1、Designation: C 1663 09Standard Test Method forMeasuring Waste Glass or Glass Ceramic Durability byVapor Hydration Test1This standard is issued under the fixed designation C 1663; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the
2、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 The vapor hydration test method can be used to studythe corrosion of a waste forms such as glasses and glassce
3、ramics2upon 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 infor
4、ma-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 perf
5、ormed 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 and health practices a
6、nd determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:4C 162 Terminology of Glass and Glass ProductsD 1125 Test Methods for Electrical Conductivity and Re-sistivity of WaterD 1193 Specification for Reagent WaterD 1293 Test Methods for pH of
7、WaterE 177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 Definitions:3.1.1 alteration layera layer of alteration products at thesurface of specimen. Several distin
8、ct layers may form at thesurface and within cracks in the glass. Layers may be com-prised of discrete crystallites. The thickness of these layers maybe used to estimate the amount of glass altered.3.1.2 alteration productscrystalline or amorphous phasesformed as a result of glass interaction with an
9、 aqueousenvironment by precipitation from solution or by in situtransformation of the chemically altered solid.3.1.3 glassan inorganic product of fusion that has cooledto a rigid condition without crystallizing. C 1623.1.4 glass ceramicsolid material, partly crystalline andpartly glassy, formed by t
10、he controlled crystallization of aglass. C 1623.1.5 glass transition temperatureon heating, the tem-perature at which a glass transforms from an elastic to aviscoelastic material, characterized by the onset of a rapidchange in thermal expansivity. C 1623.1.6 immobilized low-activity wastevitrified l
11、ow-activityfraction of waste presently contained in Hanford Site tanks.3.1.7 performance assessmentexamines the long-term en-vironmental and human health effects associated with theplanned disposal of waste. Mann et al, 2001 (2)3.1.8 sampleinitial test material with known composition.3.1.9 specimens
12、pecimen is a part of the sample used fortesting.3.1.10 traceable standarda material that supplies a link toknown test response in standards international units by anational or international standards body, for example, NIST.3.2 Abbreviations:3.2.1 DIWASTM Type I deionized water3.2.2 EDSenergy disper
13、sive X-ray spectroscopy3.2.3 OMoptical microscopy3.2.4 OM/IAoptical microscope connected to an imageanalysis system3.2.5 PTFEpolytetrafluoroethylene (chemical compoundcommonly referred to as Teflon)3.2.6 SEMscanning electron microscope1This test method is under the jurisdiction of ASTM Committee C26
14、 on NuclearFuel Cycle and is the direct responsibility of Subcommittee C26.13 on Spent Fueland High Level Waste.Current edition approved June 1, 2009. Published July 2009.2The precision and bias statements are only valid for glass waste forms at thistime. The test may be (and has been) performed on
15、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 Service at serviceastm.org. For A
16、nnual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.2.7 SiC papersilicon-carbide paper3.2.8 TBDto be determined3.2.9 TEMtra
17、nsmission electron microscope3.2.10 Tgglass transition temperature3.2.11 VHTvapor hydration test3.2.12 WDSwave-length dispersive spectroscopy3.2.13 XRDX-ray diffraction3.2.14 %RSDpercent relative standard deviation4. Summary of Test Method4.1 For the vapor hydration tests, glass or glass ceramicspec
18、imens (referred to generally as glass samples 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 at
19、the desired test temperature and left undisturbed. 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. Theremai
20、ning glass or glass ceramic thickness is measured 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. Thi
21、s method may serve as an acceleratedtest for 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
22、 be noted that with increased testtemperature 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 tes
23、tto determine the propensity of waste forms to 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 temperat
24、ures up to 300Cand maximum pressure 11.7 MPa (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 thermocoupl
25、es, or both, with a strip chart recorder ora 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 havebeen
26、 precleaned, sterilized, or individually packaged to avoidcontamination from handling.6.6 Torque WrenchTorque wrench capable of torques upto 230 Nm (170 lbfft).6.7 Vessel HolderAppropriate device/stand for holdingvessels during tightening/loosening processes.6.8 Diamond Impregnated SawHigh or low de
27、nsitydiamond-coated wafering blade and low speed saw.6.9 Polishing EquipmentPolishing equipment capable ofpolishing to 600 grit.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 th
28、especimens (such as 0.25 mm Pt wire).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
29、termination.6.15 Storage VesselsPolyethylene 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.6.23 Scissors.6.24 Glue or Thermoplasti
30、c 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 ASTM Type I WaterType I water shall have a minimalelectrical resistivity of 18.0 MVcm at 25C (see Specification
31、D 1193).7.2 SolventsAbsolute ethanol and reagent grade acetone.7.3 Reagent Grade HNO36 M HNO3and 0.16M HNO3.8. Hazards8.1 All appropriate precautions for operation of pressurizedequipment must be taken. To ensure safe operation, the testvessels should be rated to withstand the vapor pressure of wate
32、rat 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 temperatureslightly above the glass transition temperature with subsequent5Series 4701-14 22 mL Vessels from Parr In
33、strument Co., 211 53rd St., Moline,IL 61265, have been found satisfactory.C1663092slow cooling to room temperature inside the oven, care must betaken not to induce phase changes during annealing) using adiamond impregnated saw and SiC papers with different grits.6During the specimen preparation, it
34、is important to use lowcutting force and saw speed (dependent on sample). Roughsurface and damaged edges of the samples indicate roughmachining. This may cause cracks to form within the glass orglass ceramic specimen during the sample preparation anddecrease the reproducibility of the test. Preparat
35、ion of thespecimen may vary according to the equipment used. Usuallyspecimens are prepared slightly larger and subsequently pol-ished to the desired dimensions. However, with certain types ofdiamond impregnated saws, it is possible to prepare specimenswith the desired dimensions and polish the surfa
36、ce directlywith 600 grit SiC paper. The details of one example ofpreparation technique are given below. These steps (9.1.1-9.1.5) are only given as an example and can be adjusted toyield the desired specimen dimensions and surface finish.9.1.1 Cut annealed glass or glass ceramic bars with adiamond-i
37、mpregnated saw to roughly the dimensions 10.3 by10.3 by 3050 mm (with appropriate cooling fluid).9.1.2 Slice from the square glass or glass ceramic bar usinga diamond impregnated saw a roughly 1.6 mm-thick specimen(10.3 by 10.3 by 1.6 mm) (with appropriate cooling fluid).9.1.3 Polish to roughly the
38、dimensions 10.2 by 10.2 by 1.55mm using 240 grit SiC (with appropriate cooling fluid).9.1.4 Polish to roughly the dimensions 10.1 by 10.1 by 1.51mm using 400 grit SiC (with appropriate cooling fluid).9.1.5 Polish to the dimensions 10.0 by 10.0 by 1.50 mmusing 600 grit SiC paper (with appropriate coo
39、ling fluid).9.2 Ultrasonically clean specimen in ethanol 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 specim
40、en surface and heterogeneity (streaks,inclusions, and 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-tio
41、n from inside parts of previously used vessels and 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 i
42、n reagent grade0.16M HNO3at 90C for 1 h.10.1.6 Rinse 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 80
43、90 %of capacity with fresh DIW. Place lids on vessels. 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 D 1293. If the pH value isnot within the 5.0 to 7.0 range, repeat rinsing from step 10
44、.1.6.10.1.11 Dry vessels, lids, and supports in an 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 wate
45、r and the sample. This maybe an important consideration 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 3t
46、imes.10.2.4 Immerse the gaskets in fresh DIW and boil 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
47、 immersing 3 times in fresh DIW(container with gaskets is filled 3 times with fresh DIW).10.2.10 Submerge gaskets in fresh DIW. Measure pH usingthe pH probe according to Test Methods D 1293. 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 a
48、nd store in a cleanenvironment until needed.11. Calibration11.1 CalibrationsInitially calibrate all measurement in-struments used 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.
49、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 appro-priately. Have balance calibrated on an annual basis.11.2.3 Water Purification SystemCalibrate at least annu-ally following the manufacturers instructions. Standardizewith the 10 M
