1、Designation: C1663 17Standard Test Method forMeasuring Waste Glass or Glass Ceramic Durability byVapor Hydration Test1This standard is issued under the fixed designation C1663; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the ye
2、ar 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 The vapor hydration test method can be used to studythe corrosion of a waste forms such as glasses and glasscera
3、mics2upon exposure to water vapor at elevated tempera-tures. In addition, the alteration phases that form can be used asindicators of those phases that may form under repositoryconditions. These tests; which allow altering of glass at highsurface area to solution volume ratio; provide useful informa
4、-tion regarding the alteration phases that are formed, thedisposition of radioactive and hazardous components, and thealteration kinetics under the specific test conditions. Thisinformation may be used in performance assessment (McGrailet al, 2002 (1)3for example).1.2 This test method must be perfor
5、med in accordance withall quality assurance requirements for acceptance of the data.1.3 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 environment
6、al practices and deter-mine the applicability of regulatory limitations prior to use.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Gu
7、ides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:4C162 Terminology of Glass and Glass ProductsC859 Terminology Relating to Nuclear MaterialsD1125 Test Methods for Electrical Conductivity and Resis-ti
8、vity of WaterD1193 Specification for Reagent WaterD1293 Test Methods for pH of WaterE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 Please refer to Terminologies
9、 C162 and C859 foradditional terminology which may not be listed below.3.2 Definitions:3.2.1 immobilized low-activity wastevitrified low-activityfraction of waste presently contained in Hanford Site tanks.3.2.2 performance assessmentexamines the long-term en-vironmental and human health effects asso
10、ciated with theplanned disposal of waste. Mann et al, 2001 (2)3.2.3 sampleinitial test material with known composition.3.2.4 specimenspecimen is a part of the sample used fortesting.3.2.5 traceable standarda material that supplies a link toknown test response in standards international units by anat
11、ional or international standards body, for example, NIST.3.3 Abbreviations:3.3.1 DIWASTM Type I deionized water3.3.2 EDSenergy dispersive X-ray spectroscopy1This test method is under the jurisdiction of ASTM Committee C26 on NuclearFuel Cycle and is the direct responsibility of Subcommittee C26.13 o
12、n Spent Fueland High Level Waste.Current edition approved Nov. 1, 2017. Published December 2017. Originallyapproved in 2009. Last previous edition approved in 2009 as C1663 09. DOI:10.1520/C1663-17.2The precision and bias statements are only valid for glass waste forms at thistime. The test may be (
13、and has been) performed on other waste forms; however, theprecision of such tests are currently unknown.3The boldface numbers in parentheses refer to the list of references at the end ofthis standard.4For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Servic
14、e 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 Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in acc
15、ordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.13.3.3 OMoptical microscopy3.3.
16、4 OM/IAoptical microscope connected to an imageanalysis system3.3.5 PTFEpolytetrafluoroethylene (chemical compoundcommonly referred to as Teflon)3.3.6 SEMscanning electron microscope3.3.7 SiC papersilicon-carbide paper3.3.8 TBDto be determined3.3.9 TEMtransmission electron microscope3.3.10 Tgglass t
17、ransition temperature3.3.11 VHTvapor hydration test3.3.12 WDSwave-length dispersive spectroscopy3.3.13 XRDX-ray diffraction3.3.14 %RSDpercent relative standard deviation4. Summary of Test Method4.1 For the vapor hydration tests, glass or glass ceramicspecimens (referred to generally as glass samples
18、 in this testmethod) are suspended from a support rod inside the test vesselwith platinum wire. A volume of water determined by thevolume of the test vessel and the test temperature is added tothe vessel. The vessel is then sealed and placed in an oven atthe desired test temperature and left undistu
19、rbed. After thedesired test duration, the vessel is removed from the oven andthe bottom of the vessel is cooled to condense the vapor in thevessel. Specimens are removed and examined with opticalmicroscopy, XRD, SEM, and other analytical methods. Theremaining glass or glass ceramic thickness is meas
20、ured andalteration phases are identified.5. Significance and Use5.1 The vapor hydration test can be used to study thecorrosion of glass and glass ceramic waste forms underconditions of high temperature and contact by water vapor orthin films of water. This method may serve as an acceleratedtest for
21、some materials, since the high temperatures willaccelerate thermally activated processes. A wide range of testtemperatures have been reported in the literature 40C (Ebertet al, 2005 (3), for example) to 300C (Vienna et al, 2001 (4),for example). It should be noted that with increased testtemperature
22、 comes the possibility of changing the corrosionrate determining mechanism and the types of phases formedupon alteration from those that occur in the disposal environ-ment (Vienna et al, 2001 (4).5.2 The vapor hydration test can be used as a screening testto determine the propensity of waste forms t
23、o alter and forrelative comparisons in alteration rates between waste forms.6. Apparatus6.1 Test VesselsStainless steel vessels with closure fittingwith unique identifiers (on both vessel and lid), (for example,22 mL vessels, rated for service at temperatures up to 300Cand maximum pressure 11.7 MPa
24、(1700 psi).56.2 Balance(s)Any calibrated two-point (0.00 grams) bal-ance.6.3 Convection OvenConstant temperature convectionoven with the ability to control the temperature within 62C.6.4 Temperature Monitoring DeviceResistance thermom-eters or thermocouples, or both, with a strip chart recorder ora
25、data logger for periodic monitoring of the temperature of theconvection oven during the test duration. It is recommendedthat the maximum period between recorded temperature mea-surements be 0.5 h.6.5 PipettesCalibrated pipettes. Pipette tips that have beenpre-cleaned, sterilized, or individually pac
26、kaged to avoidcontamination from handling.6.6 Torque WrenchTorque wrench capable of torques upto 23.0 Nm (17.0 ftlb).6.7 Vessel HolderAppropriate device/stand for holdingvessels during tightening/loosening processes.6.8 Diamond Impregnated SawHigh or low densitydiamond-coated wafering blade and low
27、speed saw.6.9 Polishing EquipmentPolishing equipment capable ofpolishing to 600 grit (30 m).6.10 CalipersCalipers that have been calibrated withtraceable standards.6.11 Optical Microscope with Image Analysis System.6.12 Chemically Inert WireWire used to suspend thespecimens (such as 0.25 mm Pt wire)
28、.6.13 Support RodsTypically 1.5 mm diameter 304L stain-less steel (or comparable material) rods bent to the shapeshown in Fig. 2. Used to suspend specimens within thepressure vessel during tests.6.14 Non-Combustible TrayFor water to quench vesselbottom after test termination.6.15 Storage VesselsPoly
29、ethylene or glass vessels forspecimen storage.6.16 Ultrasonic Bath.6.17 pH Paper.6.18 SiC Paper.6.19 Non-Talc Surgical Gloves.6.20 Glass Slides.6.21 PTFE TapeThe type commonly used for householdplumbing.6.22 Tweezers/Forceps.5Series 4704 22 mL and 4714 45 mL “A” Socket Vessels from Parr InstrumentCo
30、., 211 53rd St., Moline, IL 61265, have been found satisfactory.C1663 1726.23 Scissors.6.24 Glue or Thermoplastic Adhesive, for attaching samplesand specimen to glass slides (for example, crystal-bond,super-glue, or wax).6.25 pH Probe, calibrated with traceable standards.7. Reagents and Standards7.1
31、 ASTM Type I WaterType I water shall have a minimalelectrical resistivity of 18.0 Mcm at 25C (see SpecificationD1193).7.2 SolventsAbsolute ethanol and reagent grade acetone.7.3 Reagent Grade HNO36 M HNO3and 0.16 M HNO3.8. Hazards8.1 All appropriate precautions for operation of pressurizedequipment m
32、ust be taken. To ensure safe operation, the testvessels should be rated to withstand the vapor pressure of waterat the test temperature with an appropriate safety factor.9. Specimen Preparation9.1 Glass or glass ceramic specimens are prepared fromannealed bars (for example, anneal 2 hours at a tempe
33、ratureslightly above the glass transition temperature with subsequentslow cooling to room temperature inside the oven, care must betaken not to induce phase changes during annealing).Annealedbars are cut with a diamond impregnated saw and SiC paperswith different grits.6During the specimen preparati
34、on, it isimportant to use low cutting force and saw speed (dependenton sample). Rough surface and damaged edges of the samplesindicate rough machining. This may cause cracks to formwithin the glass or glass ceramic specimen during the samplepreparation and decrease the reproducibility of the test. P
35、repa-ration of the specimen may vary according to the equipmentused. Usually specimens are prepared slightly larger andsubsequently polished to the desired dimensions. However,with certain types of diamond impregnated saws, it is possibleto prepare specimens with the desired dimensions and polishthe
36、 surface directly with 600 grit SiC paper. The details of oneexample of preparation technique are given below. These steps(9.1.1 9.1.4) are only given as an example and can beadjusted to yield the desired specimen dimensions and surfacefinish.9.1.1 Cut annealed glass or glass ceramic bars with adiam
37、ond-impregnated saw to roughly the dimensions 10.3 by10.3 by 1.6 mm (with appropriate cooling fluid). For certainsamples, such as glass ceramic materials, water should beavoided in order to not dissolve the soluble phase.9.1.2 Polish to roughly the dimensions 10.2 by 10.2 by 1.55mm using 240 grit Si
38、C (with appropriate cooling fluid).9.1.3 Polish to roughly the dimensions 10.1 by 10.1 by 1.51mm using 400 grit SiC (with appropriate cooling fluid).9.1.4 Polish to the dimensions 10.0 by 10.0 by 1.50 mmusing 600 grit SiC paper (with appropriate cooling fluid).9.2 Ultrasonically clean specimen in et
39、hanol for 2 min,decant, and discard ethanol.9.3 Ultrasonically clean specimen in ethanol for 4 min,decant, and discard ethanol.9.4 Dry specimen in an oven at 90C for 15 min.9.5 Examine each specimen with OM and record observa-tions concerning specimen surface and heterogeneity (streaks,inclusions, a
40、nd scratches).10. Test Vessel Cleaning10.1 Cleaning of Stainless Steel Vessels and Support Rods:10.1.1 Degrease vessels and lids with acetone. (This step isperformed only with new vessels.)10.1.2 Use 400 grit SiC paper to remove debris and oxida-tion from inside parts of previously used vessels and
41、rinse withDIW.10.1.3 Ultrasonically clean vessels, lids, and stainless steelsupports in ethanol for 5 min, decant and discard ethanol.10.1.4 Rinse vessels, lids, and supports by immersing 3times in fresh DIW.10.1.5 Soak vessels, lids, and supports in reagent grade 0.16M HNO3at 90C for 1 h.10.1.6 Rin
42、se vessels, lids, and supports by immersing 3times in fresh DIW.10.1.7 Soak vessels, lids, and supports in fresh DIW at 90Cfor1h.10.1.8 Rinse vessels, lids, and supports by immersing infresh DIW.10.1.9 Fill vessels (with supports placed inside) to 8090 %of capacity with fresh DIW. Place lids on vess
43、els. Do nottighten. Place them in an oven at 90C for a minimum of 16 h.10.1.10 After cooling, measure the pH of the DIW using thepH probe according to Test Methods D1293. If the pH value isnot within the 5.0 to 7.0 range, repeat rinsing from step 10.1.6.10.1.11 Dry vessels, lids, and supports in an
44、oven at 90Cfor at least 1 h.10.1.12 Store vessels, lids, and supports in a clean, dry,environment until use.10.2 Cleaning of PTFE Gaskets:NOTE 1Other gasket materials may be used, so long as they do notsignificantly impact the reactions between water and the sample. This maybe an important considera
45、tion in high radiation environments.10.2.1 Bake PTFE gaskets for 1 week at 200C. (This stepis performed only with new PTFE gaskets.)10.2.2 Soak the gaskets in reagent grade6MHNO3at50 6 5C for 4 h.10.2.3 Rinse the gaskets by immersing in fresh DIW 3times.10.2.4 Immerse the gaskets in fresh DIW and bo
46、il for 30min.10.2.5 Rinse by immersing the gaskets in fresh DIW.10.2.6 Soak the gaskets for8hinfresh DIW at 80C.10.2.7 Rinse the gaskets by immersing in fresh DIW.10.2.8 Immerse the gaskets in fresh DIW and boil for 30min.10.2.9 Rinse the gaskets by immersing 3 times in fresh DIW(container with gask
47、ets is filled 3 times with fresh DIW).6For detailed discussion of the influence of surface finish on corrosion seeMendel et al, 1984 (5). Some example results of vapor hydration tests with varyingsurface finish are reported in Jiricka et al, 2001 (6).C1663 17310.2.10 Submerge gaskets in fresh DIW. M
48、easure pH usingthe pH probe according to Test Methods D1293. If the pHvalue is not within the 5.0 to 7.0 range, repeat step 10.2.9.10.2.11 Dry gaskets in an oven at 90C and store in a cleanenvironment until needed.11. Calibration11.1 CalibrationsInitially calibrate all measurement in-struments used
49、in this test. Verify the calibrations during use ofthe instrument to indicate possible errors due to instrumentaldrift.11.2 Calibration and Standardization Schedule:11.2.1 Temperature Measurement DevicesCalibrate atleast annually with traceable standards or an ice/boiling waterbath.11.2.2 BalanceStandardize with traceable standardmasses on a regular basis. If a deviation in mass measurementis identified, all measurements since the last accurate standardmeasurement made with the balance must be marked
