ASTM C1517-16

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Designation: C1517 − 09 C1517 − 16
Standard Test Method for
Determination of Metallic Impurities in Uranium Metal or
Compounds by DC-Arc Emission Spectroscopy
This standard is issued under the fixed designation C1517; 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 describes the steps necessary for the preparation and determination of impurity metals in uranium metal
and uranium compounds by DC arc emission spectroscopy.
1.2 The method is valid for those materials that can be dissolved in acid and/oror converted to an oxide in a muffle furnace
furnace, or both (see Practice C1347).
1.3 This method uses the carrier distillation technique to selectively carry the impurities into the arc, leaving the uranium oxide
in the electrode. If it is necessary to determine the carrier metal(usually metal (usually a silver or strontium, or gallium compound)
as an impurity, another technique must be chosen for that element.
1.4 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.5 This standard may involve hazardous materials, operations and equipment. 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
C761 Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Uranium
Hexafluoride
C776 Specification for Sintered Uranium Dioxide Pellets
C788 Specification for Nuclear-Grade Uranyl Nitrate Solution or Crystals
C859 Terminology Relating to Nuclear Materials
C967 Specification for Uranium Ore Concentrate
C1347 Practice for Preparation and Dissolution of Uranium Materials for Analysis
E130 Practice for Designation of Shapes and Sizes of Graphite Electrodes (Withdrawn 2013)
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
3. Terminology
3.1 See definitions and terms Except as otherwise defined herein, definitions of terms are as given in Terminologies C859 and
E135.
4. Summary of Test Method
4.1 Uranium metal, solutions and compounds are converted to uranium oxide (U O ) in a muffle furnace. A weighed amount
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of the oxide is mixed with an appropriate spectrographic carrier and loaded into a graphite electrode. The electrode is excited in
a DC arc and the light is dispersed by a spectrograph or spectrometer. The resulting spectrum is measured electronically using a
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, 2009April 1, 2016. Published July 2009May 2016. Originally approved in 2002. Last previous edition approved in 20022009 as
C1517 – 02.C1517 – 09. DOI: 10.1520/C1517-09.10.1520/C1517-16.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
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C1517 − 16
CCD, CID, or CMOS camera or photographed on photographic plates or film sensitive to the proper regions. The line intensities
are compared directly to standard plates or to calibration curves derived from the arced standards.
5. Significance and Use
5.1 This test method is applicable to uranium metal, uranium oxides and compounds soluble in nitric or sulfuric acid, and
uranium solutions which can be converted to uranium oxide (U O ) in a muffle furnace. It may be used to determine the impurities
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in uranium compounds as listed in Specifications C753, C776, C788, and C967.
6. Apparatus
6.1 Spectrograph or Spectrometer—A spectrograph with sufficient resolving power and linear dispersion to separate the
analytical lines from other lines in the spectrum of the sample in the spectral region of 230.0230 to 855.0855 nm is required. Some
spectrographs may be able to access wavelengths lower than 230 nm that may allow the determination of other analytes.
Instruments with a reciprocal linear dispersion in the first order of 0.5 nm/mm or less are satisfactory. A direct-reading spectrometer
of comparable quality may be substituted for equipment listed, in which case the directions given by the manufacturer should be
substituted for those in this procedure.The spectrometer should include a CCD, CID, or CMOS camera for electronic measurement
of the resulting spectrum.
6.2 Excitation Source—Use an arc power source capable of providing a dc arc of up to 14-A dc, depending on the carrier used
and electrode design.
6.3 Excitation Stand—Conventional type with adjustable water-cooled electrode holders (may be fitted with automatic sample
changers if desired).
6.4 Photographic Processing Equipment—Use developing, fixing, washing and drying equipment.
6.5 Microphotometer, having a precision of at least 6 1 % for transmittances.
6.4 Mixer, for dry materials.
6.5 Platinum Crucible.
6.6 Venting Tool, (see Fig. 8, Test Methods C761). – 01).
6.7 Muffle Furnace, 1000°C capability.
7. Reagents and Materials
7.1 Purity of Materials—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the Committee of 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.
7.2 Electrodes—The anode and counter electrodes should be of the S-2, S 16 and C-1 types as given in Practice E130 (or
equivalent).
NOTE 1—Exact shapes and dimensions of the electrodes are not as critical as given in Practice E130; however, dimensions of the electrodes used should
be consistent and it is essential that the same dimension electrodes be used for standards and samples.
7.3 Photographic Processing Solutions—Prepare solutions as noted in available literature (1,2).
7.4 Photographic Film/Plates—Use photo emulsion SA-1 and 1-N or equivalent.
7.5 Powder Paper.
7.3 Nitric Acid (HNO )—concentrated (70 %), electronic grade, or equivalent.
7.4 Sulfuric Acid (H SO )—concentrated, electronic grade, or equivalent.
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7.5 Spectrographic Carrier—The following spectrographic carriers have been used successfully for DC Arc analysis:
7.5.1 Silver Chloride-Lithium Fluoride, 11:1 w/w ratio.
7.5.2 Silver Chloride-Silver Fluoride, 4:1 w/w ratio.
7.5.3 Gallium Oxide, 99.99 % or better.
7.5.4 Silver Chloride-Strontium Fluoride, 16.4 mol % SrF in AgCl.
7.5.5 Gallium Oxide-Lithium Fluoride, 11:1 w/w ratio.
7.6 Mixing Vial, plastic, 12.7 mm (1/2 in.) by 25.4 mm (1 in.) with cap and 10 mm (3/8 in.) plastic mixing bead.
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 Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
C1517 − 16
TABLE 1 Carrier—Sample Combinations
Carrier Carrier Wt, Oxide Wt, Electrode Mixing Time,
Material (mg) (mg) Charge, (mg) (s)
AgCl/AgF 50 250 50 180
(4:1)
AgCl/LiF 30 270 100 60
(11:1)
AgCl/SrF 50 450 100 30
(~6:1)
Ga O /LiF 20 380 100 25
2 3
(11:1)
A
Ga O 7 343 100 60
2 3
A
For the determination of Ag and Li only.
4 3
7.7 Standard Uranium Oxide (U O ) Diluent—Use NBL CRM 129 (or its replacement or equivalent) of known impurity level
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as a diluent.
8. Precautions
8.1 Consult manufacturer’s Material Safety Data Sheets (MSDS)(SDS) for chemical incompatibilities, specific hazards, or spill
cleanup for any hazardous materials used in this method.
8.2 All mixing and weighing operations involving uranium oxides should be carried out in properly functioning hoods or
exhaust boxes.gloveboxes.
9. Standardization and Calibration
9.1 Standards:
9.1.1 Standards may be synthesized by adding the impurity elements to purified U O (NBL CRM 129129-A , or equivalent)
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and homogenizing. Impurities in powder form, preferably as oxides, may be blended in U O ; impurities in solution may be added
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to U O and the mixture dried, blended and reignited, or the impurities and uranium may be combined in solution and reconverted
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to U O . The individual elements should grade in such a ratio as to facilitate visual comparisons covering the desired analytical
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range for each.
9.1.2 The compounds used to make U O impurity standards should be of the highest purity available.
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9.1.3 Alternatively, commercially available uranium impurity standards, such as NBL CRM 123 and 124 series standards, may
be used. (Other standards may be available; the user should determine quality and/or applicability or applicability, or both, prior
to use.) These may be supplemented by synthetic standards to extend calibration ranges, if necessary.
9.1.4 For each standard used, prepare in the same ratio of uranium oxide to carrier as for samples (see Table 1 for further
details).
9.1.5 Charge the electrode and arc at the same conditions as determined to be optimum for the instrument in use.
9.2 Calibration Curves:
9.2.1 If a microphotometer is used, determine emulsi
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