Designation: C1408 − 16
Standard Test Method for
Carbon (Total) in Uranium Oxide Powders and Pellets By
Direct Combustion-Infrared Detection Method1
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
1.1 This test method covers the determination of carbon in (Gd2O3) Powder
nuclear-grade uranium oxide powders and pellets to determine C922 Specification for Sintered Gadolinium Oxide-Uranium
compliance with specifications. Dioxide Pellets
2.2 NIST Standard:3
1.2 Gadolinium oxide (Gd2O3) and gadolinium oxide-
NIST SRM 101G Standard Reference Materials—Stainless
uranium oxide powders and pellets may also be analyzed using
Steel
this test method.
1.3 This test method covers the determination of 5 to 500 µg 3. Terminology
of residual carbon. 3.1 Definitions—Except as otherwise defined herein, defini-
1.4 This test method describes an induction furnace carrier tions of terms are given in Terminology C859.
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
1.5 The values stated in SI units are to be regarded as melting point of the sample.
standard. No other units of measurement are included in this
standard. 4. Summary of Test Method
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
1.6 This standard does not purport to address all of the temperature of 1600 to 1700°C in a stream of oxygen. The
safety concerns, if any, associated with its use. It is the carbon in the sample is oxidized to primarily carbon dioxide
responsibility of the user of this standard to establish appro- (CO2) with some carbon monoxide (CO) formed. A catalyst
priate safety and health practices and determine the applica- converts the CO to CO2 and the products of combustion are
bility of regulatory limitations prior to use. scavenged free of sulfur compounds, halogens, and water
vapor. The CO2 is swept into an infrared cell detector. The
2. Referenced Documents amount of carbon is automatically determined from stored
2.1 ASTM Standards:2 calibration data, and is displayed or printed out, or both, by the
C753 Specification for Nuclear-Grade, Sinterable Uranium carbon analyzer.
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 CO2
stream.
1
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.
5. Significance and Use
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:
10.1520/C1408-16.
Gadolinium oxide is used as an additive to uranium dioxide. In
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at
[email protected]. For Annual Book of ASTM
3
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
1
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 mixture5, granular tin and iron chip mixture, or
designed to determine whether the carbon content meets high purity iron chip accelerators for increased combustion
Specifications C753, C776, C888, and C922. temperature. These materials are available in appropriate purity
and form from carbon analyzer vendors. The criterion for
6. Interferences satisfactory results is the absence of significant additional
carbon release upon recombustion of the specimen.
6.1 Contamination of carrier gas, crucibles, or samples with
extraneous sources of carbon may cause a positive bias. The 8.3 Cellulose Trap Packing—Surgical grade cotton or
blank correction will help to minimize the bias from carrier gas equivalent.
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(ClO4)2.
6.2 Powdered Gd2O3 samples may adsorb CO/CO2 from the 9. Carbon Standard Materials
atmosphere. Sample preheating to 120° for 2 h is 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
6.3 The purification system typically associated with the approximately 20 µg/g sample to 1500 µg/g sample have been
recommended combustion and detection equipment is de- found satisfactory.
signed to minimize other expected sources of interferences, 9.2 LECO6 or SYLAB steel standards7
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 CO2. Special scrubbers are used for found satisfactory.
halogens created during sample combustion.
10. Hazards and Precautions
7. Apparatus 10.1 Take proper safety precautions to prevent inhalation, or
ingestion of uranium dioxide powders or dust during grinding
7.1 Low-Carbon Analyzer, consisting of an induction-heated or handling operations.
furnace suitable for operation at 1600 to 1700°C, an infrared
detector for measuring carbon dioxide, and auxiliary purifica- 10.2 Operation of equipment presents electrical and thermal
tion systems. hazards. Follow manufacturer recommendations for safe op-
eration.
7.2 Crucibles, expendable alumina or similar refractory 10.3 This procedure uses hazardous chemicals. Use appro-
material. Both the crucible and cover, if used, must be priate precautions for handling corrosives, oxidizers, and
pre-ignited at a temperature of 1000°C or higher for a time gases.
sufficient to produce constant blank values.
11. Preparation of Apparatus
7.3 Muffle Furnace, capable of attaining temperature of
1000°C, for pre-igniting crucibles. 11.1 Change instrument column packing and reagents as
recommended by manufacturer.
7.4 Tongs and Forceps, for handling crucibles and lids.
11.2 Set the operating controls of the instrument system
7.5 Stainless Steel Scoops and Spatulas according to the operating instructions for the specific equip-
ment used.
8. Reagents and Materials 11.3 Condition the apparatus by combustion of several
8.1 Purity of Reagents—Reagent grade chemicals shall be blanks prepared with sample crucible and accelerator in the
used in all tests. Unless otherwise indicated, it is intended that amount to be used with the samples. Successive blanks should
all reagents shall conform to the specifications of the Commit- approach a constant value, allowing for normal statistical
tee on Analytical Reagents of the American Chemical Society, fluctuations.
where such specifications are available.4 Other grades may be 12. Calibration
used, provided it is first ascertained that the reagent is of
12.1 The calibration range and number of standards will
sufficiently high purity to permit its use without lessening the
depend upon the instrument used. Two to four standards
accuracy of the determination.
containing 50 to 600 µg carbon are recommended.
5
The sole source of supply of the apparatus, Lecocel accelerator, known to the
4
Reagent Chemicals, American Chemical Society Specifications, American committee at this time is LECO Corporation. If you are aware of alternative
Chemical Society, Washington, DC. For suggestions on the testing of reagents not suppliers, please provide this information to ASTM Headquarters. Your comments
listed by the American Chemical Society, see Analar Standards for Laboratory will receive careful consideration at a meeting of the responsible technical
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia committee,1 that you may attend.
6
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, LECO, 3000 Lakeview Ave. St. Joesph, Michigan 49085 USA.
7
MD. SYLAB, 11 Imp. Courtes patures, F57073 Metz Cedex, 03, France.
2
C1408 − 16
12.2 Add a volumetrically measured or weighed portion of mended operating conditions. (Combustion time will vary with
accelerator and weighed portion of standard to a pre-ignited the instrument used, but it is typically in the 30 to 120-s range.)
sample crucible. (The amount of accelerator will depend upon Record the result.
the instrument used and operating conditions.) 13.5 Remove the sample crucible and examine it for incom-
12.3 Load and combust the standards according to the plete combustion. The crucible contents should be a uniformly
manufacturer’s recommended operating conditions. fused mass. Results from incompletely fused samples shall not
be accepted.
12.4 Calibrate the instrument according to operating in-
structions. Calibration coefficients are normally stored in the 14. Calculation
microprocessor memory. 14.1 Calculate the carbon content as follows:
12.5 Recalibration frequency will depend upon the type of µg C per g of sample 5 ~ C s 2 C b ! /W (1)
instrument used. As a minimum, recalibration is required when where:
critical instrument components are changed, or when control
standards data indicate that the instrument is failing to meet Cs = micrograms of carbon in test specimen,
Cb = micrograms of carbon in a blank run, and
performance criteria.
W = grams of test specimen.
13. Procedure 14.2 For samples requiring carbon results expressed as µg
carbon per g U, convert results to uranium basis as follows:
13.1 Crush pellet samples to obtain approximately 1-mm
C µg/g 3 100
(18 mesh) particles. (The particle size required may vary C, µg/g U basis 5 (2)
% U content of sample
according to the instrument used and operating conditions.)
15. Precision and Bias
13.2 Measure or weigh accelerator into a pre-ignited sample
crucible. (The amount of accelerator will depend upon the 15.1 The precision data for NIST 101G, primary steel
instrument used and operating conditions. This needs to remain standard was collected by multiple operators over a one year
constant to ensure proper accuracy and precision. Varying the period using one instrument. As the data are dependent upon
load is a source of bias.) the instrument used and operating conditions, each laboratory
will need to determine its own statistics.
13.3 Weigh a portion of sample, (0.3 g to 2 g is suggested,
depending upon the instrument model) to the nearest 0.01 g, 15.2 The precision data for Uranium Oxide Powder Work-
into the crucible. The sample size should be chosen to provide ing Standard was collected by multiple operators over a one
adequate sensitivity and accuracy at low carbon year period using one instrument.
concentrations, but should contain less than 200 µg of carbon. 16. Keywords
13.4 Load the crucible into the induction furnace and 16.1 carbon content; gadolinium oxide; gadolinium oxide-
combust the sample according to the manufacturer’s recom- uranium oxide; impurity content; uranium oxide
3
C1408 − 16
TABLE 1 Bias Estimate for Carbon
Sample Concentration (µg/g) Relative Standard Standard Deviation Bias Estimate (µg/g) Relative Difference Number of
Deviation (%) (µg/g) Determinations
NIST 101G 136 3.4 4.6 +1.9 1.4 % 45
Uranium Oxide
Powder Working 36 8.0 2.9 +2.5 7.0 % 214
Standard
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