCOPE
1.1 This test method covers the determination of carbon in nuclear-grade uranium oxide powders and pellets to determine compliance with specifications.  
1.2 Gadolinium oxide (Gd2O3) and gadolinium oxide-uranium oxide powders and pellets may also be analyzed using this test method.  
1.3 This test method covers the determination of 5 to 500 μg of residual carbon.  
1.4 This test method describes an induction furnace carrier gas combustion system equipped with an infrared detector. It may also be applied to a similar instrument equipped with a thermal conductivity detector.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5.1 The preferred system of units is micrograms carbon per gram of sample (μg/g sample) or micrograms carbon per gram of uranium (μg/g U).  
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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Published
• Publication Date: 29-Feb-2016
• ICS: 27.120.30 - Fissile materials and nuclear fuel technology
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

Relations

• Replaces: ASTM C1408-09 - Standard Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method
• Effective Date: 01-Mar-2016
• Refers: ASTM C859-24 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Jan-2024
• Refers: ASTM C888-18 - Standard Specification for Nuclear-Grade Gadolinium Oxide (Gd<inf>2</inf>O<inf>3</inf >) Powder
• Effective Date: 01-Jun-2018
• Refers: ASTM C753-16 - Standard Specification for Nuclear-Grade, Sinterable Uranium Dioxide Powder
• Effective Date: 01-Feb-2016
• Refers: ASTM C859-14a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Jun-2014
• Refers: ASTM C859-14 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Jan-2014
• Refers: ASTM C888-03(2014) - Standard Specification for Nuclear-Grade Gadolinium Oxide &#40;Gd<inf>2</inf>O<inf>3</inf >&#41; Powder
• Effective Date: 01-Jan-2014
• Refers: ASTM C859-13a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Jun-2013
• Refers: ASTM C859-13 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-May-2013
• Refers: ASTM C776-06(2011) - Standard Specification for Sintered Uranium Dioxide Pellets
• Effective Date: 01-Jun-2011
• Refers: ASTM C859-10b - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Nov-2010
• Refers: ASTM C859-10a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Aug-2010
• Refers: ASTM C859-10 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Feb-2010
• Refers: ASTM C859-09 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Feb-2009
• Refers: ASTM C888-03(2008) - Standard Specification for Nuclear-Grade Gadolinium Oxide (Gd₂O₃) Powder
• Effective Date: 01-Dec-2008

Overview

ASTM C1408-16: Standard Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method specifies procedures for the accurate measurement of total carbon content in nuclear-grade uranium oxide powders, pellets, and related materials. This method is an essential quality control tool for the nuclear fuel cycle, enabling producers and users to confirm compliance with stringent impurity limits set by regulatory specifications. Its adoption ensures reliability and safety in nuclear reactor fuel materials by monitoring residual carbon, which could impact material performance.

Key Topics

• Scope and Applicability

  • Applies to uranium oxide powders and pellets intended for use as nuclear reactor fuel
  • Covers analysis of gadolinium oxide and gadolinium oxide-uranium oxide mixtures
  • Measures residual carbon in the range of 5 to 500 micrograms (µg)
  • Supports compliance with important specifications: ASTM C753, C776, C888, and C922

• Analytical Method

  • Utilizes induction furnace/carrier gas combustion at 1600-1700°C
  • Detects carbon via infrared (IR) detection of carbon dioxide formed during combustion
  • Can be adapted to instruments with thermal conductivity detectors
  • Requires stringent control of reagents and apparatus to minimize contamination or analytical bias

• Sample Preparation and Precautions

  • Requires precise sample and reagent weighing to ensure accuracy
  • Includes procedures for pre-igniting crucibles and using accelerators to guarantee complete combustion
  • Highlights safety practices for handling radioactive and hazardous materials

• Calibration and Quality Assurance

  • Employs certified reference materials (NIST SRMs, steel standards)
  • Instrument calibration and regular quality checks are essential for reliable data

Applications

• Nuclear Fuel Fabrication

  • Ensures uranium dioxide and gadolinium oxide-uranium oxide fuels meet impurity limits for safe, efficient reactor operation
  • Verifies conformity of fuel powder and pellets before and after sintering

• Quality Assurance in Analytical Laboratories

  • Provides standardized methodology for regulatory compliance and customer assurance
  • Supports laboratories performing impurity testing for nuclear-grade materials

• Research and Development

  • Offers a reproducible analytical method for investigating process optimization and material purity in nuclear material R&D

• Regulatory Compliance

  • Critical for material release, validation, and traceability when meeting national and international nuclear fuel specifications

Related Standards

Organizations using ASTM C1408-16 may also reference or be required to meet additional key standards, including:

• ASTM C753 - Specification for Nuclear-Grade, Sinterable Uranium Dioxide Powder
• ASTM C776 - Specification for Sintered Uranium Dioxide Pellets
• ASTM C888 - Specification for Nuclear-Grade Gadolinium Oxide (Gd₂O₃) Powder
• ASTM C922 - Specification for Sintered Gadolinium Oxide-Uranium Dioxide Pellets
• ASTM C859 - Terminology Relating to Nuclear Materials

Keywords: carbon content, uranium oxide, nuclear fuel, gadolinium oxide, impurity analysis, combustion-infrared detection, ASTM C1408, fuel pellet quality, nuclear-grade materials, regulatory compliance

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: C1408 − 16
Standard Test Method for
Carbon (Total) in Uranium Oxide Powders and Pellets By
Direct Combustion-Infrared Detection Method
This standard is issued under the fixed designation C1408; 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 C888 Specification for Nuclear-Grade Gadolinium Oxide
(Gd O ) Powder
2 3
1.1 This test method covers the determination of carbon in
C922 Specification for Sintered Gadolinium Oxide-Uranium
nuclear-grade uranium oxide powders and pellets to determine
Dioxide Pellets
compliance with specifications.
2.2 NIST Standard:
1.2 Gadolinium oxide (Gd O ) and gadolinium oxide-
2 3
NIST SRM 101G Standard Reference Materials—Stainless
uranium oxide powders and pellets may also be analyzed using
Steel
this test method.
3. Terminology
1.3 Thistestmethodcoversthedeterminationof5to500µg
of residual carbon.
3.1 Definitions—Except as otherwise defined herein, defini-
tions of terms are given in Terminology C859.
1.4 This test method describes an induction furnace carrier
gas combustion system equipped with an infrared detector. It
3.2 Definitions of Terms Specific to This Standard:
may also be applied to a similar instrument equipped with a
3.2.1 accelerator—an igniter and a flux which promotes
thermal conductivity detector.
both combustion and a fluid melt by effectively lowering the
melting point of the sample.
1.5 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Summary of Test Method
standard.
1.5.1 The preferred system of units is micrograms carbon
4.1 The powered or crushed test specimen and an appropri-
per gram of sample (µg/g sample) or micrograms carbon per
ate accelerator (metal flux) are added to a crucible, placed
gram of uranium (µg/g U).
within an induction-heated furnace and burned at a nominal
temperature of 1600 to 1700°C in a stream of oxygen. The
1.6 This standard does not purport to address all of the
carbon in the sample is oxidized to primarily carbon dioxide
safety concerns, if any, associated with its use. It is the
(CO ) with some carbon monoxide (CO) formed. A catalyst
responsibility of the user of this standard to establish appro- 2
converts the CO to CO and the products of combustion are
priate safety and health practices and determine the applica-
scavenged free of sulfur compounds, halogens, and water
bility of regulatory limitations prior to use.
vapor. The CO is swept into an infrared cell detector. The
2. Referenced Documents amount of carbon is automatically determined from stored
calibration data, and is displayed or printed out, or both, by the
2.1 ASTM Standards:
carbon analyzer.
C753 Specification for Nuclear-Grade, Sinterable Uranium
Dioxide Powder
4.2 The actual configuration of the system may vary with
C776 Specification for Sintered Uranium Dioxide Pellets vendor and model. Typical systems include columns of mate-
C859 Terminology Relating to Nuclear Materials rials such as copper oxide, platinized silica gel, magnesium
perchlorate, sodium hydroxide, and cellulose to purify the CO
stream.
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
5. Significance and Use
Test.
Current edition approved March 1, 2016. Published March 2016. Originally
5.1 Uranium dioxide is used as a nuclear-reactor fuel.
approved in 1998. Last previous edition approved in 2009 as C1408 – 09. DOI:
Gadolinium oxide is used as an additive to uranium dioxide. In
10.1520/C1408-16.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on Available from National Institute of Standards and Technology (NIST), 100
the ASTM website. Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http://www.nist.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1408 − 16
order to be suitable for this purpose, these materials must meet 8.2 Accelerators—Copper metal and iron chip mixture,
certain criteria for impurity content. This test method is tin-tungsten mixture , granular tin and iron chip mixture, or
high purity iron chip accelerators for increased combustion
designed to determine whether the carbon content meets
Specifications C753, C776, C888, and C922. temperature.Thesematerialsareavailableinappropriatepurity
and form from carbon analyzer vendors. The criterion for
satisfactory results is the absence of significant additional
6. Interferences
carbon release upon recombustion of the specimen.
6.1 Contamination of carrier gas, crucibles, or samples with
8.3 Cellulose Trap Packing—Surgical grade cotton or
extraneous sources of carbon may cause a positive bias. The
equivalent.
blankcorrectionwillhelptominimizethebiasfromcarriergas
and crucibles. Interference from absorbed carbon on samples 8.4 Carbon Dioxide and Moisture Absorbents—Sodium hy-
may be eliminated by keeping the sample in an inert atmo- droxide (NaOH) on an inert support and magnesium perchlo-
sphere or vacuum. rate (Mg(ClO ) .
4 2
6.2 PowderedGd O samplesmayadsorbCO/CO fromthe 9. Carbon Standard Materials
2 3 2
atmosphere. Sample preheating to 120° for2his recom-
9.1 NIST SRM steel standards or equivalent:
mended in this case.
9.1.1 The 101, 131, 133, 339, and 343 series, ranging from
approximately 20 µg/g sample to 1500 µg/g sample have been
6.3 The purification system typically associated with the
found satisfactory.
recommended combustion and detection equipment is de-
6 7
signed to minimize other expected sources of interferences,
9.2 LECO or SYLAB steel standards
such as sulfur, halogens, and water. The external/auxiliary 9.2.1 The 1 g steel pin standards or steel rings, ranging from
purification systems are designed to minimize/remove
approximately 5 µg⁄g sample to 500 µg⁄g sample have been
hydrocarbons, water, and CO . Special scrubbers are used for found satisfactory.
halogens created during sample combustion.
10. Hazards and Precautions
10.1 Takepropersafetyprecautionstopreventinhalation,or
7. Apparatus
ingestion of uranium dioxide powders or dust during grinding
7.1 Low-CarbonAnalyzer,consistingofaninduction-heated
or handling operations.
furnace suitable for operation at 1600 to 1700°C, an infrared
10.2 Operation of equipment presents electrical and thermal
detector for measuring carbon dioxide, and auxiliary purifica-
hazards. Follow manufacturer recommendations for safe op-
tion systems.
eration.
7.2 Crucibles, expendable alumina or similar refractory
10.3 This proced
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: C1408 − 09 C1408 − 16
Standard Test Method for
Carbon (Total) in Uranium Oxide Powders and Pellets By
Direct Combustion-Infrared Detection Method
This standard is issued under the fixed designation C1408; 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
1.1 This test method covers the determination of carbon in nuclear-grade uranium oxide powders and pellets to determine
compliance with specifications.
1.2 Gadolinium oxide (Gd O ) and gadolinium oxide-uranium oxide powders and pellets may also be analyzed using this test
2 3
method.
1.3 This test method covers the determination of 5 to 500 μg of residual carbon.
1.4 This test method describes an induction furnace carrier gas combustion system equipped with an infrared detector. It may
also be applied to a similar instrument equipped with a thermal conductivity detector.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5.1 The preferred system of units is micrograms carbon per gram of sample (μg/g sample) or micrograms carbon per gram
of uranium (μg/g U).
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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
C753 Specification for Nuclear-Grade, Sinterable Uranium Dioxide Powder
C776 Specification for Sintered Uranium Dioxide Pellets
C859 Terminology Relating to Nuclear Materials
C888 Specification for Nuclear-Grade Gadolinium Oxide (Gd O ) Powder
2 3
C922 Specification for Sintered Gadolinium Oxide-Uranium Dioxide Pellets
2.2 NIST Standard:
NIST SRM 101G Standard Reference Materials—Stainless Steel
3. Terminology
3.1 Definitions—Except as otherwise defined herein, definitions of terms are given in Terminology C859.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 accelerator—an igniter and a flux which promotes both combustion and a fluid melt by effectively lowering the melting
point of the sample.
4. Summary of Test Method
4.1 The powered or crushed test specimen and an appropriate accelerator (metal flux) are added to a crucible, placed within an
induction-heated furnace and burned at a nominal temperature of 1600 to 1700°C in a stream of oxygen. A catalyst converts the
carbon monoxide (CO) to The carbon in the sample is oxidized to primarily carbon dioxide (CO ) with some carbon monoxide
This test method is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test.
Current edition approved June 1, 2009March 1, 2016. Published July 2009March 2016. Originally approved in 1998. Last previous edition approved in 20042009 as
C1408 – 98 (2004).C1408 – 09. DOI: 10.1520/C1408-09.10.1520/C1408-16.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Available from National Institute of Standards and Technology (NIST), 100 Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http://www.nist.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1408 − 16
(CO) formed. A catalyst converts the CO to CO and the products of combustion are scavenged free of sulfur compounds, halogens,
and water vapor. The CO is swept into an infrared cell detector. The amount of carbon is automatically determined from stored
calibration data, and is displayed or printed out, or both, by the carbon analyzer.
4.2 The actual configuration of the system may vary with vendor and model. Typical systems include columns of materials such
as copper oxide, platinized silica gel, magnesium perchlorate, sodium hydroxide, and cellulose to purify the CO stream.
5. Significance and Use
5.1 Uranium dioxide is used as a nuclear-reactor fuel. Gadolinium oxide is used as an additive to uranium dioxide. In order to
be suitable for this purpose, these materials must meet certain criteria for impurity content. This test method is designed to
determine whether the carbon content meets Specifications C753, C776, C888, and C922.
6. Interferences
6.1 Contamination of carrier gas, crucibles, or samples with extraneous sources of carbon may cause a positive bias. The blank
correction will help to minimize the bias from carrier gas and crucibles. Interference from absorbed carbon on samples may be
eliminated by keeping the sample in an inert atmosphere or vacuum.
6.2 Powdered Gd O samples may adsorb CO/CO from the atmosphere. Sample preheating to 120° for 2 h is recommended
2 3 2
in this case.
6.3 The purification system typically associated with the recommended combustion and detection equipment is designed to
minimize other expected sources of interferences, such as sulfur, halogens, and water. The external/auxiliary purification systems
are designed to minimize/remove hydrocarbons, water, and CO . Special scrubbers are used for halogens created during sample
combustion.
7. Apparatus
7.1 Low-Carbon Analyzer, consisting of an induction-heated furnace suitable for operation at 1600 to 1700°C, an infrared
detector for measuring carbon dioxide, and auxiliary purification systems.
7.2 Crucibles, expendable alumina or similar refractory material. Both the crucible and cover, if used, must be pre-ignited at
a temperature of 1000°C or higher for a time sufficient to produce constant blank values.
7.3 Muffle Furnace, capable of attaining temperature of 1000°C, for pre-igniting crucibles.
7.4 Tongs and Forceps, for handling crucibles and lids.
7.5 Stainless Steel Scoops and Spatulas
8. Reagents and Materials
8.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
8.2 Accelerators—Copper metal, metal and iron chip mixture, tin-tungsten mixture , copper oxide, granular tin, and tin and iron
chip mixture, or high purity iron chip accelerators for increased combustion temperature. These materials are available in
appropriate purity and form from carbon analyzer vendors. The criterion for satisfactory results is the absence of significant
additional carbon release upon recombustion of the specimen.
8.3 Cellulose Trap Packing—Surgical grade cotton or equivalent.
8.4 Carbon Dioxide and Moisture Absorbents—Sodium hydroxide (NaOH) on a fibrousan inert support and magnesium
perchlorate (Mg(ClO ) .
4 2
9. Carbon Standard Materials
9.1 NIST SRM steel standards or equivalent:
9.1.1 The 101, 131, 133, 339, and 343 series, ranging from approximately 20 μg/g sample to 1500 μg/g sample have been found
satisfactory.
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see
...