1、Designation: C1463 19Standard Practices forDissolving Glass Containing Radioactive and Mixed Wastefor Chemical and Radiochemical Analysis1This standard is issued under the fixed designation C1463; the number immediately following the designation indicates the year oforiginal adoption or, in the case
2、 of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 These practices cover techniques suitable for dissolvingglass samples that may contain nucle
3、ar 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 methods and wet chemica
4、l 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 radiation pro-tection guidel
5、ines 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 materials in glass.1.6
6、 These practices are introduced to provide the user withan alternative means to Test Methods C169 for dissolution ofwaste containing glass in shielded facilities. Test MethodsC169 is not practical for use in such facilities and withradioactive materials.1.7 The ICP-AES methods in Test Methods C1109
7、andC1111 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 C169.1.8 Solutions from this practice may be suitable for analysisusing ICP-MS
8、after establishing laboratory performance crite-ria and verification that the criteria can be met. For example,Test Methods C1287 or C1637 may be used with additionalsample preparation as necessary and appropriate matrix effectconsiderations.1.9 The values stated in SI units are to be regarded assta
9、ndard. Units in parentheses are for information only.1.10 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, health, and environmental practices and deter-mine th
10、e applicability of regulatory limitations prior to use.Specific precautionary statements are given in Sections 10, 20,and 30.1.11 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theD
11、evelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2C169 Test Methods for Chemical Analysis of Soda-Limeand Borosilicate GlassC859 Terminology Relating to Nucle
12、ar MaterialsC1109 Practice for Analysis of Aqueous Leachates fromNuclear Waste Materials Using Inductively CoupledPlasma-Atomic Emission SpectroscopyC1111 Test Method for Determining Elements in WasteStreams by Inductively Coupled Plasma-Atomic EmissionSpectroscopyC1220 Test Method for Static Leachi
13、ng of Monolithic WasteForms for Disposal of Radioactive WasteC1285 Test Methods for Determining Chemical Durabilityof Nuclear, Hazardous, and Mixed Waste Glasses andMultiphase Glass Ceramics: The Product Consistency Test(PCT)C1287 Test Method for Determination of Impurities in1These practices are un
14、der 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, 2019. Published February 2019. Originallyapproved in 2000. Last previous edition approved in 2013 as C1463 13. DOI:10.1520/C1463-
15、19.2For 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 onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Bo
16、x C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by t
17、he World Trade Organization Technical Barriers to Trade (TBT) Committee.1Nuclear Grade Uranium Compounds by InductivelyCoupled Plasma Mass SpectrometryC1637 Test Method for the Determination of Impurities inPlutonium Metal:Acid Digestion and Inductively CoupledPlasma-Mass Spectroscopy (ICP-MS) Analy
18、sisD1193 Specification for Reagent WaterE11 Specification for Woven Wire Test Sieve Cloth and TestSieves3. Terminology3.1 For definitions of terms used in this Practice, refer toTerminology C859.4. Summary of Practice4.1 The three practices for dissolving silicate matrixsamples each require the samp
19、le to be dried and ground to afine powder.4.2 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 anal
20、yses.4.3 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.4.4 Dissolution of the sample using a mi
21、crowave oven isdescribed in the third practice. The ground sample is digestedin a microwave oven using a mixture of hydrofluoric (HF) andnitric (HNO3) acids. Boric acid is added to the resultingsolution to complex excess fluoride ions.4.5 These three practices offer alternative dissolution meth-ods
22、for a total analysis of a glass sample for major, minor, andradionuclide components.5. Reagents5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of
23、the American Chemical Society.35.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean at least Type II reagentwater in conformance with Specification D1193.PRACTICE 1FUSION WITH SODIUMTETRABORATE AND SODIUM CARBONATE6. Scope6.1 This practice covers flux fusion
24、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 can be measuredin these solutions, depending on the samp
25、le weights anddilution volumes used during preparation.7. Technical Precautions7.1 This procedure is not useful for the determination ofboron or sodium since these elements are contained in the fluxmaterial.7.2 The user is cautioned that with analysis by ICP-AES,AAS, and ICP-MS, the high sodium conc
26、entrations from theflux may cause interferences.7.3 Elements that form volatile species under these alkalinefusion conditions may be lost during the fusion process (that is,As and Sb).8. Apparatus8.1 Platinum Crucibles, 30 mL.8.2 Balance, analytical type, precision to 0.1 mg.8.3 Furnace, with heatin
27、g capacity to 1000C.8.4 Crucible Tongs, (cannot be made of iron, unless usingplatinum-clad tips).8.5 Polytetrafluoroethylene (PTFE) Beaker, 125-mL capac-ity.8.6 Magnetic Stir Bar, PTFE-coated (0.32 to 0.64 cm).8.7 Magnetic Stirrer.8.8 Mortar and Pestle, agate or alumina (or equivalentgrinding appara
28、tus).8.9 Sieves, 150 m (100 mesh), as described in SpecificationE11.9. Reagents and Materials9.1 Anhydrous Sodium Carbonate (Na2CO3).9.2 Anhydrous Sodium Tetraborate (Na2B4O7).9.3 Sodium Nitrate (NaNO3).9.4 Hydrochloric Acid (HCl), 50 % (v/v), made from con-centrated hydrochloric acid (sp gr 1.19) a
29、nd water.9.5 Nitric Acid (HNO3), 50 % (v/v), made from concen-trated nitric acid (sp gr 1.44) and water.10. Hazards and Precautions10.1 Follow established laboratory practices when conduct-ing this procedure.10.2 The operator should wear suitable protective gearwhen handling chemicals.10.3 The dilut
30、ion of concentrated acids is conducted infume hoods by cautiously adding an equal part acid to an equalpart of deionized water slowly and with constant stirring.10.4 Samples that are known or suspected to contain radio-active materials must be handled with the appropriate radiationcontrol and protec
31、tion as prescribed by site health physics andradiation protection policies.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for Laborator
32、yChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.C1463 19210.5 Samples that are known or suspected to contain toxic,hazardous, or radioactive materials must be handled to mini-mize or elimina
33、te employee exposure. Fusion and leaching ofthe fused samples must be performed in a fume hood,radiation-shielded facility, or other appropriate containment.11. Sample Preparation11.1 If the material to be analyzed is not in powder form, itshould first be broken into small pieces by placing the samp
34、lein a plastic bag and then striking the sample with a hammer.The sample should then be ground to pass a 150 m (100-mesh) sieve using a clean mortar and pestle such as agate oralumina.12. Procedure12.1 Weigh 50 to 250 mg of a powdered sample into aplatinum crucible on an analytical balance to 60.1 m
35、g. Thesample size is dependent on the analyte concentration.NOTE 1Although the larger sample size has generally worked well,some matrices may not dissolve entirely, and a smaller sample size may benecessary.12.2 Add 0.5 6 0.005 g each of Na2CO3and Na2B4O7to thecrucible containing the sample.12.3 Sti
36、r the sample/flux mixture in the crucible with aspatula until a mixture is obtained. Prepare a reagent blank.12.4 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
37、 splattering. When adding nitrate, 50 % v/v HNO3should be the diluting acid in order to reduce the attack onplatinum in 12.6.12.5 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 furn
38、aceand allow the melt to cool to room temperature.12.6 Place a stir bar in each crucible and 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 thanHCl (that is, samples for ICP-MS, high lead samples, or when sodiu
39、mnitrate was added).12.7 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 22 may need to be tried for cross correlation.12.8 To a calibrated volumetric flask, typi
40、cally 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.12.9 The dilution volume is determined by th
41、e user of thepractice and is dependent upon the desired analysis.13. Precision and Bias13.1 This practice addresses only the preparation steps inthe overall preparation and measurement of the sample ana-lytes. Since the preparation alone does not produce any results,the user must determine the preci
42、sion and bias resulting fromthis preparation and subsequent analysis.13.2 See Appendix X1 for examples of analytical data usingsolutions from this fusion.PRACTICE 2FUSION WITH POTASSIUMHYDROXIDE OR SODIUM PEROXIDE14. Scope14.1 This practice covers alkaline fusion of silicate matrixsamples (or other
43、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.14.2 This fusion apparatus and the alkal
44、ine fluxes describedare suitable for use in shielded radiation containment facilitiessuch as hot cells and shielded hoods.14.3 When samples dissolved using this practice areradioactive, the user must follow radiation protection guide-lines in place for such materials.15. Summary of Practice15.1 An a
45、liquot 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 shaker. T
46、he 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, acidifi
47、ed with hydrochloric acid, and diluted to anappropriate volume for subsequent analysis.15.2 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.16. Si
48、gnificance and Use16.1 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 can be
49、 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.16.2 This practice has been used to analyze round-robinsimulated nuclear waste glass samples.16.3 This practice can be used for bulk analysis of glasssamples for the product consistency test (PCT) as described inTest Methods C1285 and for the analysis of monolithicC1463 193radioactive waste glass used in the static leach test as describedin Test Me
