ASTM C1347-02
(Practice)Standard Practice for Preparation and Dissolution of Uranium Materials for Analysis
Standard Practice for Preparation and Dissolution of Uranium Materials for Analysis
SIGNIFICANCE AND USE
The materials covered that must meet ASTM specifications are uranium metal and uranium oxide.
Uranium materials are used as nuclear reactor fuel. For this use, these materials must meet certain criteria for uranium content, uranium-235 enrichment, and impurity content, as described in Specifications C 753 and C 776. The material is assayed for uranium to determine whether the content is as specified.
Uranium alloys, refractory uranium materials, and uranium containing scrap and ash are unique uranium materials for which the user must determine the applicability of this practice. In general, these unique uranium materials are dissolved with various acid mixtures or by fusion with various fluxes.
SCOPE
1.1 This practice covers dissolution treatments for uranium materials that are applicable to the test methods used for characterizing these materials for uranium elemental, isotopic, and impurities determinations. Dissolution treatments for the major uranium materials assayed for uranium or analyzed for other components are listed.
1.2 The treatments, in order of presentation, are as follows:Procedure TitleSectionDissolution of Uranium Metal and Oxide with Nitric Acid8.1Dissolution of Uranium Oxides with Nitric Acid and Residue Treatment8.2Dissolution of Uranium-Aluminum Alloys in Hydrochloric Acid with Residue Treatment8.3Dissolution of Uranium Scrap and Ash by Leaching with Nitric Acid and Treatment of Residue by Carbonate Fusion8.4Dissolution of Refractory Uranium-Containing Material by Carbonate Fusion8.5Dissolution of Uranium-Aluminum Alloys Uranium Scrap and Ash, and RefractoryUranium-Containing Materials by Microwave Treatment8.6
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.4 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. Specific hazards statements are given in Section 7.
General Information
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Standards Content (Sample)
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Designation:C1347–02
Standard Practice for
Preparation and Dissolution of Uranium Materials for
Analysis
This standard is issued under the fixed designation C 1347; 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 D 1193 Specification for Reagent Water
1.1 This practice covers dissolution treatments for uranium
3. Summary of Practice
materials that are applicable to the test methods used for
3.1 Many uranium-containing materials such as high-purity
characterizing these materials for uranium elemental, isotopic,
metals and oxides dissolve readily in various mineral acids.
and impurities determinations. Dissolution treatments for the
The dissolution of uranium-plutonium mixed oxides is covered
major uranium materials assayed for uranium or analyzed for
in Practice C 1168. Highly refractory materials require prior
other components are listed.
grinding of samples and fusions to affect even partial dissolu-
1.2 The treatments, in order of presentation, are as follows:
tion. Combinations of the mineral acid and fusion techniques
Procedure Title Section
4,5,6
areusedfordifficulttodissolvematerials. Alternatively,the
Dissolution of Uranium Metal and Oxide with NitricAcid 8.1
Dissolution of Uranium Oxides with NitricAcid and Residue 8.2
combinationofacidsandahighpressuremicrowavehavebeen
Treatment
found to be effective with more difficult to dissolve materials
Dissolution of Uranium-AluminumAlloys in HydrochloricAcid 8.3
and can also be used for materials which dissolve in mineral
with Residue Treatment
Dissolution of Uranium Scrap andAsh by Leaching with Nitric 8.4
acid in place of heating with a steam bath or hot plate.
Acid and Treatment of Residue by Carbonate Fusion
3.2 The dissolved materials are quantitatively transferred to
Dissolution of Refractory Uranium-Containing Material by 8.5
tared polyethylene bottles for subsequent sample solution mass
Carbonate Fusion
Dissolution of Uranium—AluminumAlloys 8.6
determination and factor calculation.Aliquants are obtained by
Uranium Scrap andAsh, and Refractory
mass for high-precision analysis or by volume for less precise
Uranium-Containing Materials by
analysis methods. Quantitative transfers of samples and sub-
Microwave Treatment
sequent solutions are required. The sample is rejected when-
1.3 The values stated in SI units are to be regarded as the
ever a loss is incurred, or even suspected.
standard. The values given in parentheses are for information
3.3 Solutions of dissolved samples are inspected for undis-
only.
solved particles. Further treatment is necessary to attain com-
1.4 This standard does not purport to address all of the
plete solubility if particles are present. When analyzing the
safety concerns, if any, associated with its use. It is the
dissolved sample for trace impurities, caution should be
responsibility of the user of this standard to establish appro-
exercised so the dissolution process does not cause the impu-
priate safety and health practices and determine the applica-
rity to be lost or does not increase the level of impurity being
bility of regulatory limitations prior to use. Specific hazards
determined significantly.
statements are given in Section 7.
3.4 These dissolution procedures are written for the com-
plete or nearly complete dissolution of samples to obtain
2. Referenced Documents
destructive assay results on as near to 100 % of the sample as
2.1 ASTM Standards:
possible. When sample inhomogeneity is determined to be a
C 753 Specification for Nuclear-Grade, Sinterable Uranium
2 major contributor to assay error, nondestructive assay (NDA)
Dioxide Powder
determinations on residues from the dissolution may be re-
C 776 Specification for Sintered Uranium Dioxide Pellets
quested at an earlier stage than suggested in these procedures;
C 1168 Practice for Preparation and Dissolution of Pluto-
nium Materials for Analysis
Annual Book of ASTM Standards, Vol 11.01.
Selected Measurement Methods for Plutonium and Uranium in the Nuclear
This practice is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle, Second Edition, C. J. Rodden, ed., U.S. Atomic Energy Commission,
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of 1972.
Test. Analysis of Essential Nuclear Reactor Materials, C. J. Rodden, ed., U.S.
Current edition approved August 10, 2002. Published November 2002. Origi- Atomic Energy Commission, 1964.
nally published as C 1347 – 96. Last previous edition C 1347 – 96a. Larsen, R. P., “Dissolution of Uranium Metal and Its Alloys,” Analytical
Annual Book of ASTM Standards, Vol 12.01. Chemistry, Vol 31, No. 4, 1959, pp. 545–549.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959, United States.
C1347–02
the contribution of the error to the total assay may be 5.10 Pipettes 10 µL—5 mL (or equivalent). Accuracy of 6
propagated using the NDA assay value and errors for the 3% is adequate.
residue, and it may be determined that the error contributed to 5.11 Filter Paper—WhatmanNos.40and42,orequivalent.
the sample assay by the NDA determination on the residue is 5.12 Filter Paper Pulp.
acceptable. 5.13 Platinum Ware—Crucibles, with lids; platinum-tipped
3.5 The accuracy of the analytical method should be con- tongs; dishes, with lids.
sideredwhendeterminingifcompletedissolutionofthesample 5.14 TFE Fluorocarbon Ware—Stirring rods.
is required for difficult to dissolve matrices. 5.15 Dry Atmosphere Box.
5.16 Drying Oven.
4. Significance and Use
6. Reagents
4.1 The materials covered that must meet ASTM specifica-
6.1 Purity of Reagents—Reagent grade or better chemicals
tions are uranium metal and uranium oxide.
shall be used in all tests; impurities analyses, for example, may
4.2 Uranium materials are used as nuclear reactor fuel. For
require that all reagents and standards be prepared using
this use, these materials must meet certain criteria for uranium
Plasma grade, trace metal grade (TMG), or better. Unless
content, uranium-235 enrichment, and impurity content, as
otherwise indicated, it is intended that all reagents conform to
described in Specifications C 753 and C 776. The material is
the specifications of the Committee on Analytical Reagents of
assayed for uranium to determine whether the content is as
the American Chemical Society where such specifications are
specified.
available. Other grades may be used, provided it is first
4.3 Uranium alloys, refractory uranium materials, and ura-
ascertained that the reagent is of sufficiently high purity to
nium containing scrap and ash are unique uranium materials
permit its use without lessening the accuracy of measurements
for which the user must determine the applicability of this
made on the prepared materials.
practice. In general, these unique uranium materials are dis-
6.2 Purity of Water—Unless otherwise indicated, references
solved with various acid mixtures or by fusion with various
to water shall be understood to mean laboratory-accepted
fluxes.
demineralized or deionized water. For impurities analyses,
5. Apparatus Type 1 Reagent Grade water may be required dependent upon
the accuracy and precision of the analysis method used.
5.1 Balances, for determining the mass of samples and
6.3 Nitric Acid (HNO ), concentrated (sp gr 1.4), 16 M .
solutions.
6.4 HNO ,8 M—Add 500 mLof concentrated HNO (sp gr
3 3
5.2 Sample Mixing Equipment—Sample tumbler or mixer,
1.4) to approximately 400 mL of water and dilute to 1 L.
as appropriate; riffle splitter, stainless steel.
6.5 HNO,10% Add 100 mL of concentrated HNO (sp gr
3 3
5.3 Furnace—Muffle furnace, with fused silica tray to hold
1.4) to 800 mL. Type 1 Reagent Grade water and dilute to 1 L.
crucibles, capable of operation to 1200°C.
6.6 HNO,2% Add 20 mL of concentrated HNO to 900
3 3
5.4 HeatingEquipment—Asteambathinahood;hotplates;
mL. Type 1 Reagent Grade water and dilute to 1 L.
infrared lamps; Bunsen and blast burner, with provision for
7 6.7 Hydrochloric Acid (HCI), concentrated 12 M (sp gr
both gas and compressed air supply; microwave oven and
1.2).
high-pressure, heavy duty dissolution vessels.
6.8 Hydrofluoric Acid (HF), concentrated 29 M (sp gr 1.2).
5.5 Hardware—Metal weighing scoop; funnel racks; tongs;
6.9 HF 7.2 M Add 250 mL of concentrated HF, Electronic
rubber policemen; tripods; silica triangles; board, heat dissi-
Grade (29M ), to 700 mL Type 1 Reagent Grade water and
pating, at least 6.35-mm (0.25-in.) thick.
dilute to 1 L.
5.6 Beakers, Volumetric Flasks, and Bottles—Borosilicate
6.10 Sulfuric Acid (H SO ), concentrated 18 M (sp gr 1.8).
2 4
glass is generally recommended. However, the analyst should
6.11 Sulfuric Acid,9 M—Add 500 mL of concentrated (sp
be sure that safety and sample contamination are considered
gr 1.8) H SO to approximately 400 mL of water, cool and
2 4
when choosing appropriate containers.
dilute to 1 L. Store in a glass bottle.
5.7 Glassware—Borosilicate glass is generally recom-
6.12 Sodium Carbonate (Na CO ).
2 3
mended except as specified. Watch glasses or petri dishes, to
6.13 Sodium Bisulfate (NaHSO ).
cover beakers; funnels; stirring rods; crucibles, Vycor, with
lids.
7. Hazards
5.8 Plasticware—Wash bottle, polyethylene, 125-mL, for
7.1 Since enriched uranium-bearing materials are radioac-
aliquanting; petri dishes; narrow mouth polyethylene bottles;
tive and toxic, adequate laboratory facilities, including fume
plastic bottles, 60 mL; funnels, polypropylene; pipets, transfer.
hoods, along with safe handling techniques, must be used in
5.9 Volumetric Flask —Polypropylene, 25 mL, 50 mL, and
100 mL.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
The sole source of supply of the apparatus known to the committee at this time listed by the American Chemical Society, see Analar Standards for Laboratory
isCEMCorporation,3100SmithFarmRoad,Mathews,NC28105.Ifyouareaware Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
of alternative suppliers, please provide the information to ASTM International and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Headquarters.Your comments will receive careful consideration at a meeting of the MD.
responsible technical committee which you may attend. See Specification D 1193.
C1347–02
NOTE 3—Caution: Do not invert the flask or bottle prior to obtaining
working with samples containing these materials. A detailed
the mass of the solution.
discussion of all necessary safety precautions is beyond the
scope of this practice. However, personnel who handle radio- 8.1.7 Weigh the full flask or bottle using the top-loader
active materials should be familiar with the safe handling balance, and record the solution weight.
practices required in individual laboratory guidelines. 8.1.8 Invert the flask or bottle several times to mix the
7.2 Review the material safety data sheets and safety contents thoroughly prior to preparing aliquants.
proceduresinthelaboratory’ssafetymanualbeforeperforming 8.2 Dissolution of Uranium Oxides with Nitric Acid and
this procedure. Residue Treatment—Common laboratory techniques are de-
7.3 Elemental uranium is very reactive; assure initial reac- scribed in Annex A1. The techniques are referenced to the
tions have subsided before sealing closed vessels. As turnings appropriate section in parentheses at the first place in the
and powder, uranium is extremely pyrophoric, often igniting as procedure where they may be applicable.
a result of mechanical friction, a small addition of acid or 8.2.1 Sample Preparation—Obtain the mass of the sample
water, or even spontaneously. The reaction of uranium alloys usingafour-placebalance(usually0.5-gto0.1-mgsensitivity).
with acides may create an explosive mixture. Transfer the sample quantitatively to a beaker (A1.1.1). If the
sample is a powder, cover it gently with distilled water. Cover
8. Procedures the beaker with a watch glass.
8.1 Dissolution of Uranium Metal and Oxide with Nitric
NOTE 4—Caution: Do not wash down the walls of the beaker because
Acid: the powder may creep up the sides of the beaker and be lost.
8.1.1 Clean the surface oxide from metallic uranium by
8.2.2 Acid Dissolution:
placing the metal in a small beaker and adding enough 8 M
NOTE 5—Caution: Do not wet the beaker walls with the acid. Add
HNO to cover it. Place the beaker on a steam bath for 10 to 20
approximately 100 mL of 8 M HNO to the sample carefully in order to
min to remove the surface oxide. When the black oxide has
control the reaction rate.
been removed completely, decant the supernatant liquid into
NOTE 6—Caution: Powders may react very rapidly. If the reaction is
the appropriate container, and rinse the metal twice with
too rapid, add distilled water to decrease the reaction rate.
distilled water into the container.
8.2.2.1 Allow the reaction to subside; then heat on a
8.1.1.1 Dry the metal by rinsing twice with acetone or
steambath or hot plate (A1.1.2). Add additional 8 M HNO as
ethanol. Place the metal on filter paper, and allow it to dry for
necessary, until dissolution is complete.
30 to 60 s, rolling the metal several times to expose all faces to
8.2.2.2 When the dissolution appears to be complete, wash
the atmosphere.
down the walls of the beaker with distilled water and heat for
8.1.1.2 Tare a weighing scoop on an analytical balance.
an additional 30 min.
Place the dry uranium metal from 8.1.1.1 in the scoop and
8.2.2.3 Allow the solution to cool; then filter (A1.1.3-
weigh. Record the mass of the uranium metal (12 g of metal
A1.1.6) into a beaker.
will provide approximately 2 L of 6 g/L solution; the ratios of
8.2.2.4 Placethefilterpaperinaplatinumcrucible(A1.1.7).
metal mass and solution mass may be adjusted, as needed, to
Dry the filter paper(s) in the platinum crucible by placing it in
provide the desired concentration).
a cold muffle furnace that is then set to 700°C; maintain the
mufflefurnacetemperatureat700°Cforatleast1hforignition
NOTE 1—Measure and record the room temperature, barometric pres-
sure, and percent relative humidity if performing buoyancy corrections.
of the crucible or dish contents, or until no carbon is visible.
8.2.2.5 Allowthecrucibletocool;thenaddapproximately5
8.1.2 Tare a 2-Lflask or polyethylene bottle on a top loader
mL of concentrated HNO , 5 to 10 drops of HF, and 1 to 2
balance, or record the mass of the
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