1、Designation: C 1285 02Standard 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 the designation i
2、ndicates 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 (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 These product consistency test methods
3、 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 species released to a t
4、est 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 elemental release c
5、harac-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 test durations, t
6、est 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 durabilitycharacteristics of ho
7、mogeneous 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 consistency test for pr
8、oduction 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 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibilit
9、y 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. Referenced Documents2.1 ASTM Standards:C 92 Test Methods for Sieve Analysis and Water Content ofRefractory Materials2C 162 Terminology of Gl
10、ass and Glass Products3C 169 Test Methods for Chemical Analysis of Soda-Limeand Borosilicate Glass3C 225 Test Methods for Resistance of Glass Containers toChemical Attack3C 371 Test Method for Wire-Cloth Sieve Analysis of Non-plastic Ceramic Powders3C 429 Test Method for Sieve Analysis of Raw Materi
11、als forGlass Manufacture3C 693 Test Method for Density of Glass by BuoyancyC 1109 Test Method for Analysis of Aqueous Leachatesfrom Nuclear Waste Materials Using Inductively CoupledPlasma-Atomic Emission Spectrometry4C 1174 Practice for Prediction of the Long-Term Behaviorof Materials, Including Was
12、te Forms, Used in EngineeredBarrier Systems (EBS) for Geologic Disposal ofHighLevel Radioactive Waste4C 1463 Practices for Dissolving Glass Containing Radioac-tive and Mixed Waste for Chemical and RadiochemicalAnalysis4D 1125 Test Methods for Electrical Conductivity and Re-sistivity of Water5D 1129
13、Terminology Relating to Water5D 1193 Specification for Reagent Water5D 1293 Test Methods for pH of Water5D 4327 Test Method for Anions in Water by ChemicallySuppressed Ion Chromatography5E 7 Terminology Relating to Metallography6E 177 Practice for Use of the Terms Precision and Bias in1These test me
14、thods 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 June 10, 2002. Published August 2002. Originallypublished as C 1285 94. Last previous edition C 1285 97.2Ann
15、ual Book of ASTM Standards, Vol 15.01.3Annual Book of ASTM Standards, Vol 15.02.4Annual Book of ASTM Standards, Vol 12.01.5Annual Book of ASTM Standards, Vol 11.01.6Annual Book of ASTM Standards, Vol 03.01.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428
16、-2959, United States.ASTM Test Methods7E 456 Terminology Relating to Quality and Statistics7E 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method7E 1402 Terminology Relating to Sampling73. Terminology3.1 Definitions:3.1.1 annealto prevent or remove materia
17、ls processingstresses in glass by controlled cooling from a suitable tempera-ture (modified from Terminology C 162).3.1.2 annealinga controlled cooling process for glassdesigned to reduce thermal residual stress to an acceptablelevel, and, in some cases, modify structure (modified fromTerminology C
18、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 mho/cm at 25C, aminimum electrical resistivity of 18 MVcm at 25C (seeSpecification D 1193 and Terminology D 1129).3.1.4 chemical durability in
19、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.3.1.4.1 DiscussionThe response of a glass under otherconditions is outside the scope of these test methods.3.1.5 closed system testsa system t
20、hat 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, by comparison with a standardor a target, or by other experiments. (Websters New TwentiethCentury Dictionary, 1973)3.1.7 devitrified glassa ho
21、mogeneous and/or phase sepa-rated glass that has partially crystallized during cooling or dueto thermal heat treatment, or both.3.1.8 glassan inorganic product of fusion that has cooledto a rigid condition without crystallizing (see TerminologyC 162); a noncrystalline solid or an amorphous solid.83.
22、1.9 glass ceramicsolid material, partly crystalline andpartly glassy (see Terminology C 162).3.1.10 hazardous waste glassa glass comprised of glassforming additives and hazardous waste.3.1.11 homogeneous glassa glass that is a single amor-phous phase; a glass that is not separated into multipleamorp
23、hous 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 durabilitytest.3.1.14 mixed wastewaste containing both radioactive andhazardous components regulated by the Atomic Energy Act(AEA) (1)9and the Resource
24、 Conservation and Recovery Act(RCRA), (2) respectively; the term “radioactive component”refers only to the actual radionuclides dispersed or suspendedin the waste substance (3).3.1.15 mixed waste glassa glass comprised of glass form-ing additives and both hazardous and radioactive constituents.3.1.1
25、6 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 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, f
26、or 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 radioactiveof or exhibiting radioactivity (Ameri-can Heritage Dictionary, 1973); a material giving or capable ofgiving off radiant energy in the form o
27、f particles or rays, asalpha, beta, and gamma rays, by the disintegration of atomicnuclei; said of certain elements, such as radium, thorium, anduranium, and their products (Websters New Twentieth CenturyDictionary, 1973).3.1.21 radioactivityspontaneous nuclear disintegrationwith emission of corpusc
28、ular 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 amount of leachant as the tests withthe waste form samples but containing no waste form samplethat is conducted under the same conditions as tes
29、ts with thewaste form.3.1.23 sensitizationin austenitic steels such as Types 304and 316, the precipitation of chromium carbide at the grainboundaries in a temperature range of 400900C (modifiedfrom Terminology E 7).3.1.23.1 DiscussionThis constitutes the greatest singlethreat to their corrosion resi
30、stance (4).3.1.24 set of samplessamples tested simultaneously in thesame oven.3.1.25 simulated waste glassa glass comprised of glassforming additives with simulants 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 o
31、f 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); to cause to conform to a given standard, forexample, to make standard or uniform (Websters New Twen-tieth Century Dictionary, 1973).3.1.28 unsens
32、itized austenitic steelstainless steel that isnot sensitized (see sensitization).3.1.29 verifyto determine or test the accuracy of, as bycomparison, investigation, or reference, for example, to con-duct experiments to verify a hypothesis. (The American Heri-tage Dictionary, 1973)3.1.30 vitrification
33、the process of fusing waste with glassmaking chemicals at elevated temperatures to form a wasteglass (see Terminology C 162).4. Summary of Test Methods4.1 Test Method A is the Product Consistency Test (PCT-A),which was developed specifically to measure the chemical7Annual Book of ASTM Standards, Vol
34、 14.02.8Varshneya, A. K., “Fundamentals of Inorganic Glasses,” Academic Press,Boston, MA (1994).9The boldface numbers in parentheses refer to the list of references at the end ofthese test methods.C1285022durability of radioactive glass waste forms as defined in 1.1during production (Table 1) (5). I
35、t 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 remotely on highlyradioactive samples and can yield results rapidly. The glasswaste form does not need to be ann
36、ealed 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 an amount of sizedand cleaned glass waste form that is greater than or equal to 1g is placed in a Type 304L st
37、ainless steel vessel. An amount ofASTM Type I water equal to 10 6 0.5 cm3/g of sample mass(msolid)10is added and the vessel is sealed. The vessel is placedin a constant temperature device at 90 6 2C. The vessels mustbe placed in constant temperature devices so that there is ampleconvection around th
38、e 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 the temperature of the aliquotat the time of the pH measurement is also recorded. Theremaining leachate is f
39、iltered 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 forms (5). The testmethod is easily reproducible, can be performed remotely ifnecessary, and can yield results
40、 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) or tothe size range of interest as long as the glass waste formparticles are less than U.S. Standard ASTM
41、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 stainlesssteel vessel or a PFA TFE-fluorocarbon vessel. An amount ofASTM Type I water equal to 10 6 0.5 cm3/g of sa
42、mple mass(msolid)10is 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 device at 90 6 2C. Other test temperatures arepermissible. It is desirable that inter-comparison of test re-sp
43、onses be conducted at different temperatures to indicatewhether the reaction mechanism changes over the temperaturerange investigated. The vessels must be placed in a constanttemperature device so that there is ample convection aroundthe samples and even heat distribution (Fig. 1). After sevendays 6
44、 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 temperature of the aliquot at the time of the pHmeasurement is also recorded. The remaining leachate isfiltere
45、d 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 22.6.1).5. Significance and Use5.1 These test methods provide data useful for evaluatingthe chemical durab
46、ility (see 3.1.4) of glass waste forms asmeasured by elemental release. Accordingly, it may be appli-cable throughout manufacturing, research, and development.5.1.1 Test Method A can specifically be used to obtain datato evaluate whether the chemical durability of glass wasteforms have been consiste
47、ntly controlled during production (seeTable 1).10If waste forms of different densities 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 result
48、s for sample density (see calculation in Appendix X1).TABLE 1 Summary of Test Methods A and BTest Method A Test Method BType of WasteFormRadioactiveMixedSimulated, HazardousRadioactiveMixedSimulated, HazardousUsage During production for rapidanalysis and for wastecompliance (6)Scoping tests; Crystal
49、li-zation studies (see Note1); Comparative wasteform evaluationTest Vessel Unsensitized 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 m
