ASTM C1347-08(2014)e1

Standard Practice for Preparation and Dissolution of Uranium Materials for Analysis

SIGNIFICANCE AND USE
4.1 The materials covered that must meet ASTM specifications are uranium metal and uranium oxide.  
4.2 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 C753 and C776. The material is assayed for uranium to determine whether the content is as specified.  
4.3 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 Title  
Section  
Dissolution of Uranium Metal and Oxide with Nitric Acid  
8.1  
Dissolution of Uranium Oxides with Nitric Acid and Residue
Treatment  
8.2  
Dissolution of Uranium-Aluminum Alloys in Hydrochloric Acid
with Residue Treatment  
8.3  
Dissolution of Uranium Scrap and Ash by Leaching with Nitric
Acid and Treatment of Residue by Carbonate Fusion  
8.4  
Dissolution of Refractory Uranium-Containing Material by
Carbonate Fusion  
8.5  
Dissolution of Uranium—Aluminum Alloys
Uranium Scrap and Ash, and Refractory
Uranium-Containing Materials by
Microwave Treatment  
8.6
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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

• Status: Historical
• Publication Date: 31-May-2014
• ICS: 27.120.30 - Fissile materials and nuclear fuel technology
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
´1
Designation: C1347 − 08 (Reapproved 2014)
Standard Practice for
Preparation and Dissolution of Uranium Materials for
Analysis
This standard is issued under the fixed designation C1347; 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.
ε NOTE—Editorially relocated warning statement in 8.2.2 in June 2014.
1. Scope 2. Referenced Documents
2.1 ASTM Standards:
1.1 This practice covers dissolution treatments for uranium
C753 Specification for Nuclear-Grade, Sinterable Uranium
materials that are applicable to the test methods used for
Dioxide Powder
characterizing these materials for uranium elemental, isotopic,
C776 Specification for Sintered Uranium Dioxide Pellets
and impurities determinations. Dissolution treatments for the
C1168 PracticeforPreparationandDissolutionofPlutonium
major uranium materials assayed for uranium or analyzed for
Materials for Analysis
other components are listed.
D1193 Specification for Reagent Water
1.2 The treatments, in order of presentation, are as follows:
3. Summary of Practice
Procedure Title Section
Dissolution of Uranium Metal and Oxide with NitricAcid 8.1
3.1 Many uranium-containing materials such as high-purity
Dissolution of Uranium Oxides with NitricAcid and Residue 8.2
metals and oxides dissolve readily in various mineral acids.
Treatment
The dissolution of uranium-plutonium mixed oxides is covered
Dissolution of Uranium-AluminumAlloys in HydrochloricAcid 8.3
with Residue Treatment
in Practice C1168. Highly refractory materials require prior
Dissolution of Uranium Scrap andAsh by Leaching with Nitric 8.4
grinding of samples and fusions to affect even partial dissolu-
Acid and Treatment of Residue by Carbonate Fusion
Dissolution of Refractory Uranium-Containing Material by 8.5 tion. Combinations of the mineral acid and fusion techniques
3,4,5
Carbonate Fusion
areusedfordifficulttodissolvematerials. Alternatively,the
Dissolution of Uranium—AluminumAlloys 8.6
combinationofacidsandahighpressuremicrowavehavebeen
Uranium Scrap andAsh, and Refractory
Uranium-Containing Materials by found to be effective with more difficult to dissolve materials
Microwave Treatment
and can also be used for materials which dissolve in mineral
acid in place of heating with a steam bath or hot plate.
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
3.2 The dissolved materials are quantitatively transferred to
standard.
tared polyethylene bottles for subsequent sample solution mass
determination and factor calculation.Aliquants are obtained by
1.4 This standard does not purport to address all of the
mass for high-precision analysis or by volume for less precise
safety concerns, if any, associated with its use. It is the
analysis methods. Quantitative transfers of samples and sub-
responsibility of the user of this standard to establish appro-
sequent solutions are required. The sample is rejected when-
priate safety and health practices and determine the applica-
ever a loss is incurred, or even suspected.
bility of regulatory limitations prior to use. Specific hazards
statements are given in Section 7.
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.
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 June 1, 2014. Published June 2014. Originally Atomic Energy Commission, 1964.
approved in 1996. Last previous edition approved in 2008 as C1347 – 08. DOI: Larsen, R. P., “Dissolution of Uranium Metal and Its Alloys,” Analytical
10.1520/C1347-08R14E01. 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
´1
C1347 − 08 (2014)
3.3 Solutions of dissolved samples are inspected for undis- both gas and compressed air supply; microwave oven and
solved particles. Further treatment is necessary to attain com- high-pressure, heavy duty dissolution vessels.
plete solubility if particles are present. When analyzing the
5.5 Hardware—Metal weighing scoop; funnel racks; tongs;
dissolved sample for trace impurities, caution should be
rubber policemen; tripods; silica triangles; board, heat
exercised so the dissolution process does not cause the impu-
dissipating, at least 6.35-mm (0.25-in.) thick.
rity to be lost or does not increase the level of impurity being
determined significantly.
5.6 Beakers, Volumetric Flasks, and Bottles—Borosilicate
glass is generally recommended. However, the analyst should
NOTE 1—The use of double distilled acids may be necessary for low
level trace impurities. The use of plastic labware will be necessary so the
be sure that safety and sample contamination are considered
dissolution does not increase the level of impurities being determined.
whenchoosingappropriatecontainers.Ifthebackgroundlevels
This may be necessary in Section 8.6.
of impurities such as boron, iron and sodium are being
3.4 These dissolution procedures are written for the com-
determined, then polypropylene or polytetrafluoroethylene
plete or nearly complete dissolution of samples to obtain
containers and labware will be necessary in place of borosili-
destructive assay results on as near to 100 % of the sample as
cate glass.
possible. When sample inhomogeneity is determined to be a
major contributor to assay error, nondestructive assay (NDA) 5.7 Glassware—Borosilicate glass is generally recom-
determinations on residues from the dissolution may be re-
mended except as specified. Watch glasses or petri dishes, to
quested at an earlier stage than suggested in these procedures;
cover beakers; funnels; stirring rods; crucibles, Vycor, with
the contribution of the error to the total assay may be
lids.
propagated using the NDA assay value and errors for the
5.8 Plasticware—Wash bottle, polyethylene, 125-mL, for
residue, and it may be determined that the error contributed to
aliquanting; petri dishes; narrow mouth polyethylene bottles;
the sample assay by the NDA determination on the residue is
plastic bottles, 60 mL; funnels, polypropylene; pipets, transfer.
acceptable.
3.5 The accuracy of the analytical method should be con-
5.9 Volumetric Flask— Polypropylene, 25 mL, 50 mL, and
sideredwhendeterminingifcompletedissolutionofthesample
100 mL.
is required for difficult to dissolve matrices.
5.10 Pipettes 10 µL—5 mL (or equivalent). Accuracy of 6
3% is adequate.
4. Significance and Use
5.11 Filter Paper—Whatman Nos. 40 and 42, or equivalent.
4.1 The materials covered that must meet ASTM specifica-
tions are uranium metal and uranium oxide.
5.12 Filter Paper Pulp.
4.2 Uranium materials are used as nuclear reactor fuel. For
5.13 Platinum Ware—Crucibles, with lids; platinum-tipped
this use, these materials must meet certain criteria for uranium
tongs; dishes, with lids.
content, uranium-235 enrichment, and impurity content, as
described in Specifications C753 and C776. The material is
5.14 TFE Fluorocarbon Ware—Stirring rods.
assayed for uranium to determine whether the content is as
5.15 Dry Atmosphere Box.
specified.
4.3 Uranium alloys, refractory uranium materials, and ura-
5.16 Drying Oven.
nium containing scrap and ash are unique uranium materials
for which the user must determine the applicability of this
6. Reagents
practice. In general, these unique uranium materials are dis-
6.1 Purity of Reagents—Reagent grade or better chemicals
solved with various acid mixtures or by fusion with various
shall be used in all tests; impurities analyses, for example, may
fluxes.
require that all reagents and standards be prepared using
Plasma grade, trace metal grade (TMG), double distilled, or
5. Apparatus
better. Unless otherwise indicated, it is intended that all
5.1 Balances, for determining the mass of samples and
reagents conform to the specifications of the Committee on
solutions.
Analytical Reagents of the American Chemical Society where
5.2 Sample Mixing Equipment—Sample tumbler or mixer,
as appropriate; riffle splitter, stainless steel.
5.3 Furnace—Muffle furnace, with fused silica tray to hold 6
The sole source of supply of the apparatus known to the committee at this time
crucibles, capable of operation to 1200°C. isCEMCorporation,3100SmithFarmRoad,Mathews,NC28105.Ifyouareaware
of alternative suppliers, please provide the information to ASTM International
5.4 Heating Equipment—Asteam bath in a hood; hot plates;
Headquarters.Your comments will receive careful consideration at a meeting of the
infrared lamps; Bunsen and blast burner, with provision for responsible technical committee, which you may attend.
´1
C1347 − 08 (2014)
such specifications are available. Other grades may be used, 7.4 Warning—Hydrofluoric acid is highly corrosive acid
provided it is first ascertained that the reagent is of sufficiently that can severly burn skin, eyes, and mucous membranes.
high purity to permit its use without lessening the accuracy of Hydrofluoric acid is similar to other acids in that the initial
measurements made on the prepared materials. extent of a burn depends on the concentration, the temperature,
and the duration of contact with the acid. Hydrofluoric acid
6.2 Purity of Water—Unless otherwise indicated, references
differs from other acids because the fluoride ion readily
to water shall be understood to mean laboratory-accepted
penetrates the skin, causing destruction of deep tissue layers.
demineralized or deionized water. For impurities analyses,
Unlike other acids that are rapidly neutralized, hydrofluoric
Type 1 Reagent Grade water may be required dependent upon
acid reactions with tissue may continue for days if left
the accuracy and precision of the analysis method used.
untreated.Duetotheseriousconsequencesofhydrofluoricacid
6.3 Nitric Acid (HNO ), concentrated (sp gr 1.4), 16 M.
burns, prevention of exposure or injury of personnel is the
6.4 HNO , 8 M—Add 500 mLof concentrated HNO (sp gr primary goal. Utilization of appropriate laboratory controls
3 3
(hoods) and wearing adequate personnel protective equipment
1.4) to approximately 400 mL of water and dilute to 1 L.
to protect from skin and eye contact is essential. Acute
6.5 HNO ,10% Add 100 mL of concentrated HNO (sp gr
3 3
exposure to HF can cause painful and severe burns upon skin
1.4) to 800 mL. Type 1 Reagent Grade water and dilute to 1 L.
contact that require special medical attention. Chronic or
6.6 HNO ,2% Add 20 mL of concentrated HNO to 900
3 3
prolonged exposure to low levels on the skin may cause
mL. Type 1 Reagent Grade water and dilute to 1 L.
fluorosis.
6.7 Hydrochloric Acid(HCI),concentrated12 M(spgr1.2).
8. Procedures
6.8 Hydrofluoric Acid (HF), concentrated 29 M (sp gr 1.2).
8.1 Dissolution of Uranium Metal and Oxide with Nitric
6.9 HF 7.2 M Add 250 mL of concentrated HF, Electronic
Acid:
Grade (29M), to 700 mL Type 1 Reagent Grade water and
8.1.1 Clean the surface oxide from metallic uranium by
dilute to 1 L.
placing the metal in a small beaker and adding enough 8 M
6.10 Sulfuric Acid (H SO ), concentrated 18 M (sp gr 1.8). HNO to cover it. Place the beaker on a steam bath for 10 to 20
2 4
min to remove the surface oxide. When the black oxide has
6.11 Sulfuric Acid, 9 M—Add 500 mL of concentrated (sp
been removed completely, decant the supernatant liquid into
gr 1.8) H SO to approximately 400 mL of water, cool and
2 4
the appropriate container, and rinse the metal twice with
dilute to 1 L. Store in a glass bottle.
distilled water into the container.
6.12 Sodium Carbonate (Na CO ).
2 3
8.1.1.1 Dry the metal by rinsing twice with acetone or
ethanol. Place the metal on filter paper, and allow it to dry for
6.13 Sodium Bisulfate (NaHSO ).
30 to 60 s, rolling the metal several times to expose all faces to
7. Hazards the atmosphere.
8.1.1.2 Tare a weighing scoop on an analytical balance.
7.1 Since enriched uranium-bearing materials are radioac-
Place the dry uranium metal from 8.1.1.1 in the scoop and
tive and toxic, adequate laboratory facilities, including fume
weigh. Record the mass of the uranium metal (12 g of metal
hoods, along with safe handling techniques, must be used in
will provide approximately 2 L of 6 g/L solution; the ratios of
working with samples containing these materials. A detailed
metal mass and solution mass may be adjusted, as needed, to
discussion of all necessary safety precautions is beyond the
provide the desired concentration).
scope of this practice. However, personnel who handle radio-
active materials should be familiar with the safe handling
NOTE 2—Measure and record the room temperature, barometric
practices required in individual laboratory guidelines. pressure, and percent relative humidity if performing buoyancy correc-
tions.
7.2 Review the material safety data sheets and safety
8.1.2 Tare a 2-Lflask or polyethylene bottle on a top loader
proceduresinthelaboratory’ssafetymanualbeforeperforming
balance, or record the mass of the flask or bottle.
this procedure.
8.1.3 Transfer the metal quantitatively to the tared (or
7.3 Elemental uranium is very reactive; assure initial reac-
weighed) flask or bottle.
tions have subsided before sealing closed vessels. As turnings
8.1.4 Add 250 mL of 8 M HNO (adjust the nitric acid
andpowder,uraniumisextremelypyrophoric,oftenignitingas
volume in ratio to the metal to be dissolved since insufficient
a result of mechanical friction, a small addition of acid or
HNO will cause the metal surface to become passive) to the
water, or even spontaneously. The reaction of uranium alloys
flask or bottle. Warm the flask or bottle on a steam bath (the
with acides may create an explosive mixture.
flask or bottle must be left unstoppered due to gas generation,
but it may be covered by an inverted beaker).
NOTE 3—If desired, up to 20 mLof concentrated H SO may be added
Reagent Chemicals, American Chemical Society Specifications, American 2 4
to the mixture.This will speed dissolution and ease later dissolution of the
Chemical Society, Washington, DC. For suggestion
...

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.
´1
Designation: C1347 − 08 C1347 − 08 (Reapproved 2014)
Standard Practice for
Preparation and Dissolution of Uranium Materials for
Analysis
This standard is issued under the fixed designation C1347; 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.
ε NOTE—Editorially relocated warning statement in 8.2.2 in June 2014.
1. 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 Title Section
Dissolution of Uranium Metal and Oxide with Nitric Acid 8.1
Dissolution of Uranium Oxides with Nitric Acid and Residue 8.2
Treatment
Dissolution of Uranium-Aluminum Alloys in Hydrochloric Acid 8.3
with Residue Treatment
Dissolution of Uranium Scrap and Ash by Leaching with Nitric 8.4
Acid and Treatment of Residue by Carbonate Fusion
Dissolution of Refractory Uranium-Containing Material by 8.5
Carbonate Fusion
Dissolution of Uranium—Aluminum Alloys 8.6
Uranium Scrap and Ash, and Refractory
Uranium-Containing Materials by
Microwave Treatment
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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.
2. Referenced Documents
2.1 ASTM Standards:
C753 Specification for Nuclear-Grade, Sinterable Uranium Dioxide Powder
C776 Specification for Sintered Uranium Dioxide Pellets
C1168 Practice for Preparation and Dissolution of Plutonium Materials for Analysis
D1193 Specification for Reagent Water
3. Summary of Practice
3.1 Many uranium-containing materials such as high-purity metals and oxides dissolve readily in various mineral acids. The
dissolution of uranium-plutonium mixed oxides is covered in Practice C1168. Highly refractory materials require prior grinding
of samples and fusions to affect even partial dissolution. Combinations of the mineral acid and fusion techniques are used for
3,4,5
difficult to dissolve materials. Alternatively, the combination of acids and a high pressure microwave have been found to be
effective with more difficult to dissolve materials and can also be used for materials which dissolve in mineral acid in place of
heating with a steam bath or hot plate.
This practice 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 Dec. 1, 2008June 1, 2014. Published December 2008June 2014. Originally approved in 1996. Last previous edition approved in 20022008 as
C1347 – 02.C1347 – 08. DOI: 10.1520/C1347-08.10.1520/C1347-08R14E01.
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.
Selected Measurement Methods for Plutonium and Uranium in the Nuclear Fuel Cycle, Second Edition, C. J. Rodden, ed., U.S. Atomic Energy Commission, 1972.
Analysis of Essential Nuclear Reactor Materials, C. J. Rodden, ed., U.S. Atomic Energy Commission, 1964.
Larsen, R. P., “Dissolution of Uranium Metal and Its Alloys,” Analytical Chemistry , Vol 31, No. 4, 1959, pp. 545–549.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
C1347 − 08 (2014)
3.2 The dissolved materials are quantitatively transferred to tared polyethylene bottles for subsequent sample solution mass
determination and factor calculation. Aliquants are obtained by mass for high-precision analysis or by volume for less precise
analysis methods. Quantitative transfers of samples and subsequent solutions are required. The sample is rejected whenever a loss
is incurred, or even suspected.
3.3 Solutions of dissolved samples are inspected for undissolved particles. Further treatment is necessary to attain complete
solubility if particles are present. When analyzing the dissolved sample for trace impurities, caution should be exercised so the
dissolution process does not cause the impurity to be lost or does not increase the level of impurity being determined significantly.
NOTE 1—The use of double distilled acids may be necessary for low level trace impurities. The use of plastic labware will be necessary so the
dissolution does not increase the level of impurities being determined. This may be necessary in Section 8.6.
3.4 These dissolution procedures are written for the complete or nearly complete dissolution of samples to obtain destructive
assay results on as near to 100 % of the sample as possible. When sample inhomogeneity is determined to be a major contributor
to assay error, nondestructive assay (NDA) determinations on residues from the dissolution may be requested at an earlier stage
than suggested in these procedures; the contribution of the error to the total assay may be propagated using the NDA assay value
and errors for the residue, and it may be determined that the error contributed to the sample assay by the NDA determination on
the residue is acceptable.
3.5 The accuracy of the analytical method should be considered when determining if complete dissolution of the sample is
required for difficult to dissolve matrices.
4. Significance and Use
4.1 The materials covered that must meet ASTM specifications are uranium metal and uranium oxide.
4.2 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 C753 and C776. The material is assayed for
uranium to determine whether the content is as specified.
4.3 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.
5. Apparatus
5.1 Balances, for determining the mass of samples and solutions.
5.2 Sample Mixing Equipment—Sample tumbler or mixer, as appropriate; riffle splitter, stainless steel.
5.3 Furnace—Muffle furnace, with fused silica tray to hold crucibles, capable of operation to 1200°C.
5.4 Heating Equipment—A steam bath in a hood; hot plates; infrared lamps; Bunsen and blast burner, with provision for both
gas and compressed air supply; microwave oven and high-pressure, heavy duty dissolution vessels.
5.5 Hardware—Metal weighing scoop; funnel racks; tongs; rubber policemen; tripods; silica triangles; board, heat dissipating,
at least 6.35-mm (0.25-in.) thick.
5.6 Beakers, Volumetric Flasks, and Bottles—Borosilicate glass is generally recommended. However, the analyst should be sure
that safety and sample contamination are considered when choosing appropriate containers. If the background levels of impurities
such as boron, iron and sodium are being determined, then polypropylene or polytetrafluoroethylene containers and labware will
be necessary in place of borosilicate glass.
5.7 Glassware—Borosilicate glass is generally recommended except as specified. Watch glasses or petri dishes, to cover
beakers; funnels; stirring rods; crucibles, Vycor, with lids.
5.8 Plasticware—Wash bottle, polyethylene, 125-mL, for aliquanting; petri dishes; narrow mouth polyethylene bottles; plastic
bottles, 60 mL; funnels, polypropylene; pipets, transfer.
5.9 Volumetric Flask— Polypropylene, 25 mL, 50 mL, and 100 mL.
5.10 Pipettes 10 μL—5 mL (or equivalent). Accuracy of 6 3% is adequate.
5.11 Filter Paper—Whatman Nos. 40 and 42, or equivalent.
5.12 Filter Paper Pulp.
5.13 Platinum Ware—Crucibles, with lids; platinum-tipped tongs; dishes, with lids.
The sole source of supply of the apparatus known to the committee at this time is CEM Corporation, 3100 Smith Farm Road, Mathews, NC 28105. If you are aware
of alternative suppliers, please provide the information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical committee, which you may attend.
´1
C1347 − 08 (2014)
5.14 TFE Fluorocarbon Ware—Stirring rods.
5.15 Dry Atmosphere Box.
5.16 Drying Oven.
6. Reagents
6.1 Purity of Reagents—Reagent grade or better chemicals shall be used in all tests; impurities analyses, for example, may
require that all reagents and standards be prepared using Plasma grade, trace metal grade (TMG), double distilled, or better. Unless
otherwise indicated, it is intended that all reagents 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 measurements made on the prepared
materials.
6.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean laboratory-accepted
demineralized or deionized water. For impurities analyses, Type 1 Reagent Grade water may be required dependent upon the
accuracy and precision of the analysis method used.
6.3 Nitric Acid (HNO ), concentrated (sp gr 1.4), 16 MM. .
6.4 HNO , 8 M—Add 500 mL of concentrated HNO (sp gr 1.4) to approximately 400 mL of water and dilute to 1 L.
3 3
6.5 HNO , 10 % Add 100 mL of concentrated HNO (sp gr 1.4) to 800 mL. Type 1 Reagent Grade water and dilute to 1 L.
3 3
6.6 HNO , 2 % Add 20 mL of concentrated HNO to 900 mL. Type 1 Reagent Grade water and dilute to 1 L.
3 3
6.7 Hydrochloric Acid (HCI), concentrated 12 M (sp gr 1.2).
6.8 Hydrofluoric Acid (HF), concentrated 29 M (sp gr 1.2).
6.9 HF 7.2 M Add 250 mL of concentrated HF, Electronic Grade (29M), to 700 mL Type 1 Reagent Grade water and dilute to
1 L.
6.10 Sulfuric Acid (H SO ), concentrated 18 M (sp gr 1.8).
2 4
6.11 Sulfuric Acid, 9 M—Add 500 mL of concentrated (sp gr 1.8) H SO to approximately 400 mL of water, cool and dilute
2 4
to 1 L. Store in a glass bottle.
6.12 Sodium Carbonate (Na CO ).
2 3
6.13 Sodium Bisulfate (NaHSO ).
7. Hazards
7.1 Since enriched uranium-bearing materials are radioactive and toxic, adequate laboratory facilities, including fume hoods,
along with safe handling techniques, must be used in working with samples containing these materials. A detailed discussion of
all necessary safety precautions is beyond the scope of this practice. However, personnel who handle radioactive materials should
be familiar with the safe handling practices required in individual laboratory guidelines.
7.2 Review the material safety data sheets and safety procedures in the laboratory’s safety manual before performing this
procedure.
7.3 Elemental uranium is very reactive; assure initial reactions have subsided before sealing closed vessels. As turnings and
powder, uranium is extremely pyrophoric, often igniting as a result of mechanical friction, a small addition of acid or water, or
even spontaneously. The reaction of uranium alloys with acides may create an explosive mixture.
7.4 Warning—Hydrofluoric acid is highly corrosive acid that can severly burn skin, eyes, and mucous membranes.
Hydrofluoric acid is similar to other acids in that the initial extent of a burn depends on the concentration, the temperature, and
the duration of contact with the acid. Hydrofluoric acid differs from other acids because the fluoride ion readily penetrates the skin,
causing destruction of deep tissue layers. Unlike other acids that are rapidly neutralized, hydrofluoric acid reactions with tissue may
continue for days if left untreated. Due to the serious consequences of hydrofluoric acid burns, prevention of exposure or injury
of personnel is the primary goal. Utilization of appropriate laboratory controls (hoods) and wearing adequate personnel protective
equipment to protect from skin and eye contact is essential. Acute exposure to HF can cause painful and severe burns upon skin
contact that require special medical attention. Chronic or prolonged exposure to low levels on the skin may cause
fluorosis.Warning—Hydrofluoric acid is highly corrosive acid that can severly burn skin, eyes, and mucous membranes.
Hydrofluoric acid is similar to other acids in that the initial extent of a burn depends on the concentration, the temperature, and
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.
See Specification D1193.
´1
C1347 − 08 (2014)
the duration of contact with the acid. Hydrofluoric acid differs from other acids because the fluoride ion readily penetrates the skin,
causing destruction of deep tissue layers. Unlike other acids that are rapidly neutralized, hydrofluoric acid reactions with tissue may
continue for days if left untreated. Due to the serious consequences of hydrofluoric acid burns, prevention of exposure or injury
of personnel is the primary goal. Utilization of appropriate laboratory controls (hoods) and wearing adequate personnel protective
equipment to protect from skin and eye contact is essential. Acute exposure to HF can cause painful and severe burns upon skin
contact that require special medical attention. Chronic or prolonged exposure to low levels on the skin may cause fluorosis.
8. Procedures
8.1 Dissol
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