ASTM C1463-00

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Designation:C1463–00
Standard Practices for
Dissolving Glass Containing Radioactive and Mixed Waste
for Chemical and Radiochemical Analysis
This standard is issued under the fixed designation C 1463; 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 2. Referenced Documents
1.1 These practices cover techniques suitable for dissolving 2.1 ASTM Standards:
glass samples that may contain nuclear wastes. These tech- C 169 Test Methods for Chemical Analysis of Soda-Lime
niques used together or independently will produce solutions and Borosilicate Glass
that can be analyzed by inductively coupled plasma atomic C 1109 Test Method for Analysis of Aqueous Leachates
emission spectroscopy (ICP-AES), inductively coupled plasma from Nuclear Waste Materials Using Inductively Coupled
mass spectrometry (ICP-MS), atomic absorption spectrometry Plasma-Atomic Emission Spectrometry
(AAS), radiochemical methods and wet chemical techniques C 1111 Test Method for Determining Elements in Waste
for major components, minor components and radionuclides. Streams by Inductively Coupled Plasma-Atomic Emission
1.2 One of the fusion practices and the microwave practice Spectroscopy
can be used in hot cells and shielded hoods after modification C 1220 Test Method for Static Leaching of Monolithic
to meet local operational requirements. Waste Forms for Disposal of Radioactive Waste
1.3 The user of these practices must follow radiation pro- C 1285 Test Methods for Determining Chemical Durability
tection guidelines in place for their specific laboratories. of Nuclear Waste Glasses: The Product Consistency Test
1.4 Additional information relating to safety is included in (PCT)
the text. D 1193 Specifications for Reagent Water
1.5 The dissolution techniques described in these practices
3. Summary of Practice
can be used for quality control of the feed materials and the
3.1 The three practices for dissolving silicate matrix
product of plants vitrifying nuclear waste materials in glass.
1.6 These practices are introduced to provide the user with samples each require the sample to be dried and ground to a
fine powder.
an alternative means to Test Methods C 169 for dissolution of
3.2 In the first practice, a mixture of sodium tetraborate
waste containing glass in shielded facilities. Test Methods
C 169 is not practical for use in such facilities and with (Na B O ) and sodium carbonate (Na CO ) is mixed with the
2 4 7 2 3
sample and fused in a muffle for 25 min at 950°C. The sample
radioactive materials.
1.7 The ICP-AES methods in Test Methods C 1109 and is cooled, dissolved in hydrochloric acid, and diluted to
appropriate volume for analyses.
C 1111 can be used to analyze the dissolved sample with
additional sample preparation as necessary and with matrix 3.3 The second practice described in this standard involves
fusion of the sample with potassium hydroxide (KOH) or
effect considerations. Additional information as to other ana-
lytical methods can be found in Test Method C 169. sodium peroxide (Na O ) using an electric bunsen burner,
2 2
dissolving the fused sample in water and dilute HCl, and
1.8 Solutions from this practice may be suitable for analysis
using ICP-MS after establishing laboratory performance crite- making to volume for analysis.
3.4 Dissolution of the sample using a microwave oven is
ria.
1.9 This standard does not purport to address all of the described in the third practice. The ground sample is digested
in a microwave oven using a mixture of hydrofluoric (HF) and
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- nitric (HNO ) acids. Boric acid is added to the resulting
solution to complex excess fluoride ions.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific precau- 3.5 These three practices offer alternative dissolution meth-
ods for a total analysis of a glass sample for major, minor, and
tionary statements are given in Section 18.
radionuclide components.
These practices are under the jurisdiction of ASTM Committee C-26 on
Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on Annual Book of ASTM Standards, Vol 15.02.
Analytical Test Methods. Annual Book of ASTM Standards, Vol 12.01.
Current edition approved Apr. 10, 2000. Published May 2000. Annual Book of ASTM Standards, Vol 11.01.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C1463
4. Reagents 8.5 Nitric Acid (HNO ), 50 % (v/v), made from concen-
trated nitric acid (sp gr 1.44) and water.
4.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
9. Hazards and Precautions
all reagents conform to the specifications of the Committee on
5 9.1 Follow established laboratory practices when conduct-
Analytical Reagents of the American Chemical Society.
ing this procedure.
4.2 Purity of Water—Unless otherwise indicated, references
9.2 The operator should wear suitable protective gear when
to water shall be understood to mean at least Type II reagent
handling chemicals.
water in conformance with Specification D 1193.
9.3 The dilution of concentrated acids is conducted in fume
hoods by cautiously adding an equal part acid to an equal part
PRACTICE 1—FUSION WITH SODIUM
TETRABORATE AND SODIUM CARBONATE of deionized water slowly and with constant stirring.
9.4 Samples that are known or suspected to contain radio-
5. Scope
active materials must be handled with the appropriate radiation
control and protection as prescribed by site health physics and
5.1 This practice covers flux fusion sample decomposition
radiation protection policies.
and dissolution for the determination of SiO and many other
9.5 Samples that are known or suspected to contain toxic,
oxides in glasses, ceramics, and raw materials. The solutions
hazardous, or radioactive materials must be handled to mini-
are analyzed by atomic spectroscopy methods. Analyte con-
mize or eliminate employee exposure. Fusion and leaching of
centrations ranging from trace to major levels can be measured
the fused samples must be performed in a fume hood,
in these solutions, depending on the sample weights and
radiation-shielded facility, or other appropriate containment.
dilution volumes used during preparation.
10. Sample Preparation
6. Technical Precautions
10.1 If the material to be analyzed is not in powder form, it
6.1 This procedure is not useful for the determination of
should first be broken into small pieces by placing the sample
boron or sodium since these elements are contained in the flux
in a plastic bag and then striking the sample with a hammer.
material.
The sample should then be ground to pass a 100-mesh sieve
6.2 The user is cautioned that with analysis by ICP-AES,
using a clean mortar and pestle such as agate or alumina
AAS, and ICP-MS, the high sodium concentrations from the
flux may cause interferences.
11. Procedure
6.3 Elements that form volatile species under these alkaline
11.1 Weigh 50 to 250 mg of a powdered sample into a
fusionconditionsmaybelostduringthefusionprocess(thatis,
platinum crucible on an analytical balance to 6 0.1 mg. The
As and Sb).
sample size is dependent on the analyte concentration.
7. Apparatus
NOTE 1—Although the larger sample size has generally worked well,
7.1 Platinum Crucibles,30mL.
some matrices may not dissolve entirely. Try smaller sample sizes if that
7.2 Balance, analytical type, precision to 0.1 mg. is the case.
7.3 Furnace, with heating capacity to 1000°C.
11.2 Add0.5 60.005geachofNa CO andNa B O tothe
2 3 2 4 7
7.4 Crucible Tongs, (cannot be made of iron, unless using
crucible containing the sample.
platinum-clad tips).
11.3 Stir the sample/flux mixture in the crucible with a
7.5 Polytetrafluoroethylene (PTFE) Beaker, 125-mL capac-
spatula until a mixture is obtained. Prepare a reagent blank.
ity.
11.4 For samples containing minor to major elements that
7.6 Magnetic Stir Bar, PTFE-coated (0.32 to 0.64 cm).
do not oxidize readily (such as Pb, Fe, etc.), add 300 mg of
7.7 Magnetic Stirrer.
sodium nitrate. If desired, a Pt lid can be placed on the crucible
7.8 Mortar and Pestle, agate or alumina (or equivalent
to reduce splattering. When adding nitrate, 50 % v/v HNO
grinding apparatus).
should be the diluting acid in order to reduce the attack on
7.9 Sieves, 100 mesh.
platinum in 11.6.
11.5 Using the crucible tongs, place the crucible containing
8. Reagents and Materials
the sample/flux mixture into a muffle furnace for 25 min at a
8.1 Anhydrous Sodium Carbonate (Na CO ).
2 3
temperature of 950°C. Remove the crucible from the furnace
8.2 Anhydrous Sodium Tetraborate (Na B O ).
2 4 7
and allow the melt to cool to room temperature.
8.3 Sodium Nitrate (NaNO ).
11.6 Place a stir bar in each crucible and add 4 mL50 % v/v
8.4 Hydrochloric Acid (HCl), 50 % (v/v), made from con-
HCl, and then dilute with H O to near the top of the crucible.
centrated hydrochloric acid (sp gr 1.19) and water.
NOTE 2—In some cases, 50 % v/v HNO may be more appropriate than
HCl (that is, samples for ICP-MS, high lead samples, or when sodium
nitrate was added).
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
11.7 Place the crucible on the magnetic stirrer, and stir until
listed by the American Chemical Society, see Analar Standards for Laboratory
the sample melt is dissolved completely (approximately 30
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
min). If undissolved material remains, the fusions described in
and National Formulary, U.S. Pharmacopeia Convention, Inc. (USPC), Rockville,
MD. Section 20 may need to be tried for cross correlation.
C1463
11.8 To a calibrated volumetric flask, typically 100, 250, 14.3 This practice can be used for bulk analysis of glass
500, or 1000 mL, add enough 1:1 HCl to make the final samples for the product consistency test (PCT) as described in
concentration 2 % (including the acid already in the crucible). Test Methods C 1285 and for the analysis of monolithic
The final volume is determined by the expected analyte radioactivewasteglassusedinthestaticleachtestasdescribed
concentrations.Quantitativelytransferthesamplesolution,and in Test Method C 1220.
dilute. 14.4 This practice can be used to dissolve the glass refer-
11.9 The dilution volume is determined by the user of the ence and testing materials described in Refs (1) and (2).
practice and is dependent upon the desired analysis.
11.10 See Appendix X1 for examples of analytical data
15. Interferences
using solutions from this fusion.
15.1 Elements that form volatile species under these alka-
line fusion conditions will be lost during the fusion process.
PRACTICE 2—FUSION WITH POTASSIUM
15.2 Thehighalkalimetal(NaorK)contentoftheresulting
HYDROXIDE OR SODIUM PEROXIDE
samplesolutionscancauseinterferencewithICPnebulizerand
torch assemblies due to salt deposition. Dilution of the sample
12. Scope
solutions may be necessary.
12.1 This practice covers alkaline fusion of silicate matrix 15.3 The metallic impurities, that is, Na, K, in the alkaline
samples (or other matrices difficult to dissolve in acids) using fluxusedtofusethesamplescancauseapositivebiasifproper
an electric Bunsen burner mounted on an orbital shaker. This corrections are not applied. Method blanks must be determined
practice has been used successfully to dissolve borosilicate to allow correction for flux impurity concentration.
glass, dried glass melter feeds, various simulated nuclear waste
forms, and dried soil samples.
16. Apparatus
12.2 This fusion apparatus and the alkaline fluxes described
16.1 Analytical Balance, capable of weighing to 6 0.1 mg.
are suitable for use in shielded radiation containment facilities
16.2 Electric Bunsen Burner, capable of heating to
such as hot cells and shielded hoods.
1000°C. to accommodate the larger size (100 mL nickel)
12.3 When samples dissolved using this practice are radio-
metal crucibles, the heat shield on top of the electric Bunsen
active, the user must follow radiation protection guidelines in
Burner is wrapped with a noncorrosive wire such as inconel at
place for such materials.
three evenly distributed locations. With the wire on the heat
shield, the large size crucibles are better supported and more
13. Summary of Practice
easily removed. A wire basket made from the noncorrosive
13.1 An aliquot of the dried and ignited sample is weighed wire is also fabricated so that smaller size crucibles (55 mL
into a tared nickel or zirconium metal crucible and an appro-
zirconium) that pass through the heat shield are supported
priate amount of alkaline flux (potassium hydroxide or sodium evenly in the heating mandrel of the electric Bunsen burner.
peroxide) is added. The crucible is placed on a preheated Fig. 1 shows the electric Bunsen burner mounted on the orbital
electric Bunsen burner (1000°C capability) mounted on an shaker with the above modifications for crucible mounting.
orbital shaker. The speed of the shaker is adjusted so that the 16.3 Orbital Shaker, including a holder fabricated to fasten
liquefied alkali metal flux and the sample are completely fused
the electric Bunsen burner on the platform (see Fig. 1).
at the bottom of the crucible. When the fusion is complete 16.4 Manual Adjustable Power Supply, for controlling the
(about 5 min), the crucible is removed from the heater and
temperature of the electric Bunsen burner.
cooled to room temperature. The fused mixture is dissolved in 16.5 Zirconium Metal Crucible, 55 mL capacity, high form.
water, acidified with hydrochloric acid, and diluted to an
Different shape and capacity crucibles also may be used when
appropriate volume for subsequent analysis. necessary.
13.2 With appropriate sample preparation, the solution re-
16.6 Nickel Metal Crucible, 100 mL capacity, high form.
sulting from this procedure can be analyzed for trace metals by Different shape and capacity crucibles also may be used when
ICP-AES, ICP-MS, and AAS, and for radionuclides using
necessary.
applicable radiochemical methods. 16.7 Aluminum Oxide Crucible, 55 mL capacity. Different
shape and capacity may be used depending upon sample sizes
14. Significance and Use taken.
16.8 200 Mesh (74 um) Sieve.
14.1 This practice d
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