ASTM C889-99
(Test Method)Standard Test Methods for Chemical and Mass Spectrographic Analysis of Nuclear-Grade Gadolinium Oxide (Gd2O3) Powder
Standard Test Methods for Chemical and Mass Spectrographic Analysis of Nuclear-Grade Gadolinium Oxide (Gd<sub>2</sub>O<sub>3</sub>) Powder
SCOPE
1.1 These test methods cover procedures for the chemical and mass spectrographic analysis of nuclear-grade gadolinium oxide powders to determine compliance with specifications.
1.2 The analytical procedures appear in the following order: Sections Carbon by Direct Combustion---Thermal Conductivity 7 to 16 Total Chlorine and Fluorine by Pyrohydrolysis Ion- 17 to 23 Selective Electrode Loss of Weight on Ignition 24 to 30 Sulfur by Combustion---Iodometric Titration 31 to 38 Impurity Elements by a Spark-Source Mass Spectrographic 39 to 45 Gadolinium Content in Gadolinium Oxide by Impurity 46 to 49 Correction
1.2 This standard does not purport to address all of the safety problems 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 hazard statements, see Section 5.
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Designation:C889–99
Standard Test Methods for
Chemical and Mass Spectrographic Analysis of Nuclear-
Grade Gadolinium Oxide (Gd O ) Powder
2 3
This standard is issued under the fixed designation C 889; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope C 1287 Test Method for Determination of Impurities In
Uranium Dioxide By Inductively Coupled Plasma Mass
1.1 These test methods cover procedures for the chemical
Spectrometry
and mass spectrographic analysis of nuclear-grade gadolinium
D 1193 Specification for Reagent Water
oxide powders to determine compliance with specifications.
E 115 Practice for Photographic Processing in Optical
1.2 The analytical procedures appear in the following order:
Emission Spectrographic Analysis
Sections
E 116 Practice for Photographic Photometry in Spectro-
Carbon by Direct Combustion—Thermal Conductivity
C 1408 Test Method for Carbon (Total) in Uranium Oxide
chemical Analysis
Powders and Pel lets By Direct Combustion-Infrared Detec-
E 130 Practice for Designation of Shapes and Sizes of
tion Method
Graphite Electrodes
Total Chlorine and Fluorine by Pyrohydrolysis Ion— 7-13
Selective Electrode
C 1408 Test Method for Carbon (Total) in Uranium Oxide
Loss of Weight on Ignition 14-20
Powders and Pel lets By Direct Combustion-Infrared
Sulfur by Combustion—Iodometric Titration
Impurity Elements by a Spark-Source Mass Spectrographic Detection Method
C 761 Test Methods for Chemical, Mass Spectrometric,
Spectrochemical,Nuclear, and Radiochemical Analysis of
3. Significance and Use
Uranium Hexafluoride
C 1287 Test Method for Determination of Impurities In Ura- 3.1 Gadolinium oxide powder is used, with subsequent
nium Dioxide By Inductively Coupled Plasma Mass Spec-
processing, in nuclear fuel applications, such as an addition to
trometry
uranium dioxide.These test methods are designed to determine
Gadolinium Content in Gadolinium Oxide by Impurity 21-24
Correction whether the material meets the requirements described in
Specification C 888.
1.3 This standard does not purport to address all of the
3.1.1 The material is analyzed to determine whether it
safety concerns, if any, associated with its use. It is the
contains the minimum gadolinium oxide content specified.
responsibility of the user of this standard to establish appro-
3.1.2 The loss on ignition and impurity content are deter-
priate safety and health practices and determine the applica-
mined to ensure that the weight loss and the maximum
bility of regulatory limitations prior to use. For specific hazard
concentration limit of specified impurity elements are not
statements, see Section 5.
exceeded.
2. Referenced Documents
4. Reagents
2.1 ASTM Standards:
4.1 Purity of Reagents—Reagent grade chemicals shall be
C 696 Test Methods for Chemical, Mass Spectrometric, and
used in all tests. Unless otherwise indicated, it is intended that
Spectrochemical Analysis of Nuclear-Grade Uranium Di-
all reagents shall conform to the specifications of the Commit-
oxide Powders and Pellets
tee onAnalytical Reagents of theAmerican Chemical Society,
C 761 Test Methods for Chemical, Mass Spectrometric,
where such specifications are available. Other grades may be
Spectrochemical,Nuclear, and Radiochemical Analysis of
3 used, provided it is first ascertained that the reagent is of
Uranium Hexafluoride
sufficiently high purity to permit its use without lessening the
C 888 Specification for Nuclear-Grade Gadolinium Oxide
3 accuracy of the determination.
(Gd O ) Powder
2 3
1 4
These test methods are under the jurisdiction of ASTM Committee C-26 on Annual Book of ASTM Standards, Vol 11.01.
Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Annual Book of ASTM Standards, Vol 03.05.
Methods of Test. “Reagent Chemicals,American Chemical Society Specifications,”Am. Chemi-
Current edition approved Jan. 10, 1999. Published March 1999. Originally cal Soc., Washington, DC. For suggestions on the testing of reagents not listed by
published as C 889 – 78. Last previous edition C 889 – 90. theAmerican Chemical Society, see “Reagent Chemicals and Standards,” by Joseph
Discontined January 1999. See C 889–90. Rosin, D. Van Nostrand Co., Inc., New York, NY, and the “United States
Annual Book of ASTM Standards, Vol 12.01. Pharmacopeia.”
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C889
4.2 Purity of Water—Unless otherwise indicated, references 9. Apparatus
to water shall be understood to mean reagent water as defined
9.1 Pyrohydrolysis Equipment—A suitable assembly of ap-
in Specification D 1193.
paratus as shown in Fig. 1.
9.1.1 Gas Flow Regulator and Flowmeter.
5. Hazards
9.1.2 Hot Plate, used to warm the water saturating the
5.1 Proper precautions should be taken to prevent inhalation sparge gas to 50 to 80°C.
or ingestion of gadolinium oxide powders or dust during 9.1.3 Combustion Tube Furnace, having a bore of about 32
grinding or handling operations. mm (1 ⁄4in.), a length of about 305 mm (12 in.), and the
5.2 Workers should observe precautions as specified in capability of maintaining a temperature of 1000°C.
vendor supplied Material Safety Data Sheets (MSDS).
9.1.4 Quartz Reaction Tube (Fig. 2)—The exit end should
not extend over 51 mm (2 in.) beyond the furnace with a
6. Sampling
ground joint connecting to the delivery tube. The delivery tube
extendsintoapolyethyleneabsorptionvesselwithatipcapable
6.1 Criteria for sampling this material are given in Specifi-
of giving a stream of fine bubbles.
cation C 888.
9.1.5 Combustion Boat—A ceramic, platinum, or quartz
boat with a 10-mL capacity, 89 to 102 mm (3 ⁄2 to 4 in.) long,
CARBON BY DIRECT COMBUSTION—
1 3
12.7 mm ( ⁄2 in.) wide, and 9.53 mm ( ⁄8 in.) high.
THERMAL CONDUCTIVITY
9.1.6 Absorption Vessel—A 50-mL polyethylene graduate
This Test Method was discontinued in January 1999 and
or tube is satisfactory.
replaced by C1408
9.2 Ion-Selective Electrodes—A chloride-ion-selective ac-
8 9
tivity electrode; fluoride-ion-selective activity electrode.
TOTAL CHLORINE AND FLUORINE BY
9.3 pH Meter and Double-Junction Reference Electrode,
PYROHYDROLYSIS ION—SELECTIVE ELECTRODE
such as a mercuric sulfate, sleeve junction type. The meter
should have an expandable scale with a sensitivity of 1 mV.
7. Scope
9.4 Magnetic Stirrer.
7.1 This test method covers the determination of chlorine
9.5 Beakers, 50-mL, polyethylene.
and fluorine in nuclear-grade gadolinium oxide (Gd O ) pow-
2 3
der.Witha1to 10-g sample of Gd O , concentrations of 5 to
10. Reagents
2 3
200 µg of chlorine and 1 to 200 µg of fluorine per gram of
10.1 Accelerator, U O (Halogen-free), can be used, but a
3 8
Gd O are determined without interference.
2 3
flux of sodium tungstate (Na WO ) with tungsten trioxide
2 4
(WO ) may be used to advantage (1). (See Method C 696.)
8. Summary of Test Method
Special preparation of the mixture is necessary, that is, dehy-
8.1 The halogens are separated from powdered gadolinium
drate 165 g of Na WO in a large platinum dish. Transfer the
2 4
oxide by pyrohydrolysis in a quartz tube with a stream of wet
dried material to a mortar, add 116 g of WO , and grind the
oxygen at a temperature of 900 to 1000°C (1, 2, 3, 4).
mixture to ensure good mixing. Transfer the mixture into a
Chlorine and fluorine are volatilized simultaneously as acids,
platinum dish and heat with a burner for 2 h. Cool the melt,
absorbed in a buffer solution as chloride and fluoride, and
transferthefluxtoamortar,andgrindtoacoarsepowder.Store
measured with ion-selective electrodes (4, 5, 6).
the flux in an airtight bottle. Mix about 8 g of flux with each
portion of sample to be pyrohydrolyzed.
The Orion Model No. 96–17 has been found satisfactory.
The Orion Model No. 9409 has been found satisfactory.
The boldface numbers in parentheses refer to the list of references appended to
this standard.
FIG. 1 Pyrohydrolysis of Gadolinium Oxide
C889
FIG. 2 Quartz Reaction Tube
10.2 Buffer Solution (0.001 N)—Dissolve 0.1 g of potas- and collection tube with a minimum of buffer solution. Make
sium acetate (KC H O ) in water, add 0.050 mL of acetic acid uptovolume.Use10-mLaliquotsofthedilutedcondensatefor
2 3 2
(CH CO H, sp gr 1.05), and dilute to 1 L. each determination.
3 2
11.5 Determination of Chloride and Fluoride with Ion-
10.3 Chloride, Standard Solution (1 mL 5 100 µg Cl)—
Dissolve 165 mg of dry sodium chloride (NaCl) in water and Selective Electrodes:
11.5.1 Assemble the meter and electrode in accordance with
dilute to 1 L.
the instructions provided with the ion-selective electrode and
10.4 Compressed Oxygen, Nitrogen, Helium, or Air.
the expanded scale meter being used.
10.5 Distilled Water—The water must be free of all chlo-
11.5.2 Use successive dilutions of the chloride and fluoride
rides and fluorides.
standards in the buffer solution on a 25-mL volume basis to
10.6 Fluoride, Standard Solution (1 mL 5 50 µg F)—
prepare calibration curves for each electrode. Plot the millivolt
Dissolve 111 mg of sodium fluoride (NaF) in water and dilu
...
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