1、Designation: C1663 17C1663 18Standard 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
2、, 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 The vapor hydration test method can be used to study the corrosion of a waste forms such as glasses and
3、glass ceramics2upon exposure to water vapor at elevated temperatures. In addition, the alteration phases that form can be used as indicators ofthose phases that may form under repository conditions. These tests; which allow altering of glass at high surface area to solutionvolume ratio; provide usef
4、ul information regarding the alteration phases that are formed, the disposition of radioactive andhazardous components, and the alteration kinetics under the specific test conditions. This information may be used in performanceassessment (McGrail et al, 2002 (1)3 for example).1.2 This test method mu
5、st be performed in accordance with all quality assurance requirements for acceptance of the data.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety, health, an
6、d environmental practices and determine the applicability ofregulatory limitations prior to use.1.4 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Stan
7、dards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers 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
8、Resistivity of WaterD1193 Specification for Reagent WaterD1293 Test Methods for pH of WaterE177 Practice for Use of the Terms Precision and Bias in ASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method3. Terminology3.1 Please refer to Term
9、inologies C162 and C859 for additional terminology which may not be listed below.3.2 Definitions:3.2.1 immobilized low-activity wastevitrified low-activity fraction of waste presently contained in Hanford Site tanks.3.2.2 performance assessmentexamines the long-term environmental and human health ef
10、fects associated with the planneddisposal 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 for testing.1 This test method is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and is the direct
11、responsibility of Subcommittee C26.13 on Spent Fuel andHigh Level Waste.Current edition approved Nov. 1, 2017Nov. 1, 2018. Published December 2017January 2019. Originally approved in 2009. Last previous edition approved in 20092017as C1663 09.C1663 17. DOI: 10.1520/C1663-17.10.1520/C1663-18.2 The pr
12、ecision and bias statements are only valid for glass waste forms at this time. The test may be (and has been) performed on other waste forms; however, the precisionof such tests are currently unknown.3 The boldface numbers in parentheses refer to the list of references at the end of this standard.4
13、For referencedASTM standards, visit theASTM website, 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 p
14、rovide the user of an ASTM standard an indication 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 t
15、he standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.2.5 traceable standarda material that supplies a link to known test response in standards international units
16、 by a nationalor international standards body, for example, NIST.3.3 Abbreviations:3.3.1 DIWASTM Type I deionized water3.3.2 EDSenergy dispersive X-ray spectroscopy3.3.3 OMoptical microscopy3.3.4 OM/IAoptical microscope connected to an image analysis system3.3.5 PTFEpolytetrafluoroethylene (chemical
17、 compound commonly 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 transition temperature3.3.11 VHTvapor hydration test3.3.12 WDSwave-length dispersive spectroscopy3.3.13 X
18、RDX-ray diffraction3.3.14 %RSDpercent relative standard deviation4. Summary of Test Method4.1 For the vapor hydration tests, glass or glass ceramic specimens (referred to generally as glass samples in this test method)are suspended from a support rod inside the test vessel with platinum wire. A volu
19、me of water determined by the volume of thetest vessel and the test temperature is added to the vessel. The vessel is then sealed and placed in an oven at the desired testtemperature and left undisturbed. After the desired test duration, the vessel is removed from the oven and the bottom of the vess
20、elis cooled to condense the vapor in the vessel. Specimens are removed and examined with optical microscopy, XRD, SEM, andother analytical methods. The remaining glass or glass ceramic thickness is measured and alteration phases are identified.5. Significance and Use5.1 The vapor hydration test can
21、be used to study the corrosion of glass and glass ceramic waste forms under conditions of hightemperature and contact by water vapor or thin films of water. This method may serve as an accelerated test for some materials,since the high temperatures will accelerate thermally activated processes. A wi
22、de range of test temperatures have been reportedin the literature 40C (Ebert et al, 2005 (3), for example) to 300C (Vienna et al, 2001 (4), for example). It should be noted thatwith increased test temperature comes the possibility of changing the corrosion rate determining mechanism and the types of
23、phases formed upon alteration from those that occur in the disposal environment (Vienna et al, 2001 (4).5.2 The vapor hydration test can be used as a screening test to determine the propensity of waste forms to alter and for relativecomparisons in alteration rates between waste forms.6. Apparatus6.1
24、 Test VesselsStainless steel vessels with closure fitting with unique identifiers (on both vessel and lid), (for example, 22mL vessels, rated for service at temperatures up to 300C and maximum pressure 11.7 MPa (1700 psi).56.2 Balance(s)Any calibrated two-point (0.00 grams) balance.6.3 Convection Ov
25、enConstant temperature convection oven with the ability to control the temperature within 62C.6.4 Temperature Monitoring DeviceResistance thermometers or thermocouples, or both, with a strip chart recorder or a datalogger for periodic monitoring of the temperature of the convection oven during the t
26、est duration. It is recommended that themaximum period between recorded temperature measurements be 0.5 h.6.5 PipettesCalibrated pipettes. Pipette tips that have been pre-cleaned, sterilized, or individually packaged to avoidcontamination from handling.6.6 Torque WrenchTorque wrench capable of torqu
27、es up to 23.0 Nm (17.0 ftlb).6.7 Vessel HolderAppropriate device/stand for holding vessels during tightening/loosening processes.6.8 Diamond Impregnated SawHigh or low density diamond-coated wafering blade and low speed saw.5 Series 4704 22 mL and 4714 45 mL “A” Socket Vessels from Parr Instrument C
28、o., 211 53rd St., Moline, IL 61265, have been found satisfactory.C1663 1826.9 Polishing EquipmentPolishing equipment capable of polishing to 600 grit (30 m).6.10 CalipersCalipers that have been calibrated with traceable standards.6.11 Optical Microscope with Image Analysis System.6.12 Chemically Ine
29、rt WireWire used to suspend the specimens (such as 0.25 mm Pt wire).6.13 Support RodsTypically 1.5 mm diameter 304L stainless steel (or comparable material) rods bent to the shape shown inFig. 2. Used to suspend specimens within the pressure vessel during tests.6.14 Non-Combustible TrayFor water to
30、quench vessel bottom after test termination.6.15 Storage VesselsPolyethylene or glass vessels for specimen 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 household plumbing.6.22 Tweezers/Forceps.6.23
31、Scissors.6.24 Glue or Thermoplastic Adhesive, for attaching samples and 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 minimal electrical resistivity of
32、 18.0 Mcm at 25C (see SpecificationD1193).7.2 SolventsAbsolute ethanol and reagent grade acetone.7.3 Reagent Grade HNO36 M HNO3 and 0.16 M HNO3.8. Hazards8.1 All appropriate precautions for operation of pressurized equipment must be taken. To ensure safe operation, the test vesselsshould be rated to
33、 withstand the vapor pressure of water at the test temperature with an appropriate safety factor.9. Specimen Preparation9.1 Glass or glass ceramic specimens are prepared from annealed bars (for example, anneal 2 hours at a temperature slightlyabove the glass transition temperature with subsequent sl
34、ow cooling to room temperature inside the oven, care must be taken notto induce phase changes during annealing). Annealed bars are cut with a diamond impregnated saw and SiC papers with differentgrits.6 During the specimen preparation, it is important to use low cutting force and saw speed (dependen
35、t on sample). Roughsurface and damaged edges of the samples indicate rough machining. This may cause cracks to form within the glass or glassceramic specimen during the sample preparation and decrease the reproducibility of the test. Preparation of the specimen may varyaccording to the equipment use
36、d. Usually specimens are prepared slightly larger and subsequently polished to the desireddimensions. However, with certain types of diamond impregnated saws, it is possible to prepare specimens with the desireddimensions and polish the surface directly with 600 grit SiC paper. The details of one ex
37、ample of preparation technique are givenbelow. These steps (9.1.1 9.1.4) are only given as an example and can be adjusted to yield the desired specimen dimensions andsurface finish.9.1.1 Cut annealed glass or glass ceramic bars with a diamond-impregnated saw to roughly the dimensions 10.3 by 10.3 by
38、 1.6mm (with appropriate cooling fluid). For certain samples, such as glass ceramic materials, water should be avoided in order to notdissolve the soluble phase.9.1.2 Polish to roughly the dimensions 10.2 by 10.2 by 1.55 mm using 240 grit (70 m) SiC (with appropriate cooling fluid).9.1.3 Polish to r
39、oughly the dimensions 10.1 by 10.1 by 1.51 mm using 400 grit (40 m) SiC (with appropriate cooling fluid).9.1.4 Polish to the dimensions 10.0 by 10.0 by 1.50 mm using 600 grit (30 m) SiC paper (with appropriate cooling fluid).6 For detailed discussion of the influence of surface finish on corrosion s
40、ee Mendel et al, 1984 (5). Some example results of vapor hydration tests with varying surfacefinish are reported in Jiricka et al, 2001 (6).C1663 1839.2 Ultrasonically clean specimen in ethanol for 2 min, decant, and discard ethanol.9.3 Ultrasonically clean specimen in ethanol for 4 min, decant, and
41、 discard ethanol.9.4 Dry specimen in an oven at 90C for 15 min.9.5 Examine each specimen with OM and record observations concerning specimen surface and heterogeneity (streaks,inclusions, and scratches).10. Test Vessel Cleaning10.1 Cleaning of Stainless Steel Vessels and Support Rods:10.1.1 Degrease
42、 vessels and lids with acetone. (This step is performed only with new vessels.)10.1.2 Use 400 grit SiC paper to remove debris and oxidation from inside parts of previously used vessels and rinse with DIW.10.1.3 Ultrasonically clean vessels, lids, and stainless steel supports in ethanol for 5 min, de
43、cant and discard ethanol.10.1.4 Rinse vessels, lids, and supports by immersing 3 times in fresh DIW.10.1.5 Soak vessels, lids, and supports in reagent grade 0.16 M HNO3 at 90C for 1 h.10.1.6 Rinse vessels, lids, and supports by immersing 3 times in fresh DIW.10.1.7 Soak vessels, lids, and supports i
44、n fresh DIW at 90C for 1 h.10.1.8 Rinse vessels, lids, and supports by immersing in fresh DIW.10.1.9 Fill vessels (with supports placed inside) to 8090 % of capacity with fresh DIW. Place lids on vessels. Do not tighten.Place them in an oven at 90C for a minimum of 16 h.10.1.10 After cooling, measur
45、e the pH of the DIW using the pH 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 oven at 90C for at least 1 h.10.1.12 Store vessels, lids, and supports in a clean, dry, environment
46、 until use.10.2 Cleaning of PTFE Gaskets:NOTE 1Other gasket materials may be used, so long as they do not significantly impact the reactions between water and the sample. This may bean important consideration in high radiation environments.10.2.1 Bake PTFE gaskets for 1 week at 200C. (This step is p
47、erformed only with new PTFE gaskets.)10.2.2 Soak the gaskets in reagent grade 6 M HNO3 at 50 6 5C for 4 h.10.2.3 Rinse the gaskets by immersing in fresh DIW 3 times.10.2.4 Immerse the gaskets in fresh DIW and boil for 30 min.10.2.5 Rinse by immersing the gaskets in fresh DIW.10.2.6 Soak the gaskets
48、for 8 h in fresh 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 30 min.10.2.9 Rinse the gaskets by immersing 3 times in fresh DIW (container with gaskets is filled 3 times with fresh DIW).10.2.10 Submerge gaskets in fresh DIW. Measu
49、re pH using the pH probe according to Test Methods D1293. If the pH valueis 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 clean environment until needed.11. Calibration11.1 CalibrationsInitially calibrate all measurement instruments used in this test. Verify the calibrations during use of theinstrument to indicate possible errors due to instrumental drift.11.2 Calibration and Standardization Schedule:11.2.1 Temperature Measurement DevicesCalibrate at l
