1、Designation: C 1463 00 (Reapproved 2007)Standard Practices forDissolving Glass Containing Radioactive and Mixed Wastefor Chemical and Radiochemical Analysis1This standard is issued under the fixed designation C 1463; the number immediately following the designation indicates the year oforiginal adop
2、tion or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 These practices cover techniques suitable for dissolvingglass samples t
3、hat may contain nuclear wastes. These tech-niques used together or independently will produce solutionsthat can be analyzed by inductively coupled plasma atomicemission spectroscopy (ICP-AES), inductively coupled plasmamass spectrometry (ICP-MS), atomic absorption spectrometry(AAS), radiochemical me
4、thods and wet chemical techniquesfor major components, minor components and radionuclides.1.2 One of the fusion practices and the microwave practicecan be used in hot cells and shielded hoods after modificationto meet local operational requirements.1.3 The user of these practices must follow radiati
5、on pro-tection guidelines in place for their specific laboratories.1.4 Additional information relating to safety is included inthe text.1.5 The dissolution techniques described in these practicescan be used for quality control of the feed materials and theproduct of plants vitrifying nuclear waste m
6、aterials in glass.1.6 These practices are introduced to provide the user withan alternative means to Test Methods C 169 for dissolution ofwaste containing glass in shielded facilities. Test MethodsC 169 is not practical for use in such facilities and withradioactive materials.1.7 The ICP-AES methods
7、 in Test Methods C 1109 andC 1111 can be used to analyze the dissolved sample withadditional sample preparation as necessary and with matrixeffect considerations. Additional information as to other ana-lytical methods can be found in Test Method C 169.1.8 Solutions from this practice may be suitable
8、 for analysisusing ICP-MS after establishing laboratory performance crite-ria.1.9 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and deter
9、mine the applica-bility of regulatory limitations prior to use. Specific precau-tionary statements are given in Section 18.2. Referenced Documents2.1 ASTM Standards:2C 169 Test Methods for Chemical Analysis of Soda-Limeand Borosilicate GlassC 1109 Practice for Analysis of Aqueous Leachates fromNucle
10、ar Waste Materials Using Inductively CoupledPlasma-Atomic Emission SpectroscopyC 1111 Test Method for Determining Elements in WasteStreams by Inductively Coupled Plasma-Atomic EmissionSpectroscopyC 1220 Test Method for Static Leaching of MonolithicWaste Forms for Disposal of Radioactive WasteC 1285
11、Test Methods for Determining Chemical Durabilityof Nuclear, Hazardous, and Mixed Waste Glasses andMultiphase Glass Ceramics: The Product Consistency Test(PCT)D 1193 Specification for Reagent Water3. Summary of Practice3.1 The three practices for dissolving silicate matrixsamples each require the sam
12、ple to be dried and ground to afine powder.3.2 In the first practice, a mixture of sodium tetraborate(Na2B4O7) and sodium carbonate (Na2CO3) is mixed with thesample and fused in a muffle for 25 min at 950C. The sampleis cooled, dissolved in hydrochloric acid, and diluted toappropriate volume for ana
13、lyses.3.3 The second practice described in this standard involvesfusion of the sample with potassium hydroxide (KOH) orsodium peroxide (Na2O2) using an electric bunsen burner,dissolving the fused sample in water and dilute HCl, andmaking to volume for analysis.3.4 Dissolution of the sample using a m
14、icrowave oven isdescribed in the third practice. The ground sample is digested1These practices are under the jurisdiction ofASTM Committee C26 on NuclearFuel Cycle and are the direct responsibility of Subcommittee C26.05 on Methods ofTest.Current edition approved Feb. 1, 2007. Published March 2007.
15、Originallyapproved in 2000. Last previous edition approved in 2000 as C 146300.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page o
16、nthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.in a microwave oven using a mixture of hydrofluoric (HF) andnitric (HNO3) acids. Boric acid is added to the resultingsolution to complex excess fluoride ions.3.5 These
17、 three practices offer alternative dissolution meth-ods for a total analysis of a glass sample for major, minor, andradionuclide components.4. Reagents4.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the s
18、pecifications of the Committee onAnalytical Reagents of the American Chemical Society.34.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean at least Type II reagentwater in conformance with Specification D 1193.PRACTICE 1FUSION WITH SODIUMTETRABORATE AND SODI
19、UM CARBONATE5. Scope5.1 This practice covers flux fusion sample decompositionand dissolution for the determination of SiO2and many otheroxides in glasses, ceramics, and raw materials. The solutionsare analyzed by atomic spectroscopy methods. Analyte con-centrations ranging from trace to major levels
20、 can be measuredin these solutions, depending on the sample weights anddilution volumes used during preparation.6. Technical Precautions6.1 This procedure is not useful for the determination ofboron or sodium since these elements are contained in the fluxmaterial.6.2 The user is cautioned that with
21、analysis by ICP-AES,AAS, and ICP-MS, the high sodium concentrations from theflux may cause interferences.6.3 Elements that form volatile species under these alkalinefusion conditions may be lost during the fusion process (that is,As and Sb).7. Apparatus7.1 Platinum Crucibles,30mL.7.2 Balance, analyt
22、ical type, precision to 0.1 mg.7.3 Furnace, with heating capacity to 1000C.7.4 Crucible Tongs, (cannot be made of iron, unless usingplatinum-clad tips).7.5 Polytetrafluoroethylene (PTFE) Beaker, 125-mL capac-ity.7.6 Magnetic Stir Bar, PTFE-coated (0.32 to 0.64 cm).7.7 Magnetic Stirrer.7.8 Mortar and
23、 Pestle, agate or alumina (or equivalentgrinding apparatus).7.9 Sieves, 100 mesh.8. Reagents and Materials8.1 Anhydrous Sodium Carbonate (Na2CO3).8.2 Anhydrous Sodium Tetraborate (Na2B4O7).8.3 Sodium Nitrate (NaNO3).8.4 Hydrochloric Acid (HCl), 50 % (v/v), made from con-centrated hydrochloric acid (
24、sp gr 1.19) and water.8.5 Nitric Acid (HNO3), 50 % (v/v), made from concen-trated nitric acid (sp gr 1.44) and water.9. Hazards and Precautions9.1 Follow established laboratory practices when conduct-ing this procedure.9.2 The operator should wear suitable protective gear whenhandling chemicals.9.3
25、The dilution of concentrated acids is conducted in fumehoods by cautiously adding an equal part acid to an equal partof deionized water slowly and with constant stirring.9.4 Samples that are known or suspected to contain radio-active materials must be handled with the appropriate radiationcontrol an
26、d protection as prescribed by site health physics andradiation protection policies.9.5 Samples that are known or suspected to contain toxic,hazardous, or radioactive materials must be handled to mini-mize or eliminate employee exposure. Fusion and leaching ofthe fused samples must be performed in a
27、fume hood,radiation-shielded facility, or other appropriate containment.10. Sample Preparation10.1 If the material to be analyzed is not in powder form, itshould first be broken into small pieces by placing the samplein a plastic bag and then striking the sample with a hammer.The sample should then
28、be ground to pass a 100-mesh sieveusing a clean mortar and pestle such as agate or alumina11. Procedure11.1 Weigh 50 to 250 mg of a powdered sample into aplatinum crucible on an analytical balance to 6 0.1 mg. Thesample size is dependent on the analyte concentration.NOTE 1Although the larger sample
29、size has generally worked well,some matrices may not dissolve entirely. Try smaller sample sizes if thatis the case.11.2 Add 0.5 6 0.005 g each of Na2CO3and Na2B4O7to thecrucible containing the sample.11.3 Stir the sample/flux mixture in the crucible with aspatula until a mixture is obtained. Prepar
30、e a reagent blank.11.4 For samples containing minor to major elements thatdo not oxidize readily (such as Pb, Fe, etc.), add 300 mg ofsodium nitrate. If desired, a Pt lid can be placed on the crucibleto reduce splattering. When adding nitrate, 50 % v/v HNO3should be the diluting acid in order to red
31、uce the attack onplatinum in 11.6.11.5 Using the crucible tongs, place the crucible containingthe sample/flux mixture into a muffle furnace for 25 min at atemperature of 950C. Remove the crucible from the furnaceand allow the melt to cool to room temperature.11.6 Place a stir bar in each crucible an
32、d add 4 mL 50 % v/vHCl, and then dilute with H2O to near the top of the crucible.NOTE 2In some cases, 50 % v/v HNO3may be more appropriate than3Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted
33、 by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeia Convention, Inc. (USPC), Rockville,MD.C 1463 00 (2007)2HCl (that is, samples for ICP-MS, high lead samples, or w
34、hen sodiumnitrate was added).11.7 Place the crucible on the magnetic stirrer, and stir untilthe sample melt is dissolved completely (approximately 30min). If undissolved material remains, the fusions described inSection 20 may need to be tried for cross correlation.11.8 To a calibrated volumetric fl
35、ask, typically 100, 250,500, or 1000 mL, add enough 1:1 HCl to make the finalconcentration 2 % (including the acid already in the crucible).The final volume is determined by the expected analyteconcentrations. Quantitatively transfer the sample solution, anddilute.11.9 The dilution volume is determi
36、ned by the user of thepractice and is dependent upon the desired analysis.11.10 See Appendix X1 for examples of analytical datausing solutions from this fusion.PRACTICE 2FUSION WITH POTASSIUMHYDROXIDE OR SODIUM PEROXIDE12. Scope12.1 This practice covers alkaline fusion of silicate matrixsamples (or
37、other matrices difficult to dissolve in acids) usingan electric Bunsen burner mounted on an orbital shaker. Thispractice has been used successfully to dissolve borosilicateglass, dried glass melter feeds, various simulated nuclear wasteforms, and dried soil samples.12.2 This fusion apparatus and the
38、 alkaline fluxes describedare suitable for use in shielded radiation containment facilitiessuch as hot cells and shielded hoods.12.3 When samples dissolved using this practice are radio-active, the user must follow radiation protection guidelines inplace for such materials.13. Summary of Practice13.
39、1 An aliquot of the dried and ignited sample is weighedinto a tared nickel or zirconium metal crucible and an appro-priate amount of alkaline flux (potassium hydroxide or sodiumperoxide) is added. The crucible is placed on a preheatedelectric Bunsen burner (1000C capability) mounted on anorbital sha
40、ker. The speed of the shaker is adjusted so that theliquefied alkali metal flux and the sample are completely fusedat the bottom of the crucible. When the fusion is complete(about 5 min), the crucible is removed from the heater andcooled to room temperature. The fused mixture is dissolved inwater, a
41、cidified with hydrochloric acid, and diluted to anappropriate volume for subsequent analysis.13.2 With appropriate sample preparation, the solution re-sulting from this procedure can be analyzed for trace metals byICP-AES, ICP-MS, and AAS, and for radionuclides usingapplicable radiochemical methods.
42、14. Significance and Use14.1 This practice describes a method to fuse and dissolvesilicate and refractory matrix samples for subsequent analysisfor trace metals and radionuclides. These samples may containhigh-level radioactive nuclear waste. Nuclear waste glassvitrification plant feeds and product
43、can be characterized usingthis dissolution method followed by the appropriate analysis ofthe resulting solutions. Other matrices such as soil and sedi-ment samples and geological samples may be totally dissolvedusing this practice.14.2 This practice has been used to analyze round-robinsimulated nucl
44、ear waste glass samples.14.3 This practice can be used for bulk analysis of glasssamples for the product consistency test (PCT) as described inTest Methods C 1285 and for the analysis of monolithicradioactive waste glass used in the static leach test as describedin Test Method C 1220.14.4 This pract
45、ice can be used to dissolve the glass refer-ence and testing materials described in Refs (1) and (2).415. Interferences15.1 Elements that form volatile species under these alka-line fusion conditions will be lost during the fusion process.15.2 The high alkali metal (Na or K) content of the resulting
46、sample solutions can cause interference with ICP nebulizer andtorch assemblies due to salt deposition. Dilution of the samplesolutions may be necessary.15.3 The metallic impurities, that is, Na, K, in the alkalineflux used to fuse the samples can cause a positive bias if propercorrections are not ap
47、plied. Method blanks must be determinedto allow correction for flux impurity concentration.16. Apparatus16.1 Analytical Balance, capable of weighing to 6 0.1 mg.16.2 Electric Bunsen Burner, capable of heating to1000C.5to accommodate the larger size (100 mL nickel)metal crucibles, the heat shield on
48、top of the electric BunsenBurner is wrapped with a noncorrosive wire such as inconel atthree evenly distributed locations. With the wire on the heatshield, the large size crucibles are better supported and moreeasily removed. A wire basket made from the noncorrosivewire is also fabricated so that sm
49、aller size crucibles (55 mLzirconium) that pass through the heat shield are supportedevenly in the heating mandrel of the electric Bunsen burner.Fig. 1 shows the electric Bunsen burner mounted on the orbitalshaker with the above modifications for crucible mounting.16.3 Orbital Shaker, including a holder fabricated to fastenthe electric Bunsen burner on the platform (see Fig. 1).616.4 Manual Adjustable Power Supply, for controlling thetemperature of the electric Bunsen burner.716.5 Zirconium Metal Crucible, 55 mL capacity, high form.Different shape and capacity crucibles als
