ASTM C1463-00(2007)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Designation: C1463 − 00 (Reapproved2007)
Standard Practices for
Dissolving Glass Containing Radioactive and Mixed Waste
for Chemical and Radiochemical Analysis
This standard is issued under the fixed designation C1463; 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 1.9 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 These practices cover techniques suitable for dissolving
responsibility of the user of this standard to establish appro-
glass samples that may contain nuclear wastes. These tech-
priate safety and health practices and determine the applica-
niques used together or independently will produce solutions
bility of regulatory limitations prior to use. Specific precau-
that can be analyzed by inductively coupled plasma atomic
tionary statements are given in Section 18.
emission spectroscopy (ICP-AES), inductively coupled plasma
mass spectrometry (ICP-MS), atomic absorption spectrometry
2. Referenced Documents
(AAS), radiochemical methods and wet chemical techniques
2.1 ASTM Standards:
for major components, minor components and radionuclides.
C169 Test Methods for Chemical Analysis of Soda-Lime
1.2 One of the fusion practices and the microwave practice
and Borosilicate Glass
can be used in hot cells and shielded hoods after modification
C1109 Practice for Analysis of Aqueous Leachates from
to meet local operational requirements.
Nuclear Waste Materials Using Inductively Coupled
Plasma-Atomic Emission Spectroscopy
1.3 The user of these practices must follow radiation pro-
C1111 Test Method for Determining Elements in Waste
tection guidelines in place for their specific laboratories.
StreamsbyInductivelyCoupledPlasma-AtomicEmission
1.4 Additional information relating to safety is included in
Spectroscopy
the text.
C1220 Test Method for Static Leaching of MonolithicWaste
Forms for Disposal of Radioactive Waste
1.5 The dissolution techniques described in these practices
C1285 Test Methods for Determining Chemical Durability
can be used for quality control of the feed materials and the
of Nuclear, Hazardous, and Mixed Waste Glasses and
product of plants vitrifying nuclear waste materials in glass.
MultiphaseGlassCeramics:TheProductConsistencyTest
1.6 These practices are introduced to provide the user with
(PCT)
an alternative means to Test Methods C169 for dissolution of
D1193 Specification for Reagent Water
waste containing glass in shielded facilities. Test Methods
C169 is not practical for use in such facilities and with
3. Summary of Practice
radioactive materials.
3.1 The three practices for dissolving silicate matrix
1.7 The ICP-AES methods in Test Methods C1109 and
samples each require the sample to be dried and ground to a
C1111 can be used to analyze the dissolved sample with
fine powder.
additional sample preparation as necessary and with matrix
3.2 In the first practice, a mixture of sodium tetraborate
effect considerations. Additional information as to other ana-
(Na B O ) and sodium carbonate (Na CO ) is mixed with the
2 4 7 2 3
lytical methods can be found in Test Method C169.
sample and fused in a muffle for 25 min at 950°C. The sample
1.8 Solutions from this practice may be suitable for analysis is cooled, dissolved in hydrochloric acid, and diluted to
using ICP-MS after establishing laboratory performance crite- appropriate volume for analyses.
ria.
3.3 The second practice described in this standard involves
fusion of the sample with potassium hydroxide (KOH) or
sodium peroxide (Na O ) using an electric bunsen burner,
2 2
These practices are under the jurisdiction ofASTM Committee C26 on Nuclear
Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on Methods of
Test. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Feb. 1, 2007. Published March 2007. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 2000. Last previous edition approved in 2000 as C1463 – 00. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/C1463-00R07. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1463 − 00 (2007)
dissolving the fused sample in water and dilute HCl, and 7.5 Polytetrafluoroethylene (PTFE) Beaker, 125-mL capac-
making to volume for analysis. ity.
3.4 Dissolution of the sample using a microwave oven is 7.6 Magnetic Stir Bar, PTFE-coated (0.32 to 0.64 cm).
described in the third practice. The ground sample is digested
7.7 Magnetic Stirrer.
in a microwave oven using a mixture of hydrofluoric (HF) and
7.8 Mortar and Pestle, agate or alumina (or equivalent
nitric (HNO ) acids. Boric acid is added to the resulting
grinding apparatus).
solution to complex excess fluoride ions.
7.9 Sieves, 100 mesh.
3.5 These three practices offer alternative dissolution meth-
ods for a total analysis of a glass sample for major, minor, and
8. Reagents and Materials
radionuclide components.
8.1 Anhydrous Sodium Carbonate (Na CO ).
2 3
4. Reagents
8.2 Anhydrous Sodium Tetraborate (Na B O ).
2 4 7
4.1 Purity of Reagents—Reagent grade chemicals shall be
8.3 Sodium Nitrate (NaNO ).
used in all tests. Unless otherwise indicated, it is intended that
8.4 Hydrochloric Acid (HCl), 50 % (v/v), made from con-
all reagents conform to the specifications of the Committee on
centrated hydrochloric acid (sp gr 1.19) and water.
Analytical Reagents of the American Chemical Society.
8.5 Nitric Acid (HNO ), 50 % (v/v), made from concen-
4.2 Purity of Water—Unless otherwise indicated, references 3
trated nitric acid (sp gr 1.44) and water.
to water shall be understood to mean at least Type II reagent
water in conformance with Specification D1193.
9. Hazards and Precautions
PRACTICE 1—FUSION WITH SODIUM
9.1 Follow established laboratory practices when conduct-
TETRABORATE AND SODIUM CARBONATE
ing this procedure.
9.2 The operator should wear suitable protective gear when
5. Scope
handling chemicals.
5.1 This practice covers flux fusion sample decomposition
9.3 The dilution of concentrated acids is conducted in fume
and dissolution for the determination of SiO and many other
hoods by cautiously adding an equal part acid to an equal part
oxides in glasses, ceramics, and raw materials. The solutions
of deionized water slowly and with constant stirring.
are analyzed by atomic spectroscopy methods. Analyte con-
centrations ranging from trace to major levels can be measured
9.4 Samples that are known or suspected to contain radio-
in these solutions, depending on the sample weights and
active materials must be handled with the appropriate radiation
dilution volumes used during preparation.
control and protection as prescribed by site health physics and
radiation protection policies.
6. Technical Precautions
9.5 Samples that are known or suspected to contain toxic,
6.1 This procedure is not useful for the determination of
hazardous, or radioactive materials must be handled to mini-
boron or sodium since these elements are contained in the flux
mize or eliminate employee exposure. Fusion and leaching of
material.
the fused samples must be performed in a fume hood,
6.2 The user is cautioned that with analysis by ICP-AES, radiation-shielded facility, or other appropriate containment.
AAS, and ICP-MS, the high sodium concentrations from the
10. Sample Preparation
flux may cause interferences.
6.3 Elements that form volatile species under these alkaline 10.1 If the material to be analyzed is not in powder form, it
should first be broken into small pieces by placing the sample
fusionconditionsmaybelostduringthefusionprocess(thatis,
As and Sb). in a plastic bag and then striking the sample with a hammer.
The sample should then be ground to pass a 100-mesh sieve
7. Apparatus
using a clean mortar and pestle such as agate or alumina
7.1 Platinum Crucibles, 30 mL.
11. Procedure
7.2 Balance, analytical type, precision to 0.1 mg.
11.1 Weigh 50 to 250 mg of a powdered sample into a
7.3 Furnace, with heating capacity to 1000°C.
platinum crucible on an analytical balance to 60.1 mg. The
7.4 Crucible Tongs, (cannot be made of iron, unless using sample size is dependent on the analyte concentration.
platinum-clad tips).
NOTE 1—Although the larger sample size has generally worked well,
some matrices may not dissolve entirely. Try smaller sample sizes if that
is the case.
Reagent Chemicals, American Chemical Society Specifications, American
11.2 Add0.5 60.005geachofNa CO andNa B O tothe
Chemical Society, Washington, DC. For suggestions on the testing of reagents not 2 3 2 4 7
listed by the American Chemical Society, see Analar Standards for Laboratory crucible containing the sample.
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
11.3 Stir the sample/flux mixture in the crucible with a
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD. spatula until a mixture is obtained. Prepare a reagent blank.
C1463 − 00 (2007)
11.4 For samples containing minor to major elements that (about 5 min), the crucible is removed from the heater and
do not oxidize readily (such as Pb, Fe, etc.), add 300 mg of cooled to room temperature. The fused mixture is dissolved in
sodium nitrate. If desired, a Pt lid can be placed on the crucible water, acidified with hydrochloric acid, and diluted to an
to reduce splattering. When adding nitrate, 50 % v/v HNO appropriate volume for subsequent analysis.
should be the diluting acid in order to reduce the attack on
13.2 With appropriate sample preparation, the solution re-
platinum in 11.6.
sulting from this procedure can be analyzed for trace metals by
11.5 Using the crucible tongs, place the crucible containing ICP-AES, ICP-MS, and AAS, and for radionuclides using
the sample/flux mixture into a muffle furnace for 25 min at a applicable radiochemical methods.
temperature of 950°C. Remove the crucible from the furnace
14. Significance and Use
and allow the melt to cool to room temperature.
14.1 This practice describes a method to fuse and dissolve
11.6 Place a stir bar in each crucible and add 4 mL50 % v/v
silicate and refractory matrix samples for subsequent analysis
HCl, and then dilute with H O to near the top of the crucible.
for trace metals and radionuclides. These samples may contain
NOTE 2—In some cases, 50 % v/v HNO may be more appropriate than
high-level radioactive nuclear waste. Nuclear waste glass
HCl (that is, samples for ICP-MS, high lead samples, or when sodium
vitrification plant feeds and product can be characterized using
nitrate was added).
this dissolution method followed by the appropriate analysis of
11.7 Place the crucible on the magnetic stirrer, and stir until
the resulting solutions. Other matrices such as soil and sedi-
the sample melt is dissolved completely (approximately 30
ment samples and geological samples may be totally dissolved
min). If undissolved material remains, the fusions described in
using this practice.
Section 20 may need to be tried for cross correlation.
14.2 This practice has been used to analyze round-robin
11.8 To a calibrated volumetric flask, typically 100, 250,
simulated nuclear waste glass samples.
500, or 1000 mL, add enough 1:1 HCl to make the final
14.3 This practice can be used for bulk analysis of glass
concentration 2 % (including the acid already in the crucible).
samples for the product consistency test (PCT) as described in
The final volume is determined by the expected analyte
Test Methods C1285 and for the analysis of monolithic
concentrations.Quantitativelytransferthesamplesolution,and
radioactivewasteglassusedinthestaticleachtestasdescribed
dilute.
in Test Method C1220.
11.9 The dilution volume is determined by the user of the
14.4 This practice can be used to dissolve the glass refer-
practice and is dependent upon the desired analysis.
ence and testing materials described in Refs (1) and (2).
11.10 See Appendix X1 for examples of analytical data
using solutions from this fusion.
15. Interferences
15.1 Elements that form volatile species under these alka-
PRACTICE 2—FUSION WITH POTASSIUM
line fusion conditions will be lost during the fusion process.
HYDROXIDE OR SODIUM PEROXIDE
15.2 Thehighalkalimetal(NaorK)contentoftheresulting
12. Scope
samplesolutionscancauseinterferencewithICPnebulizerand
12.1 This practice covers alkaline fusion of silicate matrix
torch assemblies due to salt deposition. Dilution of the sample
samples (or other matrices difficult to dissolve in acids) using
solutions may be necessary.
an electric Bunsen burner mounted on an orbital shaker. This
15.3 The metallic impurities, that is, Na, K, in the alkaline
practice has been used successfully to dissolve borosilicate
fluxusedtofusethesamplescancauseapositivebiasifproper
glass,driedglassmelterfeeds,varioussimulatednuclearwaste
corrections are not applied. Method blanks must be determined
forms, and dried soil samples.
to allow correction for flux impurity concentration.
12.2 This fusion apparatus and the alkaline fluxes described
16. Apparatus
are suitable for use in shielded radiation containment facilities
such as hot cells and shielded hoods.
16.1 Analytical Balance, capable of weighing to 6 0.1 mg.
12.3 When samples dissolved using this practice are
16.2 Electric Bunsen Burner,capableofheatingto1000°C.
radioactive, the user must follow radiation protection guide-
to accommodate the larger size (100 mL nickel) metal
lines in place for such materials.
crucibles, the heat shield on top of the electric Bunsen Burner
is wrapped with a noncorrosive wire such as inconel at three
13. Summary of Practice
evenly distributed locations. With the wire on the heat shield,
13.1 An aliquot of the dried and ignited sample is weighed the large size crucibles are better supported and more easily
into a tared nickel or zirconium metal crucible and an appro- removed. A wire basket made from the noncorrosive wire is
priate amount of alkaline flux (potassium hydroxide or sodium alsofabricatedsothatsmallersizecrucibles(55mLzirconium)
peroxide) is added. The crucible is placed on a preheated
electric Bunsen burner (1000°C capability) mounted on an
The boldface numbers in parentheses refer to the list of references at the end of
orbital shaker. The speed of the shaker is adjusted so that the
this practice.
liquefied alkali metal flux and the sample ar
...