ASTM C1663-09
(Test Method)Standard Test Method for Measuring Waste Glass or Glass Ceramic Durability by Vapor Hydration Test
Standard Test Method for Measuring Waste Glass or Glass Ceramic Durability by Vapor Hydration Test
SIGNIFICANCE AND USE
The vapor hydration test can be used to study the corrosion of glass and glass ceramic waste forms under conditions of high temperature 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 wide range of test temperatures have been reported in the literature –40°C (Ebert et al, 2005 (3), for example) to 300°C (Vienna et al, 2001 (4), for example). It should be noted that with increased test temperature comes the possibility of changing the corrosion rate determining mechanism and the types of phases formed upon alteration from those that occur in the disposal environment (Vienna et al, 2001 (4)).
The vapor hydration test can be used as a screening test to determine the propensity of waste forms to alter and for relative comparisons in alteration rates between waste forms.
SCOPE
1.1 The vapor hydration test method can be used to study the corrosion of a waste forms such as glasses and glass ceramics upon exposure to water vapor at elevated temperatures. In addition, the alteration phases that form can be used as indicators of those phases that may form under repository conditions. These tests; which allow altering of glass at high surface area to solution volume ratio; provide useful information regarding the alteration phases that are formed, the disposition of radioactive and hazardous components, and the alteration kinetics under the specific test conditions. This information may be used in performance assessment (McGrail et al, 2002 (1) for example).
1.2 This test method must 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 responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: C1663 − 09
Standard Test Method for
Measuring Waste Glass or Glass Ceramic Durability by
Vapor Hydration Test
This standard is issued under the fixed designation C1663; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope ASTM Test Methods
E691 Practice for Conducting an Interlaboratory Study to
1.1 The vapor hydration test method can be used to study
Determine the Precision of a Test Method
the corrosion of a waste forms such as glasses and glass
ceramics upon exposure to water vapor at elevated tempera-
3. Terminology
tures.Inaddition,thealterationphasesthatformcanbeusedas
indicators of those phases that may form under repository
3.1 Definitions:
conditions. These tests; which allow altering of glass at high
3.1.1 alteration layer—a layer of alteration products at the
surface area to solution volume ratio; provide useful informa-
surface of specimen. Several distinct layers may form at the
tion regarding the alteration phases that are formed, the surface and within cracks in the glass. Layers may be com-
disposition of radioactive and hazardous components, and the
prisedofdiscretecrystallites.Thethicknessoftheselayersmay
alteration kinetics under the specific test conditions. This be used to estimate the amount of glass altered.
information may be used in performance assessment (McGrail
3.1.2 alteration products—crystalline or amorphous phases
et al, 2002 (1) for example).
formed as a result of glass interaction with an aqueous
1.2 This test method must be performed in accordance with environment by precipitation from solution or by in situ
all quality assurance requirements for acceptance of the data. transformation of the chemically altered solid.
1.3 This standard does not purport to address all of the 3.1.3 glass—an inorganic product of fusion that has cooled
safety concerns, if any, associated with its use. It is the to a rigid condition without crystallizing. C162
responsibility of the user of this standard to establish appro-
3.1.4 glass ceramic—solid material, partly crystalline and
priate safety and health practices and determine the applica-
partly glassy, formed by the controlled crystallization of a
bility of regulatory limitations prior to use.
glass. C162
3.1.5 glasstransitiontemperature—onheating,thetempera-
2. Referenced Documents
tureatwhichaglasstransformsfromanelastictoaviscoelastic
2.1 ASTM Standards:
material, characterized by the onset of a rapid change in
C162 Terminology of Glass and Glass Products
thermal expansivity. C162
D1125 Test Methods for Electrical Conductivity and Resis-
3.1.6 immobilized low-activity waste—vitrified low-activity
tivity of Water
fraction of waste presently contained in Hanford Site tanks.
D1193 Specification for Reagent Water
D1293 Test Methods for pH of Water
3.1.7 performance assessment—examines the long-term en-
E177 Practice for Use of the Terms Precision and Bias in vironmental and human health effects associated with the
planned disposal of waste. Mann et al, 2001 (2)
3.1.8 sample—initial test material with known composition.
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.13 on Spent Fuel
3.1.9 specimen—specimen is a part of the sample used for
and High Level Waste.
testing.
Current edition approved June 1, 2009. Published July 2009. DOI: 10.1520/
C1663-09.
3.1.10 traceable standard—a material that supplies a link to
The precision and bias statements are only valid for glass waste forms at this
known test response in standards international units by a
time. The test may be (and has been) performed on other waste forms; however, the
national or international standards body, for example, NIST.
precision of such tests are currently unknown.
The boldface numbers in parentheses refer to the list of references at the end of
3.2 Abbreviations:
this standard.
4 3.2.1 DIW—ASTM Type I deionized water
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3.2.2 EDS—energy dispersive X-ray spectroscopy
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 3.2.3 OM—optical microscopy
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1663 − 09
3.2.4 OM/IA—optical microscope connected to an image 6.2 Balance(s)—Any calibrated two-point (0.00 grams) bal-
analysis system ance.
3.2.5 PTFE—polytetrafluoroethylene (chemical compound
6.3 Convection Oven—Constant temperature convection
commonly referred to as Teflon)
oven with the ability to control the temperature within 62°C.
3.2.6 SEM—scanning electron microscope
6.4 Temperature Monitoring Device—Resistance thermom-
3.2.7 SiC paper—silicon-carbide paper
eters or thermocouples, or both, with a strip chart recorder or
3.2.8 TBD—to be determined a data logger for periodic monitoring of the temperature of the
convection oven during the test duration. It is recommended
3.2.9 TEM—transmission electron microscope
that the maximum period between recorded temperature mea-
3.2.10 T —glass transition temperature
g
surements be 0.5 h.
3.2.11 VHT—vapor hydration test
6.5 Pipettes—Calibratedpipettes.Pipettetipsthathavebeen
3.2.12 WDS—wave-length dispersive spectroscopy
precleaned, sterilized, or individually packaged to avoid con-
3.2.13 XRD—X-ray diffraction
tamination from handling.
3.2.14 %RSD—percent relative standard deviation
6.6 Torque Wrench—Torque wrench capable of torques up
to 230 N·m (170 lbf·ft).
4. Summary of Test Method
6.7 Vessel Holder—Appropriate device/stand for holding
4.1 For the vapor hydration tests, glass or glass ceramic
vessels during tightening/loosening processes.
specimens (referred to generally as glass samples in this test
method)aresuspendedfromasupportrodinsidethetestvessel
6.8 Diamond Impregnated Saw—High or low density
with platinum wire. A volume of water determined by the
diamond-coated wafering blade and low speed saw.
volume of the test vessel and the test temperature is added to
6.9 Polishing Equipment—Polishing equipment capable of
the vessel. The vessel is then sealed and placed in an oven at
polishing to 600 grit.
the desired test temperature and left undisturbed. After the
desired test duration, the vessel is removed from the oven and
6.10 Calipers—Calipers that have been calibrated with
the bottom of the vessel is cooled to condense the vapor in the
traceable standards.
vessel. Specimens are removed and examined with optical
6.11 Optical Microscope with Image Analysis System.
microscopy, XRD, SEM, and other analytical methods. The
remaining glass or glass ceramic thickness is measured and
6.12 Chemically Inert Wire—Wire used to suspend the
alteration phases are identified.
specimens (such as 0.25 mm Pt wire).
5. Significance and Use
6.13 Support Rods—Typically 1.5 mm diameter 304Lstain-
less steel (or comparable material) rods bent to the shape
5.1 The vapor hydration test can be used to study the
shown in Fig. 2. Used to suspend specimens within the
corrosion of glass and glass ceramic waste forms under
pressure vessel during tests.
conditions of high temperature and contact by water vapor or
thin films of water. This method may serve as an accelerated
6.14 Non-Combustible Tray—For water to quench vessel
test for some materials, since the high temperatures will
bottom after test termination.
accelerate thermally activated processes. A wide range of test
6.15 Storage Vessels—Polyethylene or glass vessels for
temperatures have been reported in the literature –40°C (Ebert
specimen storage.
et al, 2005 (3), for example) to 300°C (Vienna et al, 2001 (4),
for example). It should be noted that with increased test
6.16 Ultrasonic Bath.
temperature comes the possibility of changing the corrosion
6.17 pH Paper.
rate determining mechanism and the types of phases formed
upon alteration from those that occur in the disposal environ-
6.18 SiC Paper.
ment (Vienna et al, 2001 (4)).
6.19 Non-Talc Surgical Gloves.
5.2 The vapor hydration test can be used as a screening test
6.20 Glass Slides.
to determine the propensity of waste forms to alter and for
relative comparisons in alteration rates between waste forms.
6.21 PTFE Tape—The type commonly used for household
plumbing.
6. Apparatus
6.22 Tweezers/Forceps.
6.1 Test Vessels—Stainless steel vessels with closure fitting
with unique identifiers (on both vessel and lid), (for example,
6.23 Scissors.
22 mL vessels, rated for service at temperatures up to 300°C
6.24 Glue or Thermoplastic Adhesive, for attaching samples
and maximum pressure 11.7 MPa (1700 psi)).
and specimen to glass slides (for example, crystal-bond,
super-glue, or wax).
Series 4701-14 22 mLVessels from Parr Instrument Co., 211 53rd St., Moline,
IL 61265, have been found satisfactory. 6.25 pH Probe, calibrated with traceable standards.
C1663 − 09
7. Reagents and Standards 9.5 Examine each specimen with OM and record observa-
tions concerning specimen surface and heterogeneity (streaks,
7.1 ASTM Type I Water—Type I water shall have a minimal
inclusions, and scratches).
electrical resistivity of 18.0 MΩ·cm at 25°C (see Specification
D1193).
10. Test Vessel Cleaning
7.2 Solvents—Absolute ethanol and reagent grade acetone.
10.1 Cleaning of Stainless Steel Vessels and Support Rods:
7.3 Reagent Grade HNO —6 M HNO and 0.16M HNO .
3 3 3
10.1.1 Degrease vessels and lids with acetone. (This step is
performed only with new vessels.)
8. Hazards
10.1.2 Use 400 grit SiC paper to remove debris and oxida-
8.1 All appropriate precautions for operation of pressurized
tion from inside parts of previously used vessels and rinse with
equipment must be taken. To ensure safe operation, the test
DIW.
vesselsshouldberatedtowithstandthevaporpressureofwater
10.1.3 Ultrasonically clean vessels, lids, and stainless steel
at the test temperature with an appropriate safety factor.
supports in ethanol for 5 min, decant and discard ethanol.
10.1.4 Rinse vessels, lids, and supports by immersing 3
9. Specimen Preparation
times in fresh DIW.
9.1 Glass or glass ceramic specimens are prepared from
10.1.5 Soak vessels, lids, and supports in reagent grade
annealed bars (for example, anneal 2 hours at a temperature
0.16M HNO at 90°C for 1 h.
slightly above the glass transition temperature with subsequent
10.1.6 Rinse vessels, lids, and supports by immersing 3
slowcoolingtoroomtemperatureinsidetheoven,caremustbe
times in fresh DIW.
taken not to induce phase changes during annealing) using a
10.1.7 Soakvessels,lids,andsupportsinfreshDIWat90°C
diamond impregnated saw and SiC papers with different grits.
for1h.
During the specimen preparation, it is important to use low
10.1.8 Rinse vessels, lids, and supports by immersing in
cutting force and saw speed (dependent on sample). Rough
fresh DIW.
surface and damaged edges of the samples indicate rough
10.1.9 Fill vessels (with supports placed inside) to 80–90 %
machining. This may cause cracks to form within the glass or
of capacity with fresh DIW. Place lids on vessels. Do not
glass ceramic specimen during the sample preparation and
tighten. Place them in an oven at 90°C for a minimum of 16 h.
decrease the reproducibility of the test. Preparation of the
10.1.10 After cooling, measure the pH of the DIWusing the
specimen may vary according to the equipment used. Usually
pH probe according to Test Methods D1293. If the pH value is
specimens are prepared slightly larger and subsequently pol-
not within the 5.0 to 7.0 range, repeat rinsing from step 10.1.6.
ishedtothedesireddimensions.However,withcertaintypesof
10.1.11 Dry vessels, lids, and supports in an oven at 90°C
diamond impregnated saws, it is possible to prepare specimens
for at least 1 h.
with the desired dimensions and polish the surface directly
10.1.12 Store vessels, lids, and supports in a clean, dry,
with 600 grit SiC paper. The details of one example of
environment until use.
preparation technique are given below. These steps (9.1.1 –
10.2 Cleaning of PTFE Gaskets:
9.1.5) are only given as an example and can be adjusted to
yield the desired specimen dimensions and surface finish.
NOTE 1—Other gasket materials may be used, so long as they do not
9.1.1 Cut annealed glass or glass ceramic bars with a significantlyimpactthereactionsbetweenwaterandthesample.Thismay
be an important consideration in high radiation environments.
diamond-impregnated saw to roughly the dimensions 10.3 by
10.3 by 30–50 mm (with appropriate cooling fluid).
10.2.1 Bake PTFE gaskets for 1 week at 200°C. (This step
9.1.2 Slice from the square glass or glass ceramic bar using
is performed only with new PTFE gaskets.)
a diamond impregnated saw a roughly 1.6 mm-thick specimen
10.2.2 Soak the gaskets in reagent grade6MHNO at
(10.3 by 10.3 by 1.6 mm) (with appropriate cooling fluid).
50 6 5°C for 4 h.
9.1.3 Polish to roughly the dimensions 10.2 by 10.2 by 1.55
10.2.3 Rinse the gaskets by immersing in fresh DIW 3
mm using 240 grit SiC (with appropriate cooling fluid).
times.
9.1.4 Polish to roughly the dimensions 10.1 by 10.1 by 1.51
10.2.4 Immerse the gaskets in fresh DIW and boil for 30
mm using 400 grit SiC (with appropriate cooling fluid).
min.
9.1.5 Polish to the dimensions 10.0 by 10.0 by 1.50 mm
10.2.5 Rinse by immersing the gaskets in fresh DIW.
using 600 grit SiC paper (with appropriate cooling fluid).
10.2.6 Soak the gaskets for8hin fresh DIW at 80°C.
10.2.7 Rinse the gaskets by immersing in fresh DIW.
9.2 Ultrasonically clean specimen in ethanol for 2 min,
decant, and discard ethanol. 10.2.8 Immerse the gaskets in fresh DIW and boil for 30
min.
9.3 Ultrasonically clean specimen in ethanol for 4 min,
10.2.9 Rinsethegasketsbyimmersing3timesinfreshDIW
decant, and discard ethanol.
(container with gaskets is filled 3 times with fresh DIW).
9.4 Dry specimen in an oven at 90°C for 15 min.
10.2.10 Submerge gaskets in fresh DIW. Measure pH using
the pH probe according to Test Methods D1293. If the pH
value is not within the 5.0 to 7.0 range, repeat step 10.2.9.
For detailed discussion of the influence of surface finish on corrosion see
10.2.11 Dry gaskets in an oven at 90°C and store in a clean
Mendel et al, 1984 (5). Some example results of vapor hydration tests with varying
surface finish are reported in Jiricka et al, 2001 (6). environment until needed.
C1663 − 09
11. Cali
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