1、Designation: C 1285 02 (Reapproved 2008)Standard Test Methods forDetermining Chemical Durability of Nuclear, Hazardous, andMixed Waste Glasses and Multiphase Glass Ceramics: TheProduct Consistency Test (PCT)1This standard is issued under the fixed designation C 1285; the number immediately following
2、 the designation indicates the year oforiginal 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 product consist
3、ency test methods A and B evalu-ate the chemical durability of homogeneous glasses, phaseseparated glasses, devitrified glasses, glass ceramics, and/ormultiphase glass ceramic waste forms hereafter collectivelyreferred to as “glass waste forms” by measuring the concen-trations of the chemical specie
4、s released to a test solution.1.1.1 Test Method A is a seven-day chemical durability testperformed at 90 6 2C in a leachant of ASTM-Type I water.The test method is static and conducted in stainless steelvessels. Test Method A can specifically be used to evaluatewhether the chemical durability and el
5、emental release charac-teristics of nuclear, hazardous, and mixed glass waste formshave been consistently controlled during production. This testmethod is applicable to radioactive and simulated glass wasteforms as defined above.1.1.2 Test Method B is a durability test that allows testing atvarious
6、test durations, test temperatures, mesh size, mass ofsample, leachant volume, and leachant compositions. This testmethod is static and can be conducted in stainless steel or PFATFE-fluorocarbon vessels, or both. Test Method B can specifi-cally be used to evaluate the relative chemical durabilitychar
7、acteristics of homogeneous glasses, phase separatedglasses, devitrified glasses, glass ceramics, and/or multiphaseglass ceramic waste forms. This test method is applicable toradioactive (nuclear) and mixed, hazardous, and simulatedwaste forms as defined above. Test Method B cannot be usedas a consis
8、tency test for production of high level radioactiveglass waste forms.1.2 These test methods must be performed in accordancewith all quality assurance requirements for acceptance of thedata.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in
9、thisstandard.1.4 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 determine the applica-bility of regulatory limitations prior to use.2.
10、 Referenced Documents2.1 ASTM Standards:2C92 Test Methods for SieveAnalysis and Water Content ofRefractory MaterialsC 162 Terminology of Glass and Glass ProductsC 169 Test Methods for Chemical Analysis of Soda-Limeand Borosilicate GlassC 225 Test Methods for Resistance of Glass Containers toChemical
11、 AttackC 371 Test Method for Wire-Cloth Sieve Analysis of Non-plastic Ceramic PowdersC 429 Test Method for SieveAnalysis of Raw Materials forGlass ManufactureC 693 Test Method for Density of Glass by BuoyancyC 1109 Practice for Analysis of Aqueous Leachates fromNuclear Waste Materials Using Inductiv
12、ely CoupledPlasma-Atomic Emission SpectroscopyC 1174 Practice for Prediction of the Long-Term Behaviorof Materials, Including Waste Forms, Used in EngineeredBarrier Systems (EBS) for Geological Disposal of High-Level Radioactive WasteC 1463 Practices for Dissolving Glass Containing Radioac-tive and
13、Mixed Waste for Chemical and RadiochemicalAnalysisC 1125 Test Method for Penetration Index of AsbestosD 1129 Terminology Relating to WaterD 1193 Specification for Reagent WaterD 1293 Test Methods for pH of WaterD 4327 Test Method for Anions in Water by ChemicallySuppressed Ion Chromatography1These t
14、est methods are under the jurisdiction of ASTM Committee C26 onNuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.13 onSpent Fuel and High Level Waste.Current edition approved July 1, 2008. Published August 2008. Originallyapproved in 1994. Last previous edition approved in 200
15、2 as C 1285 02.2For 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.1Copyright ASTM International, 100 Barr Harbor
16、 Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.E7 Terminology Relating to MetallographyE 177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE 456 Terminology Relating to Quality and StatisticsE 691 Practice for Conducting an Interlaboratory Study toDetermin
17、e the Precision of a Test MethodE 1402 Terminology Relating to Sampling3. Terminology3.1 Definitions:3.1.1 annealto prevent or remove materials processingstresses in glass by controlled cooling from a suitable tempera-ture (modified from Terminology C 162).3.1.2 annealinga controlled cooling process
18、 for glassdesigned to reduce thermal residual stress to an acceptablelevel, and, in some cases, modify structure (modified fromTerminology C 162).3.1.3 ASTM Type I waterpurified water with a maximumtotal matter content including soluble silica of 0.1 g/m3,amaximum electrical conductivity of 0.056 mh
19、o/cm at 25C, aminimum electrical resistivity of 18 MVcm at 25C (seeSpecification D 1193 and Terminology D 1129).3.1.4 chemical durability in these test methods, the resis-tance of a glass waste form to the release of its constituents toan aqueous solution under the specific conditions of this test.3
20、.1.4.1 DiscussionThe response of a glass under otherconditions is outside the scope of these test methods.3.1.5 closed system testsa system that precludes thetransport of matter either into or out of the system.3.1.6 consistently controlledto verify with a high degreeof accuracy, as an experiment, b
21、y comparison with a standardor a target, or by other experiments. (Websters New TwentiethCentury Dictionary, 1973)3.1.7 devitrified glassa homogeneous or phase (or both)separated glass that has partially crystallized during cooling ordue to thermal heat treatment, or both.3.1.8 glassan inorganic pro
22、duct of fusion that has cooledto a rigid condition without crystallizing (see TerminologyC 162); a noncrystalline solid or an amorphous solid.33.1.9 glass ceramicsolid material, partly crystalline andpartly glassy (see Terminology C 162).3.1.10 hazardous waste glassa glass comprised of glassforming
23、additives and hazardous waste.3.1.11 homogeneous glassa glass that is a single amor-phous phase; a glass that is not separated into multipleamorphous phases.3.1.12 leachantthe solution that is being used, or isintended for use, in a durability test.3.1.13 leachatethe solution resulting from a durabi
24、litytest.3.1.14 mixed wastewaste containing both radioactive andhazardous components regulated by the Atomic Energy Act(AEA) (1)4and the Resource Conservation and Recovery Act(RCRA), (2) respectively; the term “radioactive component”refers only to the actual radionuclides dispersed or suspendedin th
25、e waste substance (3).3.1.15 mixed waste glassa glass comprised of glass form-ing additives and both hazardous and radioactive constituents.3.1.16 multiphase glass ceramic waste forma ceramicconsisting of more than one phase, one of which must be aglass.3.1.17 nuclear waste glassa glass comprised of
26、 glassforming additives and radioactive waste.3.1.18 open system testsa system that permits the trans-port of matter into or out of the system, for example, O2or CO2diffusion, or both, into or out of the system.3.1.19 phase separated glassa glass containing more thanone amorphous phase.3.1.20 radioa
27、ctiveof or exhibiting radioactivity (Ameri-can Heritage Dictionary, 1973); a material giving or capable ofgiving off radiant energy in the form of particles or rays, asalpha, beta, and gamma rays, by the disintegration of atomicnuclei; said of certain elements, such as radium, thorium, anduranium, a
28、nd their products (Websters New Twentieth CenturyDictionary, 1973).3.1.21 radioactivityspontaneous nuclear disintegrationwith emission of corpuscular or electromagnetic radiation, orboth (consult Terminology D 1129).3.1.22 sample blanka test in a cleaned test vessel that hasbeen filled with the same
29、 amount of leachant as the tests withthe waste form samples but containing no waste form samplethat is conducted under the same conditions as tests with thewaste form.3.1.23 sensitizationin austenitic steels such as Types 304and 316, the precipitation of chromium carbide at the grainboundaries in a
30、temperature range of 400900C (modifiedfrom Terminology E7).3.1.23.1 DiscussionThis constitutes the greatest singlethreat to their corrosion resistance (4).3.1.24 set of samplessamples tested simultaneously in thesame oven.3.1.25 simulated waste glassa glass comprised of glassforming additives with s
31、imulants of, or actual chemical spe-cies, or both, in radioactive wastes or in mixed nuclear wastes,or both.3.1.26 standardto have the quality of a model, gage,pattern, or type. (Websters New Twentieth Century Dictionary,1973)3.1.27 standardizeto make, cause, adjust, or adapt to fit astandard (3); t
32、o cause to conform to a given standard, forexample, to make standard or uniform (Websters New Twen-tieth Century Dictionary, 1973).3.1.28 unsensitized austenitic steelstainless steel that isnot sensitized (see sensitization).3.1.29 verifyto determine or test the accuracy of, as bycomparison, investi
33、gation, or reference, for example, to con-duct experiments to verify a hypothesis. (The American Heri-tage Dictionary, 1973)3.1.30 vitrificationthe process of fusing waste with glassmaking chemicals at elevated temperatures to form a wasteglass (see Terminology C 162).3Varshneya, A. K., “Fundamental
34、s of Inorganic Glasses,” Academic Press,Boston, MA (1994).4The boldface numbers in parentheses refer to the list of references at the end ofthese test methods.C 1285 02 (2008)24. Summary of Test Methods4.1 Test MethodAis the Product Consistency Test (PCT-A),which was developed specifically to measur
35、e the chemicaldurability of radioactive glass waste forms as defined in 1.1during production (Table 1) (5). It can also be used to measurethe chemical durability of hazardous, mixed, and varioussimulated glass waste forms as defined in 1.1. The test methodis easily reproducible, can be performed rem
36、otely on highlyradioactive samples and can yield results rapidly. The glasswaste form does not need to be annealed prior to testing. In thistest method the glass waste form is crushed and sieved to U.S.Standard ASTM 100 to + 200 mesh (0.1490.074 mm), theparticles are cleaned of adhering fines, and a
37、n amount of sizedand cleaned glass waste form that is greater than or equal to 1g is placed in a Type 304L stainless steel vessel. An amount ofASTM Type I water equal to 10 6 0.5 cm3/g of sample mass(msolid)5is added and the vessel is sealed. The vessel is placedin a constant temperature device at 9
38、0 6 2C. The vessels mustbe placed in constant temperature devices so that there is ampleconvection around the samples and even heat distribution (Fig.1). After seven days 63.4 h the vessel is removed from theoven and cooled to ambient temperature. The pH is measuredon an aliquot of the leachate and
39、the temperature of the aliquotat the time of the pH measurement is also recorded. Theremaining leachate is filtered and sent for analysis.4.2 Test Method B is the Product Consistency Test (PCT-B),which was developed to measure the chemical durability ofradioactive, mixed, or simulated glass waste fo
40、rms (5). The testmethod is easily reproducible, can be performed remotely ifnecessary, and can yield results rapidly. The glass waste formdoes not need to be annealed prior to testing. In this testmethod the glass waste form is crushed and sieved to U.S.Standard ASTM 100 to + 200 mesh (0.1490.074 mm
41、) or tothe size range of interest as long as the glass waste formparticles are less than U.S. Standard ASTM 40 mesh (0.420mm). The particles are cleaned of adhering fines (see Note 1),and an amount of sized and cleaned glass waste form greaterthan or equal to1gisplaced in either a Type 304 L stainle
42、sssteel vessel or a PFA TFE-fluorocarbon vessel. An amount ofASTM Type I water equal to 10 6 0.5 cm3/g of sample mass(msolid)5is added and the vessel is sealed. Other ratios ofsolution volume to sample mass are allowed and otherleachants are allowed. The vessel is placed in a constanttemperature dev
43、ice at 90 6 2C. Other test temperatures arepermissible. It is desirable that inter-comparison of test re-sponses be conducted at different temperatures to indicatewhether the reaction mechanism changes over the temperaturerange investigated. The vessels must be placed in a constanttemperature device
44、 so that there is ample convection aroundthe samples and even heat distribution (Fig. 1). After sevendays 6 3.4 h, or other optional test durations, the vessel isremoved from the constant temperature device and cooled toambient temperature. The pH is measured on an aliquot of theleachate and the tem
45、perature of the aliquot at the time of the pHmeasurement is also recorded. The remaining leachate isfiltered and sent for analysis.NOTE 1Devitrified glasses, glass ceramics, and multiphase glassceramic waste forms containing soluble secondary phases require specialhandling procedures (see 19.6.1 and
46、 22.6.1).5. Significance and Use5.1 These test methods provide data useful for evaluatingthe chemical durability (see 3.1.4) of glass waste forms asmeasured by elemental release. Accordingly, it may be appli-cable throughout manufacturing, research, and development.5If waste forms of different densi
47、ties are being compared then the leachateresults from the test must be compared using the calculation in 25.2.4 whichaccounts for density differences in the SA/V term in the denominator which adjuststhe leachate results for sample density (see calculation in Appendix X1).TABLE 1 Summary of Test Meth
48、ods A and BTest Method A Test Method BType of WasteFormRadioactiveMixedSimulated, HazardousRadioactiveMixedSimulated, HazardousUsage During production for rapidanalysis and for wastecompliance (6)Scoping tests; Crystalli-zation studies (see Note1); Comparative wasteform evaluationTest Vessel Unsensi
49、tized Type 304Lstainless steel; vesselsrated to 0.5 MPa (seeSection 9)Unsensitized Type 304Lstainless steel or PFATFE-fluorocarbon9vesselsrated to 0.5 MPa (seeSection 9)Test Duration 7 days 6 2% 7 days 6 2% or varyingtimesLeachant ASTM Type I water ASTM Type I water or othersolutionsCondition Static StaticMinimum SampleMass$1g $1gParticle Size U.S. Standard ASTM 100to + 200 mesh (0.149 to0.074 mm)U.S. Standard ASTM 100to + 200 mesh (0.149 to0.074 mm) or other sizeswhich are 20 mL capacity designed to takeinternal pressures of 0