1、Designation: C1463 00 (Reapproved 2007)C1463 13Standard 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 oforigina
2、l adoption or, in the case 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 dissolving glass sam
3、ples that may contain nuclear wastes. These techniquesused together or independently will produce solutions that can be analyzed by inductively coupled plasma atomic emissionspectroscopy (ICP-AES), inductively coupled plasma mass spectrometry (ICP-MS), atomic absorption spectrometry (AAS),radiochemi
4、cal methods and wet chemical techniques for major components, minor components and radionuclides.1.2 One of the fusion practices and the microwave practice can be used in hot cells and shielded hoods after modification tomeet local operational requirements.1.3 The user of these practices must follow
5、 radiation protection guidelines in place for their specific laboratories.1.4 Additional information relating to safety is included in the text.1.5 The dissolution techniques described in these practices can be used for quality control of the feed materials and the productof plants vitrifying nuclea
6、r waste materials in glass.1.6 These practices are introduced to provide the user with an alternative means to Test Methods C169 for dissolution of wastecontaining glass in shielded facilities. Test Methods C169 is not practical for use in such facilities and with radioactive materials.1.7 The ICP-A
7、ES methods in Test Methods C1109 and C1111 can be used to analyze the dissolved sample with additionalsample preparation as necessary and with matrix effect considerations. Additional information as to other analytical methods canbe found in Test Method C169.1.8 Solutions from this practice may be s
8、uitable for analysis using ICP-MS after establishing laboratory performance criteria.1.9 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.10 This standard does not purport to address all of the safety concerns, if any, associ
9、ated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. Specific precautionary statements are given in SectionSections 10, 1820, and 30.2. Referenced Documents2
10、.1 ASTM Standards:2C169 Test Methods for Chemical Analysis of Soda-Lime and Borosilicate GlassC859 Terminology Relating to Nuclear MaterialsC1109 Practice for Analysis of Aqueous Leachates from Nuclear Waste Materials Using Inductively Coupled Plasma-AtomicEmission SpectroscopyC1111 Test Method for
11、Determining Elements in Waste Streams by Inductively Coupled Plasma-Atomic Emission SpectroscopyC1220 Test Method for Static Leaching of Monolithic Waste Forms for Disposal of Radioactive WasteC1285 Test Methods for Determining Chemical Durability of Nuclear, Hazardous, and Mixed Waste Glasses and M
12、ultiphaseGlass Ceramics: The Product Consistency Test (PCT)D1193 Specification for Reagent WaterE11 Specification for Woven Wire Test Sieve Cloth and Test Sieves1 These practices are under the jurisdiction ofASTM Committee C26 on Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C
13、26.05 on Methods of Test.Current edition approved Feb. 1, 2007July 1, 2013. Published March 2007July 2013. Originally approved in 2000. Last previous edition approved in 20002007 asC1463 00.C1463 00 (2007). DOI: 10.1520/C1463-00R07.10.1520/C1463-13.2 For referencedASTM standards, visit theASTM websi
14、te, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication
15、 of what changes have been made to the previous version. Becauseit 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 versionof the standard as published by ASTM is to be conside
16、red the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13. Terminology3.1 For definitions of terms used in this Practice, refer to Terminology C859.4. Summary of Practice4.1 The three practices for dissolving silicat
17、e matrix samples each require the sample to be dried and ground to a fine powder.4.2 In the first practice, a mixture of sodium tetraborate (Na2B4O7) and sodium carbonate (Na2CO3) is mixed with the sampleand fused in a muffle for 25 min at 950C. The sample is cooled, dissolved in hydrochloric acid,
18、and diluted to appropriate volumefor analyses.4.3 The second practice described in this standard involves fusion of the sample with potassium hydroxide (KOH) or sodiumperoxide (Na2O2) using an electric bunsenBunsen burner, dissolving the fused sample in water and dilute HCl, and making tovolume for
19、analysis.4.4 Dissolution of the sample using a microwave oven is described in the third practice. The ground sample is digested in amicrowave oven using a mixture of hydrofluoric (HF) and nitric (HNO3) acids. Boric acid is added to the resulting solution tocomplex excess fluoride ions.4.5 These thre
20、e practices offer alternative dissolution methods for a total analysis of a glass sample for major, minor, andradionuclide components.5. Reagents5.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents conform to the specif
21、ications of the Committee on Analytical Reagents of the American Chemical Society.35.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean at least Type II reagent waterin conformance with Specification D1193.PRACTICE 1FUSION WITH SODIUM TETRABORATE AND SODIUM
22、CARBONATE6. Scope6.1 This practice covers flux fusion sample decomposition and dissolution for the determination of SiO2 and many other oxidesin glasses, ceramics, and raw materials. The solutions are analyzed by atomic spectroscopy methods. Analyte concentrationsranging from trace to major levels c
23、an be measured in these solutions, depending on the sample weights and dilution volumes usedduring preparation.7. Technical Precautions7.1 This procedure is not useful for the determination of boron or sodium since these elements are contained in the flux material.7.2 The user is cautioned that with
24、 analysis by ICP-AES,AAS, and ICP-MS, the high sodium concentrations from the flux maycause interferences.7.3 Elements that form volatile species under these alkaline fusion conditions may be lost during the fusion process (that is,Asand Sb).8. Apparatus8.1 Platinum Crucibles, 30 mL.8.2 Balance, ana
25、lytical type, precision to 0.1 mg.8.3 Furnace, with heating capacity to 1000C.8.4 Crucible Tongs, (cannot be made of iron, unless using platinum-clad tips).8.5 Polytetrafluoroethylene (PTFE) Beaker, 125-mL capacity.8.6 Magnetic Stir Bar, PTFE-coated (0.32 to 0.64 cm).8.7 Magnetic Stirrer.8.8 Mortar
26、and Pestle, agate or alumina (or equivalent grinding apparatus).8.9 Sieves, 100 mesh.3 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards f
27、or Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.C1463 1329. Reagents and Materials9.1 Anhydrous Sodium Carbonate (Na2CO3).9.2 Anhydrous Sodium Tetraborate (Na2B4O7).9.3 Sodium
28、Nitrate (NaNO3).9.4 Hydrochloric Acid (HCl), 50 % (v/v), made from concentrated hydrochloric acid (sp gr 1.19) and water.9.5 Nitric Acid (HNO3), 50 % (v/v), made from concentrated nitric acid (sp gr 1.44) and water.10. Hazards and Precautions10.1 Follow established laboratory practices when conducti
29、ng this procedure.10.2 The operator should wear suitable protective gear when handling chemicals.10.3 The dilution of concentrated acids is conducted in fume hoods by cautiously adding an equal part acid to an equal part ofdeionized water slowly and with constant stirring.10.4 Samples that are known
30、 or suspected to contain radioactive materials must be handled with the appropriate radiationcontrol and protection as prescribed by site health physics and radiation protection policies.10.5 Samples that are known or suspected to contain toxic, hazardous, or radioactive materials must be handled to
31、 minimizeor eliminate employee exposure. Fusion and leaching of the fused samples must be performed in a fume hood, radiation-shieldedfacility, or other appropriate containment.11. Sample Preparation11.1 If the material to be analyzed is not in powder form, it should first be broken into small piece
32、s by placing the sample ina plastic bag and then striking the sample with a hammer. The sample should then be ground to pass a 100-mesh sieve using aclean mortar and pestle such as agate or alumina12. Procedure12.1 Weigh 50 to 250 mg of a powdered sample into a platinum crucible on an analytical bal
33、ance to 60.1 mg. The sample sizeis dependent on the analyte concentration.NOTE 1Although the larger sample size has generally worked well, some matrices may not dissolve entirely. Try smaller sample sizes if that is thecase.12.2 Add 0.5 6 0.005 g each of Na2CO3 and Na2B4O7 to the crucible containing
34、 the sample.12.3 Stir the sample/flux mixture in the crucible with a spatula until a mixture is obtained. Prepare a reagent blank.12.4 For samples containing minor to major elements that do not oxidize readily (such as Pb, Fe, etc.), add 300 mg of sodiumnitrate. If desired, a Pt lid can be placed on
35、 the crucible to reduce splattering. When adding nitrate, 50 % v/v HNO3 should be thediluting acid in order to reduce the attack on platinum in 11.612.6.12.5 Using the crucible tongs, place the crucible containing the sample/flux mixture into a muffle furnace for 25 min at atemperature of 950C. Remo
36、ve the crucible from the furnace and allow the melt to cool to room temperature.12.6 Place a stir bar in each crucible and add 4 mL 50 % v/v HCl, and then dilute with H2O to near the top of the crucible.NOTE 2In some cases, 50 % v/v HNO3 may be more appropriate than HCl (that is, samples for ICP-MS,
37、 high lead samples, or when sodium nitratewas added).12.7 Place the crucible on the magnetic stirrer, and stir until the sample melt is dissolved completely (approximately 30 min).If undissolved material remains, the fusions described in Section 2022 may need to be tried for cross correlation.12.8 T
38、o a calibrated volumetric flask, typically 100, 250, 500, or 1000 mL, add enough 1:1 HCl to make the final concentration2 % (including the acid already in the crucible). The final volume is determined by the expected analyte concentrations.Quantitatively transfer the sample solution, and dilute.12.9
39、 The dilution volume is determined by the user of the practice and is dependent upon the desired analysis.11.10 See Appendix X1 for examples of analytical data using solutions from this fusion.13. Precision and Bias13.1 This practice addresses only the preparation steps in the overall preparation an
40、d measurement of the sample analytes. Sincethe preparation alone does not produce any results, the user must determine the precision and bias resulting from this preparationand subsequent analysis.13.2 See Appendix X1 for examples of analytical data using solutions from this fusion.C1463 133PRACTICE
41、 2FUSION WITH POTASSIUM HYDROXIDE OR SODIUM PEROXIDE14. Scope14.1 This practice covers alkaline fusion of silicate matrix samples (or other matrices difficult to dissolve in acids) using anelectric Bunsen burner mounted on an orbital shaker. This practice has been used successfully to dissolve boros
42、ilicate glass, driedglass melter feeds, various simulated nuclear waste forms, and dried soil samples.14.2 This fusion apparatus and the alkaline fluxes described are suitable for use in shielded radiation containment facilities suchas hot cells and shielded hoods.14.3 When samples dissolved using t
43、his practice are radioactive, the user must follow radiation protection guidelines in placefor such materials.15. Summary of Practice15.1 An aliquot of the dried and ignited sample is weighed into a tared nickel or zirconium metal crucible and an appropriateamount of alkaline flux (potassium hydroxi
44、de or sodium peroxide) is added. The crucible is placed on a preheated electric Bunsenburner (1000C capability) mounted on an orbital shaker. The speed of the shaker is adjusted so that the liquefied alkali metal fluxand the sample are completely fused at the bottom of the crucible. When the fusion
45、is complete (about 5 min), the crucible isremoved from the heater and cooled to room temperature.The fused mixture is dissolved in water, acidified with hydrochloric acid,and diluted to an appropriate volume for subsequent analysis.15.2 With appropriate sample preparation, the solution resulting fro
46、m this procedure can be analyzed for trace metals byICP-AES, ICP-MS, and AAS, and for radionuclides using applicable radiochemical methods.16. Significance and Use16.1 This practice describes a method to fuse and dissolve silicate and refractory matrix samples for subsequent analysis fortrace metals
47、 and radionuclides. These samples may contain high-level radioactive nuclear waste. Nuclear waste glass vitrificationplant feeds and product can be characterized using this dissolution method followed by the appropriate analysis of the resultingsolutions. Other matrices such as soil and sediment sam
48、ples and geological samples may be totally dissolved using this practice.16.2 This practice has been used to analyze round-robin simulated nuclear waste glass samples.16.3 This practice can be used for bulk analysis of glass samples for the product consistency test (PCT) as described in TestMethods
49、C1285 and for the analysis of monolithic radioactive waste glass used in the static leach test as described in Test MethodC1220.16.4 This practice can be used to dissolve the glass reference and testing materials described in Refs (1) and (2).417. Interferences17.1 Elements that form volatile species under these alkaline fusion conditions will be lost during the fusion process.17.2 The high alkali metal (Na or K) content of the resulting sample solutions can cause interference with ICP nebulizer andtorch assemblies due to salt deposition. Dilution of the sample solut
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