1、Designation: C1663 09C1663 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
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 safety, hea
6、lth, and healthenvironmental practices and determine theapplicability of regulatory 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 Inter
7、national Standards, 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 Cond
8、uctivity and 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
9、refer to Terminologies C162 and C859 for additional terminology which may not be listed below.3.2 Definitions:3.1.1 alteration layera layer of alteration products at the surface of specimen. Several distinct layers may form at the surfaceand within cracks in the glass. Layers may be comprised of dis
10、crete crystallites. The thickness of these layers may be used toestimate the amount of glass altered.3.1.2 alteration productscrystalline or amorphous phases formed as a result of glass interaction with an aqueous environmentby precipitation from solution or by in situ transformation of the chemical
11、ly altered solid.1 This test method is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.13 on Spent Fuel andHigh Level Waste.Current edition approved June 1, 2009Nov. 1, 2017. Published July 2009December 2017. Originally approved
12、 in 2009. Last previous edition approved in 2009 asC1663 09. DOI: 10.1520/C1663-09.10.1520/C1663-17.2 The precision 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
13、unknown.3 The boldface numbers in parentheses refer to the list of references at the end of this standard.4 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 standar
14、ds Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide 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,
15、 ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the 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 States13.1
16、3 glassan inorganic product of fusion that has cooled to a rigid condition without crystallizing. C1623.1.4 glass ceramicsolid material, partly crystalline and partly glassy, formed by the controlled crystallization of a glass. C1623.1.5 glass transition temperatureon heating, the temperature at wh
17、ich a glass transforms from an elastic to a viscoelasticmaterial, characterized by the onset of a rapid change in thermal expansivity. C1623.2.1 immobilized low-activity wastevitrified low-activity fraction of waste presently contained in Hanford Site tanks.3.2.2 performance assessmentexamines the l
18、ong-term environmental and human health effects 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.3.2.5 traceable standarda material that supplies a link to known
19、test response in standards international units 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 sys
20、tem3.3.5 PTFEpolytetrafluoroethylene (chemical 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
21、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 ceramic specimens (referred to generally as glass samples in this test method)are suspended from a support rod ins
22、ide the test vessel with platinum wire. A volume 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 re
23、moved from the oven and the bottom of the vesselis 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. Signifi
24、cance and Use5.1 The vapor hydration test can 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
25、accelerate thermally activated processes. A wide 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 corrosi
26、on rate determining mechanism and the types ofphases 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 altera
27、tion rates between waste forms.6. Apparatus6.1 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 tw
28、o-point (0.00 grams) balance.5 Series 4701-144704 22 mL and 4714 45 mL “A” Socket Vessels from Parr Instrument Co., 211 53rd St., Moline, IL 61265, have been found satisfactory.C1663 1726.3 Convection OvenConstant temperature convection oven with the ability to control the temperature within 62C.6.4
29、 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 test duration. It is recommended that themaximum period between recorded temperature measurements
30、be 0.5 h.6.5 PipettesCalibrated pipettes. Pipette tips that have been precleaned,pre-cleaned, sterilized, or individually packaged toavoid contamination from handling.6.6 Torque WrenchTorque wrench capable of torques up to 23023.0 Nm (170 lbfft).(17.0 ftlb).6.7 Vessel HolderAppropriate device/stand
31、for holding vessels during tightening/loosening processes.6.8 Diamond Impregnated SawHigh or low density diamond-coated wafering blade and low speed saw.6.9 Polishing EquipmentPolishing equipment capable of polishing to 600 grit.grit (30 m).6.10 CalipersCalipers that have been calibrated with tracea
32、ble standards.6.11 Optical Microscope with Image Analysis System.6.12 Chemically Inert 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 spec
33、imens within the pressure vessel during tests.6.14 Non-Combustible TrayFor water to 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.6.2
34、1 PTFE TapeThe type commonly used for household plumbing.6.22 Tweezers/Forceps.6.23 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 Stand
35、ards7.1 ASTM Type I WaterType I water shall have a minimal electrical resistivity of 18.0 Mcm at 25C (see SpecificationD1193).7.2 SolventsAbsolute ethanol and reagent grade acetone.7.3 Reagent Grade HNO36 M HNO3 and 0.16M 0.16 M HNO3.8. Hazards8.1 All appropriate precautions for operation of pressur
36、ized equipment must be taken. To ensure safe operation, the test vesselsshould be rated to 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
37、2 hours at a temperature slightlyabove the glass transition temperature with subsequent slow cooling to room temperature inside the oven, care must be taken notto induce phase changes during annealing) using annealing). Annealed bars are cut with a diamond impregnated saw and SiCpapers with differen
38、t grits.6 During the specimen preparation, it is important to use low cutting force and saw speed (dependenton sample). Rough surface and damaged edges of the samples indicate rough machining. This may cause cracks to form withinthe glass or glass ceramic specimen during the sample preparation and d
39、ecrease the reproducibility of the test. Preparation of thespecimen may vary according to the equipment used. Usually specimens are prepared slightly larger and subsequently polished6 For detailed discussion of the influence of surface finish on corrosion see Mendel et al, 1984 (5). Some example res
40、ults of vapor hydration tests with varying surfacefinish are reported in Jiricka et al, 2001 (6).C1663 173to the desired dimensions. However, with certain types of diamond impregnated saws, it is possible to prepare specimens with thedesired dimensions and polish the surface directly with 600 grit S
41、iC paper. The details of one example of preparation techniqueare given below. These steps (9.1.1 9.1.49.1.5) are only given as an example and can be adjusted to yield the desired specimendimensions and surface finish.9.1.1 Cut annealed glass or glass ceramic bars with a diamond-impregnated saw to ro
42、ughly the dimensions 10.3 by 10.3 by30501.6 mm (with appropriate cooling fluid). For certain samples, such as glass ceramic materials, water should be avoided inorder to not dissolve the soluble phase.9.1.2 Slice from the square glass or glass ceramic bar using a diamond impregnated saw a roughly 1.
43、6 mm-thick specimen (10.3by 10.3 by 1.6 mm) (with appropriate cooling fluid).9.1.2 Polish to roughly the dimensions 10.2 by 10.2 by 1.55 mm using 240 grit SiC (with appropriate cooling fluid).9.1.3 Polish to roughly the dimensions 10.1 by 10.1 by 1.51 mm using 400 grit SiC (with appropriate cooling
44、fluid).9.1.4 Polish to the dimensions 10.0 by 10.0 by 1.50 mm using 600 grit SiC paper (with appropriate cooling 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 spec
45、imen 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 vessels and lids with aceton
46、e. (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, decant and discard ethanol.10.1
47、4 Rinse vessels, lids, and supports by immersing 3 times in fresh DIW.10.1.5 Soak vessels, lids, and supports in reagent grade 0.16M 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 in fresh DIW at 90C for
48、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, measure the pH of the DIW usi
49、ng 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 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
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