ASTM C1663-18

Standard Test Method for Measuring Waste Glass or Glass Ceramic Durability by Vapor Hydration Test

SIGNIFICANCE AND USE
5.1 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)).  
5.2 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 ceramics2 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)3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 31-Oct-2018
• ICS: 81.040.10 - Raw materials and raw glass
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.13 - Spent Fuel and High Level Waste

Relations

• Replaces: ASTM C1663-17 - Standard Test Method for Measuring Waste Glass or Glass Ceramic Durability by Vapor Hydration Test
• Effective Date: 01-Nov-2018
• Refers: ASTM C859-24 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Jan-2024
• Refers: ASTM C162-23 - Standard Terminology of Glass and Glass Products
• Effective Date: 01-Oct-2023
• Refers: ASTM C162-05(2015) - Standard Terminology of<brk type="line"/> Glass and Glass Products
• Effective Date: 01-Nov-2015
• Refers: ASTM C859-14a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Jun-2014
• Refers: ASTM E177-14 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2014
• Refers: ASTM C859-14 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Jan-2014
• Refers: ASTM C859-13a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Jun-2013
• Refers: ASTM C859-13 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-May-2013
• Refers: ASTM E177-13 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2013
• Refers: ASTM E691-13 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-May-2013
• Refers: ASTM D1293-12 - Standard Test Methods for pH of Water
• Effective Date: 01-Jan-2012
• Refers: ASTM E691-11 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Nov-2011
• Refers: ASTM C859-10b - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Nov-2010
• Refers: ASTM E177-10 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Oct-2010

Overview

ASTM C1663-18 is the Standard Test Method for Measuring Waste Glass or Glass Ceramic Durability by Vapor Hydration Test, issued by ASTM International. This standard provides a scientific method for evaluating the corrosion resistance and long-term durability of waste glass and glass ceramic materials when exposed to water vapor at elevated temperatures. The vapor hydration test (VHT) serves as an accelerated aging procedure, offering crucial data on potential alteration mechanisms and phase formations relevant for waste repository environments.

By simulating high-temperature, water vapor-rich scenarios, ASTM C1663-18 is instrumental in supporting the safe disposal of radioactive and hazardous materials encased in glass or glass ceramic matrices. The standard enables researchers and engineers to make relative comparisons between materials and assess the impact of repository conditions on waste forms' integrity.

Key Topics

• Durability Assessment: Evaluates the corrosion and alteration of glass and glass ceramic waste forms in contact with water vapor or thin water films at elevated temperatures, simulating possible repository conditions.
• Accelerated Testing: Utilizes high temperatures to speed up thermally activated corrosion processes, yielding results in shorter timespans compared to natural environmental conditions.
• Screening and Comparison: Serves as a screening tool to determine alteration propensity and compare the performance of different waste forms.
• Alteration Phase Analysis: Identifies secondary phases formed during testing, offering insight into potential phase developments under real disposal situations.
• Quality Assurance: Mandates rigorous instrument calibration, specimen preparation, and data recording to ensure result reliability and repeatability.
• Safety and Compliance: Addresses safe handling and regulatory considerations, emphasizing the need for adherence to health, safety, and environmental practices.

Applications

ASTM C1663-18 is extensively used in several critical sectors:

• Nuclear Waste Management: Supports the long-term performance assessment of vitrified radioactive waste forms, helping to predict their behavior in geological repositories.
• Hazardous Waste Immobilization: Assists in validating the durability of glass and glass ceramic matrices for encapsulating hazardous substances, ensuring minimal leaching over time.
• Materials Research and Development: Provides standardized methodologies for laboratories investigating new glass or glass ceramic waste forms, facilitating material optimization and innovation.
• Regulatory Compliance: Delivers evidence of waste form suitability to satisfy national and international disposal criteria, aiding in licensing and stakeholder approval processes.

By applying this standard, organizations can demonstrate the robustness of their waste forms, mitigate environmental risks, and ensure public and environmental safety in waste containment strategies.

Related Standards

For comprehensive practice, ASTM C1663-18 is used in conjunction with several other ASTM standards:

• ASTM C162: Terminology of Glass and Glass Products
• ASTM C859: Terminology Relating to Nuclear Materials
• ASTM D1125: Test Methods for Electrical Conductivity and Resistivity of Water
• ASTM D1193: Specification for Reagent Water
• ASTM D1293: Test Methods for pH of Water
• ASTM E177: Practice for Use of Terms Precision and Bias in ASTM Test Methods
• ASTM E691: Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method

These related standards provide the necessary terminology, water quality guidelines, calibration instructions, and evaluation frameworks that underpin the reliability of the vapor hydration test results.

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Keywords: ASTM C1663-18, vapor hydration test, glass ceramic durability, waste glass corrosion, waste form performance, nuclear waste disposal, hazardous material immobilization, alteration phase, accelerated corrosion testing, materials standard.

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: C1663 − 18
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 2. Referenced Documents
1.1 The vapor hydration test method can be used to study 2.1 ASTM Standards:
the corrosion of a waste forms such as glasses and glass C162 Terminology of Glass and Glass Products
ceramics upon exposure to water vapor at elevated tempera- C859 Terminology Relating to Nuclear Materials
tures.Inaddition,thealterationphasesthatformcanbeusedas D1125 Test Methods for Electrical Conductivity and Resis-
indicators of those phases that may form under repository tivity of Water
conditions. These tests; which allow altering of glass at high D1193 Specification for Reagent Water
surface area to solution volume ratio; provide useful informa- D1293 Test Methods for pH of Water
tion regarding the alteration phases that are formed, the E177 Practice for Use of the Terms Precision and Bias in
disposition of radioactive and hazardous components, and the ASTM Test Methods
alteration kinetics under the specific test conditions. This E691 Practice for Conducting an Interlaboratory Study to
information may be used in performance assessment (McGrail Determine the Precision of a Test Method
et al, 2002 (1) for example).
3. Terminology
1.2 This test method must be performed in accordance with
3.1 Please refer to Terminologies C162 and C859 for
all quality assurance requirements for acceptance of the data.
additional terminology which may not be listed below.
1.3 This standard does not purport to address all of the
3.2 Definitions:
safety concerns, if any, associated with its use. It is the
3.2.1 immobilized low-activity waste—vitrified low-activity
responsibility of the user of this standard to establish appro-
fraction of waste presently contained in Hanford Site tanks.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. 3.2.2 performance assessment—examines the long-term en-
1.4 This international standard was developed in accor-
vironmental and human health effects associated with the
dance with internationally recognized principles on standard- planned disposal of waste. Mann et al, 2001 (2)
ization established in the Decision on Principles for the
3.2.3 sample—initial test material with known composition.
Development of International Standards, Guides and Recom-
3.2.4 specimen—specimen is a part of the sample used for
mendations issued by the World Trade Organization Technical
testing.
Barriers to Trade (TBT) Committee.
3.2.5 traceable standard—a material that supplies a link to
known test response in standards international units by a
national or international standards body, for example, NIST.
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
3.3 Abbreviations:
and High Level Waste.
3.3.1 DIW—ASTM Type I deionized water
Current edition approved Nov. 1, 2018. Published January 2019. Originally
approved in 2009. Last previous edition approved in 2017 as C1663 – 17. DOI: 3.3.2 EDS—energy dispersive X-ray spectroscopy
10.1520/C1663-18.
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 For referenced ASTM standards, visit the ASTM website, www.astm.org, or
precision of such tests are currently unknown. contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
The boldface numbers in parentheses refer to the list of references at the end of Standards volume information, refer to the standard’s Document Summary page on
this standard. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1663 − 18
3.3.3 OM—optical microscopy 22 mL vessels, rated for service at temperatures up to 300°C
and maximum pressure 11.7 MPa (1700 psi)).
3.3.4 OM/IA—optical microscope connected to an image
analysis system
6.2 Balance(s)—Any calibrated two-point (0.00 grams) bal-
ance.
3.3.5 PTFE—polytetrafluoroethylene (chemical compound
commonly referred to as Teflon)
6.3 Convection Oven—Constant temperature convection
oven with the ability to control the temperature within 62°C.
3.3.6 SEM—scanning electron microscope
3.3.7 SiC paper—silicon-carbide paper 6.4 Temperature Monitoring Device—Resistance thermom-
eters or thermocouples, or both, with a strip chart recorder or
3.3.8 TBD—to be determined
a data logger for periodic monitoring of the temperature of the
3.3.9 TEM—transmission electron microscope
convection oven during the test duration. It is recommended
3.3.10 T —glass transition temperature
g that the maximum period between recorded temperature mea-
3.3.11 VHT—vapor hydration test surements be 0.5 h.
3.3.12 WDS—wave-length dispersive spectroscopy 6.5 Pipettes—Calibratedpipettes.Pipettetipsthathavebeen
pre-cleaned, sterilized, or individually packaged to avoid
3.3.13 XRD—X-ray diffraction
contamination from handling.
3.3.14 %RSD—percent relative standard deviation
6.6 Torque Wrench—Torque wrench capable of torques up
4. Summary of Test Method
to 23.0 N·m (17.0 ft·lb).
4.1 For the vapor hydration tests, glass or glass ceramic
6.7 Vessel Holder—Appropriate device/stand for holding
specimens (referred to generally as glass samples in this test
vessels during tightening/loosening processes.
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 (30 µm).
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
6.12 Chemically Inert Wire—Wire used to suspend the
remaining glass or glass ceramic thickness is measured and
specimens (such as 0.25 mm Pt wire).
alteration phases are identified.
6.13 Support Rods—Typically 1.5 mm diameter 304Lstain-
5. Significance and Use
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
6.14 Non-Combustible Tray—For water to quench vessel
thin films of water. This method may serve as an accelerated
bottom after test termination.
test for some materials, since the high temperatures will
6.15 Storage Vessels—Polyethylene or glass vessels for
accelerate thermally activated processes. A wide range of test
specimen storage.
temperatures have been reported in the literature –40°C (Ebert
et al, 2005 (3), for example) to 300°C (Vienna et al, 2001 (4),
6.16 Ultrasonic Bath.
for example). It should be noted that with increased test
6.17 pH Paper.
temperature comes the possibility of changing the corrosion
6.18 SiC Paper.
rate determining mechanism and the types of phases formed
upon alteration from those that occur in the disposal environ-
6.19 Non-Talc Surgical Gloves.
ment (Vienna et al, 2001 (4)).
6.20 Glass Slides.
5.2 The vapor hydration test can be used as a screening test
6.21 PTFE Tape—The type commonly used for household
to determine the propensity of waste forms to alter and for
plumbing.
relative comparisons in alteration rates between waste forms.
6.22 Tweezers/Forceps.
6. Apparatus
6.1 Test Vessels—Stainless steel vessels with closure fitting
Series 4704 22 mL and 4714 45 mL “A” Socket Vessels from Parr Instrument
with unique identifiers (on both vessel and lid), (for example, Co., 211 53rd St., Moline, IL 61265, have been found satisfactory.
C1663 − 18
6.23 Scissors. 9.1.4 Polish to the dimensions 10.0 by 10.0 by 1.50 mm
using 600 grit (30 µm) SiC paper (with appropriate cooling
6.24 Glue or Thermoplastic Adhesive, for attaching samples
fluid).
and specimen to glass slides (for example, crystal-bond,
super-glue, or wax). 9.2 Ultrasonically clean specimen in ethanol for 2 min,
decant, and discard ethanol.
6.25 pH Probe, calibrated with traceable standards.
9.3 Ultrasonically clean specimen in ethanol for 4 min,
7. Reagents and Standards
decant, and discard ethanol.
7.1 ASTM Type I Water—Type I water shall have a minimal
9.4 Dry specimen in an oven at 90°C for 15 min.
electrical resistivity of 18.0 MΩ·cm at 25°C (see Specification
9.5 Examine each specimen with OM and record observa-
D1193).
tions concerning specimen surface and heterogeneity (streaks,
7.2 Solvents—Absolute ethanol and reagent grade acetone.
inclusions, and scratches).
7.3 Reagent Grade HNO —6 M HNO and 0.16 M HNO .
3 3 3
10. Test Vessel Cleaning
8. Hazards
10.1 Cleaning of Stainless Steel Vessels and Support Rods:
8.1 All appropriate precautions for operation of pressurized
10.1.1 Degrease vessels and lids with acetone. (This step is
equipment must be taken. To ensure safe operation, the test
performed only with new vessels.)
vesselsshouldberatedtowithstandthevaporpressureofwater
10.1.2 Use 400 grit SiC paper to remove debris and oxida-
at the test temperature with an appropriate safety factor.
tion from inside parts of previously used vessels and rinse with
DIW.
9. Specimen Preparation
10.1.3 Ultrasonically clean vessels, lids, and stainless steel
9.1 Glass or glass ceramic specimens are prepared from
supports in ethanol for 5 min, decant and discard ethanol.
annealed bars (for example, anneal 2 hours at a temperature
10.1.4 Rinse vessels, lids, and supports by immersing 3
slightly above the glass transition temperature with subsequent
times in fresh DIW.
slowcoolingtoroomtemperatureinsidetheoven,caremustbe
10.1.5 Soak vessels, lids, and supports in reagent grade 0.16
taken not to induce phase changes during annealing).Annealed
M HNO at 90°C for 1 h.
bars are cut with a diamond impregnated saw and SiC papers
10.1.6 Rinse vessels, lids, and supports by immersing 3
with different grits. During the specimen preparation, it is
times in fresh DIW.
important to use low cutting force and saw speed (dependent
10.1.7 Soakvessels,lids,andsupportsinfreshDIWat90°C
on sample). Rough surface and damaged edges of the samples
for1h.
indicate rough machining. This may cause cracks to form
10.1.8 Rinse vessels, lids, and supports by immersing in
within the glass or glass ceramic specimen during the sample
fresh DIW.
preparation and decrease the reproducibility of the test. Prepa-
10.1.9 Fill vessels (with supports placed inside) to 80–90 %
ration of the specimen may vary according to the equipment
of capacity with fresh DIW. Place lids on vessels. Do not
used. Usually specimens are prepared slightly larger and
tighten. Place them in an oven at 90°C for a minimum of 16 h.
subsequently polished to the desired dimensions. However,
10.1.10 After cooling, measure the pH of the DIWusing the
with certain types of diamond impregnated saws, it is possible
pH probe according to Test Methods D1293. If the pH value is
to prepare specimens with the desired dimensions and polish
not within the 5.0 to 7.0 range, repeat rinsing from step 10.1.6.
the surface directly with 600 grit SiC paper. The details of one
10.1.11 Dry vessels, lids, and supports in an oven at 90°C
example of preparation technique are given below. These steps
for at least 1 h.
(9.1.1 – 9.1.4) are only given as an example and can be
10.1.12 Store vessels, lids, and supports in a clean, dry,
adjusted to yield the desired specimen dimensions and surface
environment until use.
finish.
10.2 Cleaning of PTFE Gaskets:
9.1.1 Cut annealed glass or glass ceramic bars with a
diamond-impregnated saw to roughly the dimensions 10.3 by
NOTE 1—Other gasket materials may be used, so long as they do not
significantlyimpactthereactionsbetweenwaterandthesample.Thismay
10.3 by 1.6 mm (with appropriate cooling fluid). For certain
be an important consideration in high radiation environments.
samples, such as glass ceramic materials, water should be
avoided in order to not dissolve the soluble phase. 10.2.1 Bake PTFE gaskets for 1 week at 200°C. (This step
9.1.2 Polish to roughly the dimensions 10.2 by 10.2 by 1.55
is performed only with new PTFE gaskets.)
mm using 240 grit (70 µm) SiC (with appropriate cooling 10.2.2 Soak the gaskets in reagent grade6MHNO at
fluid).
50 6 5°C for 4 h.
9.1.3 Polish to roughly the dimensions 10.1 by 10.1 by 1.51 10.2.3 Rinse the gaskets by immersing in fresh DIW 3
mm using 400 grit (40 µm) SiC (with appropriate cooling
times.
fluid).
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.
For detailed discussion of the influence of surface finish on corrosion see
10.2.6 Soak the gaskets for8hin fresh DIW at 80°C.
Mendel et al, 1984 (5). Some example results of vapor hydration tests with varying
surface finish are reported in Jiricka et al, 2001 (6). 10.2.7 Rinse the gaskets by immersing in fresh DIW.
C1663 − 18
10.2.8 Immerse the gaskets in fresh DIW and boil for 30 12.2.2 Verify that the stainless steel test vessels have been
min. cleaned according to Section 10. The vessels must have a
unique number permanently affixed to the vessel cap and
10.2.9 Rinsethegasketsbyimmersing3timesinfreshDIW
bottom.
(container with gaskets is filled 3 times with fresh DIW).
12.2.3 Wind the threads of the vessel closure fittings with
10.2.10 Submerge gaskets in fresh DIW. Measure pH using
PTFE tape to prevent binding of the closure threads (roughly 2
the pH probe according to Test Methods D1293. If the pH
wraps).
value is not within the 5.0 to 7.0 range, repeat step 10.2.9.
12.2.4 Verify that a calibrated balance accurate to 60.01 g
10.2.11 Dry gaskets in an oven at 90°C and store in a clean
is available.
environment until needed.
12.2.5 Verify that a pipette and fresh DIW are available.
12.2.6 Verify that a torque wrench is available and set to the
11. Calibration
desired setting between 20.3 N·m and 23.0 N·m (15.0 ft·lbf to
17.0 ft·lbf).
11.1 Calibrations—Initially calibrate all measurement in-
12.2.7 Verify that the stainless steel support rods have been
struments used in this test.Verify the calibrations during use of
cleaned and thoroughly rinsed with ethanol according to
the instrument to indicate possible errors due to instrumental
Section 10.
drift.
12.2.8 Verifythattherequireddatasheetandtestparameters
11.2 Calibration and Standardization Schedule:
for the VHT are available, see Appendix X1 for an example
11.2.1 Temperature Measurement Devices—Calibrate at
data sheet.
least annually with traceable standards or an ice/boiling water
12.2.9 Verify that the test specimens are prepared according
bath.
to Section 9.
11.2.2 Balance—Standardize with traceable standard
12.3 Test Start-Up Procedure:
masses on a regular basis. If a deviation in mass measurement
12.3.1 Record the following information on a VHT Data
is identified, all measurements since the last accurate standard
Sheet: (1) Test number, (2) Test temperature, (3) Planned test
measurement made with the balance must be marked appro-
duration, (4) Vessel and cap identification number, and (5)
priately. Have balance calibrated on an annual basis.
Sample/specimen identification.
11.2.3 Water Purification System—Calibrate at least annu-
12.3.2 Wear non-talc gloves (or equivalent covering if in
ally following the manufacturer’s instructions. Standardize
remote environment) and use tweezers when tying the speci-
with the 10 MΩ·cm at 25°C resistivity calibration cell (or
men as shown in Fig. 1.
equivalent) on the water purification system (see Test Methods
12.3.3 Place the support with specimen in proper position
D1125).
inside the assigned vessel as shown in Fig. 2.
12.3.4 Place a clean PTFE gasket (or equivalent) inside a
11.2.4 Calipers—Calibrate with traceable standards at least
annually. vessel cap.
11.2.5 Image Analysis System—Calibrate with a micromet-
NOTE 2—The PTFE gasket should be replaced by a different material in
ric calibration ruler designed for image analysis calibration. those cases where high radiation fields and long test times are expected to
introduce sufficient fluorine onto the test specimen to influence test result.
12. Procedure for Conducting the Vapor Hydration Test 12.3.5 Place vessel bottom, cap and vessel closure (not
assembled) on a balance accurate to 60.01 g and record the
12.1 Amount of Water Needed—In order to conduct reliable
mass.
VHTs, the amount of water added to the vessel must be
12.3.6 Using a pipette, add the targeted amount (in mL) of
sufficient to saturate the vessel’s volume at the test temperature
fresh DIW (See Table 1 as example for 22 mL vessel with one
and provide excess water that can condense on the test
sample. The exact volume can be determined as the maximum
specimen surface without sufficient water to reflux during
volumethatdoesnotresultinsolutionreflux(see13.6.1)tothe
testing. The amount of water needed for saturating a 22 mL
vessel was calculated assuming ideal conditions, H O, N , and
2 2
O . It consists of an amount of water needed to saturate the
vessel at a given temperature (determined from steam tables)
plus an additional 0.05 mL of excess water needed for each
specimen with dimensions of 10.0 by 10.0 by 1.5 mm (surface
area 260 mm ). The volume of the specimen assembly
(specimen, support rod, and chemically inert wire) was not
accounted for in steam saturation calculations. Similar calcu-
lations should be performed if using vessels with different
volumes.
12.2 Test Set-Up:
12.2.1 Verify that the convection oven is at the desired
temperature and temperature-monitoring device has been cali-
FIG. 1 Glass Specimen Suspended with Thin Pt Wire
brated. (roughly 0.2 mm diameter)
C1663 − 18
FIG. 2 Apparatus for Conducting Vapor Hydration Tests
TABLE 1 Vapor Pressure and Amounts of Water Needed for the
12.3.9 Place the test vessel inside the oven and record the
VHT with 22 mL Vessels for Temperatures from 5°C to 300°C
time and date on the data sheet.
NOTE 1—The table should be used as a guide to determine the mass of
12.4 During Test:
water necessary to perform a test.
12.4.1 It is allowed, but not required, to check the test
A A
T [°C] P [MPa] H O [g] T [°C] P [MPa] H O[g]
2 2
vessels for fluid leakage during testing (for example, after one
5 6.1E-04 0.05 110 1.4E-01 0.07
day) by quickly removing the vessel from the oven, weighing
10 8.8E-04 0.05 115 1.7E-01 0.07
15 1.2E-03 0.05 120 2.0E-01 0.08 it on a calibrated balance, and returning it to the oven. This is
20 1.7E-03 0.05 125 2.3E-01 0.08
particularly important in long-term tests when water loss has
25 2.4E-03 0.05 130 2.7E-01 0.09
been found to be significant. Record the results on the data
30 3.2E-03 0.05 140 3.6E-01 0.10
sheet.
35 4.3E-03 0.05 150 4.8E-01 0.11
40 5.7E-03 0.05 160 6.2E-01 0.13
12.4.2 Record the temperature during the test period in 0.5
45 7.4E-03 0.05 170 8.0E-01 0.15
h intervals with a calibrated measurement device.
50 9.6E-03 0.05 180 1.0E+00 0.18
55 1.2E-02 0.05 190 1.3E+00 0.21
12.5 Test Termination:
60 1.6E-02 0.05 200 1.6E+00 0.25
65 2.0E-02 0.05 210 1.9E+00 0.29 12.5.1 Record the temperature, date and time out of the
70 2.5E-02 0.05 220 2.3E+00 0.35
oven on the data sheet when the test is complete.
75 3.1E-02 0.06 230 2.8E+00 0.42
12.5.2 Place a piece of refractory block on a calibrated
80 3.9E-02 0.06 240 3.4E+00 0.49
85 4.8E-02 0.06 250 4.0E+00 0.59 balance accurate to 60.01 g and tare the balance.
90 5.8E-02 0.06 260 4.7E+00 0.70
12.5.3 Remove the test vessels, one at a time, and place on
95 7.0E-02 0.06 270 5.5E+00 0.83
the refractory piece on the balance. Record the mass of each
100 8.5E-02 0.06 280 6.4E+00 0.98
105 1.0E-01 0.07 300 7.5E+00 1.39 test vessel. The difference in mass between test initiation and
A
“NBS/NRS Steam Tables,” Lester Haar et al, Hemisphere Publishing Corp., 1984, termination indicates the amount of water evaporated during
pp. 9–14.
the test.
12.5.4 Place the vessel in cold water (roughly 20 mm deep)
for approximately 20 min. For temperatures higher than 200°C
ice water is recommended.
vessel and record the mass. Verify that the amount of water
12.5.5 Place assembly in an appropriate device/stand for
added is the difference between dry assembly and assembly
including water. holding vessels during loosening. Loosen and remove the
closure fitting.
12.3.7 Place the assembly in an appropriate device/stand for
holding vessels during tightening and tighten with torque 12.5.6 Open the vessel, remove the test specimen, allow
wrench to between 20.3 N·m and 23.0 N·m (15.0 ft·lb to 17.0 specimen to dry. It is recommended that the time between
ft·lb). terminating the test and opening the vessel does not exceed 30
12.3.8 Recordtheoventemperatureandcalibrationstatusof min due to the potential hygroscopic nature of the specimen’s
the temperature monitoring device on the data sheet. surface.
C1663 − 18
12.5.7 Record observations pertaining to specimen(s) 13.2.2 Toillustratethemethodforselectingsampleanalyses
surface, drying pattern, secondary phase development, and techniques we use a specimen reported by Vienna et al, 2001
overall integrity of the specimen(s). (4)—HLP-51 glass tested at 300°C for 2 days. An optical
12.5.8 Place the specimen(s) into the pre-labeled contain- micrograph of the cross section of this specimen is shown in
er(s). Labels should include test number (indicating the type of Fig. 3. For measurement of this sample, we can choose
sample tested), test temperature, and test period. betweenOMandSEM,andmeasurementofremainingglassor
12.5.9 Note the presence or absence of fluid remaining on glass ceramic thickness or alteration products thickness. Ten
the bottom of the test vessel and on specimens. measurements of the remaining glass or glass ceramic thick-
12.5.10 Measure and record the approximate pH of the fluid nessreturnathicknessof0.39 60.06mm.Theprecisionofthe
in the test vessel with pH paper capable of indicating pH in the OM/IAwas determined to be 0.003 mm while the precision of
range from 5 to 10. the SEM/IAmethod (not shown) was found to be 1 %, relative,
or 0.004 mm for a measurement of 0.4 mm. In this case, the
13. Interpretation of Results
precision of remaining glass or glass ceramic thickness mea-
surement by both methods are roughly equal and an order of
13.1 Specimen Analyses for Alteration Products:
magnitude less than the variation in the sample. So, either
13.1.1 Specimens can be analyzed for the presence of
method could be performed without impacting measurement
secondary phases by visual observation and OM; type of
precision. The other key decision is the measurement of
secondaryphasesbyXRD,OM,SEM/EDS,microprobe/WDS,
remaining glass or glass ceramic thickness or the thickness of
or TEM/EDS, or combinations thereof; remaining glass layer
alteration products. For this sample, the alteration products
thicknessbyOM/IAorSEM/EDS(seeSection13.3);alteration
thickness is found to be 0.91 6 0.35 mm on the top and 1.14
layer thickness by SEM/IA or OM/IA (see section 13.4), and
6 0.45 mm on the bottom. Clearly, in this particular sample
extent of corrosion (see section 13.5). The thickness of these
there is significantly more variation in alteration products
layers may be used to estimate the amount of glass altered.
thickness making the measurement less precise than measuring
Section 13.2 describes the advantages and disadvantages of the
remaining glass or glass ceramic thickness. In addition, the
two methods for sample analyses and suggests how to select
overall sample thickness grew from 1.52 6 0.008 mm before
between the two methods.
testing to 2.51 6 0.45 mm after testing. The mass grew only
13.2 Selection of Method for Sample Analyses:
slightly due to the addition of water so the density of the
13.2.1 To determine the amount of glass or glass ceramic
alteration layer is significantly lower than the initial glass or
converted into alteration products, it is possible to measure the
glassceramic.Thisdifferenceindensitycanbecorrectedforas
remaining glass thickness or the thickness of alteration layers.
described in section 13.5.3, but, adds to imprecision.
Generally, the method with the highest precision is preferred.
13.2.3 For samples with lower variation in alteration layer
Jiricka et al, 2001
...

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. Because
it 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 version
of the standard as published by ASTM is to be considered the official document.
Designation: C1663 − 17 C1663 − 18
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
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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
C162 Terminology of Glass and Glass Products
C859 Terminology Relating to Nuclear Materials
D1125 Test Methods for Electrical Conductivity and Resistivity of Water
D1193 Specification for Reagent Water
D1293 Test Methods for pH of Water
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Terminology
3.1 Please refer to Terminologies C162 and C859 for additional terminology which may not be listed below.
3.2 Definitions:
3.2.1 immobilized low-activity waste—vitrified low-activity fraction of waste presently contained in Hanford Site tanks.
3.2.2 performance assessment—examines the long-term environmental and human health effects associated with the planned
disposal of waste. Mann et al, 2001 (2)
3.2.3 sample—initial test material with known composition.
3.2.4 specimen—specimen is a part of the sample used for testing.
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 and
High Level Waste.
Current edition approved Nov. 1, 2017Nov. 1, 2018. Published December 2017January 2019. Originally approved in 2009. Last previous edition approved in 20092017
as C1663 – 09.C1663 – 17. DOI: 10.1520/C1663-17.10.1520/C1663-18.
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 precision
of such tests are currently unknown.
The boldface numbers in parentheses refer to the list of references at the end of this standard.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1663 − 18
3.2.5 traceable standard—a material that supplies a link to known test response in standards international units by a national
or international standards body, for example, NIST.
3.3 Abbreviations:
3.3.1 DIW—ASTM Type I deionized water
3.3.2 EDS—energy dispersive X-ray spectroscopy
3.3.3 OM—optical microscopy
3.3.4 OM/IA—optical microscope connected to an image analysis system
3.3.5 PTFE—polytetrafluoroethylene (chemical compound commonly referred to as Teflon)
3.3.6 SEM—scanning electron microscope
3.3.7 SiC paper—silicon-carbide paper
3.3.8 TBD—to be determined
3.3.9 TEM—transmission electron microscope
3.3.10 T —glass transition temperature
g
3.3.11 VHT—vapor hydration test
3.3.12 WDS—wave-length dispersive spectroscopy
3.3.13 XRD—X-ray diffraction
3.3.14 %RSD—percent relative standard deviation
4. Summary of Test Method
4.1 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 volume of water determined by the volume of the
test vessel and the test temperature is added to the vessel. The vessel is then sealed and placed in an oven at the desired test
temperature and left undisturbed. After the desired test duration, the vessel is removed from the oven and the bottom of the vessel
is cooled to condense the vapor in the vessel. Specimens are removed and examined with optical microscopy, XRD, SEM, and
other analytical methods. The remaining glass or glass ceramic thickness is measured and alteration phases are identified.
5. Significance and Use
5.1 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)).
5.2 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.
6. Apparatus
6.1 Test Vessels—Stainless steel vessels with closure fitting with unique identifiers (on both vessel and lid), (for example, 22
mL vessels, rated for service at temperatures up to 300°C and maximum pressure 11.7 MPa (1700 psi)).
6.2 Balance(s)—Any calibrated two-point (0.00 grams) balance.
6.3 Convection Oven—Constant temperature convection oven with the ability to control the temperature within 62°C.
6.4 Temperature Monitoring Device—Resistance thermometers or thermocouples, or both, with a strip chart recorder or a data
logger for periodic monitoring of the temperature of the convection oven during the test duration. It is recommended that the
maximum period between recorded temperature measurements be 0.5 h.
6.5 Pipettes—Calibrated pipettes. Pipette tips that have been pre-cleaned, sterilized, or individually packaged to avoid
contamination from handling.
6.6 Torque Wrench—Torque wrench capable of torques up to 23.0 N·m (17.0 ft·lb).
6.7 Vessel Holder—Appropriate device/stand for holding vessels during tightening/loosening processes.
6.8 Diamond Impregnated Saw—High or low density diamond-coated wafering blade and low speed saw.
Series 4704 22 mL and 4714 45 mL “A” Socket Vessels from Parr Instrument Co., 211 53rd St., Moline, IL 61265, have been found satisfactory.
C1663 − 18
6.9 Polishing Equipment—Polishing equipment capable of polishing to 600 grit (30 μm).
6.10 Calipers—Calipers that have been calibrated with traceable standards.
6.11 Optical Microscope with Image Analysis System.
6.12 Chemically Inert Wire—Wire used to suspend the specimens (such as 0.25 mm Pt wire).
6.13 Support Rods—Typically 1.5 mm diameter 304L stainless steel (or comparable material) rods bent to the shape shown in
Fig. 2. Used to suspend specimens within the pressure vessel during tests.
6.14 Non-Combustible Tray—For water to quench vessel bottom after test termination.
6.15 Storage Vessels—Polyethylene 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 Tape—The 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 Standards
7.1 ASTM Type I Water—Type I water shall have a minimal electrical resistivity of 18.0 MΩ·cm at 25°C (see Specification
D1193).
7.2 Solvents—Absolute ethanol and reagent grade acetone.
7.3 Reagent Grade HNO —6 M HNO and 0.16 M HNO .
3 3 3
8. Hazards
8.1 All appropriate precautions for operation of pressurized equipment must be taken. To ensure safe operation, the test vessels
should be rated to withstand the vapor pressure of water at the test temperature with an appropriate safety factor.
9. Specimen Preparation
9.1 Glass or glass ceramic specimens are prepared from annealed bars (for example, anneal 2 hours at a temperature slightly
above the glass transition temperature with subsequent slow cooling to room temperature inside the oven, care must be taken not
to induce phase changes during annealing). Annealed bars are cut with a diamond impregnated saw and SiC papers with different
grits. During the specimen preparation, it is important to use low cutting force and saw speed (dependent on sample). Rough
surface and damaged edges of the samples indicate rough machining. This may cause cracks to form within the glass or glass
ceramic specimen during the sample preparation and decrease the reproducibility of the test. Preparation of the specimen may vary
according to the equipment used. Usually specimens are prepared slightly larger and subsequently polished to the desired
dimensions. However, with certain types of diamond impregnated saws, it is possible to prepare specimens with the desired
dimensions and polish the surface directly with 600 grit SiC paper. The details of one example of preparation technique are given
below. These steps (9.1.1 – 9.1.4) are only given as an example and can be adjusted to yield the desired specimen dimensions and
surface 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 1.6
mm (with appropriate cooling fluid). For certain samples, such as glass ceramic materials, water should be avoided in order to not
dissolve the soluble phase.
9.1.2 Polish to roughly the dimensions 10.2 by 10.2 by 1.55 mm using 240 grit (70 μm) 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 (40 μm) 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 μm) SiC paper (with appropriate cooling fluid).
For detailed discussion of the influence of surface finish on corrosion see Mendel et al, 1984 (5). Some example results of vapor hydration tests with varying surface
finish are reported in Jiricka et al, 2001 (6).
C1663 − 18
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 90°C 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 Cleaning
10.1 Cleaning of Stainless Steel Vessels and Support Rods:
10.1.1 Degrease 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, decant 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 HNO at 90°C 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 90°C 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 80–90 % of capacity with fresh DIW. Place lids on vessels. Do not tighten.
Place them in an oven at 90°C for a minimum of 16 h.
10.1.10 After cooling, measure the pH of the DIW using the pH probe according to Test Methods D1293. If the pH value is
not 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 90°C 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 1—Other gasket materials may be used, so long as they do not significantly impact the reactions between water and the sample. This may be
an important consideration in high radiation environments.
10.2.1 Bake PTFE gaskets for 1 week at 200°C. (This step is performed only with new PTFE gaskets.)
10.2.2 Soak the gaskets in reagent grade 6 M HNO at 50 6 5°C 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 for 8 h in fresh DIW at 80°C.
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. 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.
10.2.11 Dry gaskets in an oven at 90°C and store in a clean environment until needed.
11. Calibration
11.1 Calibrations—Initially calibrate all measurement instruments used in this test. Verify the calibrations during use of the
instrument to indicate possible errors due to instrumental drift.
11.2 Calibration and Standardization Schedule:
11.2.1 Temperature Measurement Devices—Calibrate at least annually with traceable standards or an ice/boiling water bath.
11.2.2 Balance—Standardize with traceable standard masses on a regular basis. If a deviation in mass measurement is identified,
all measurements since the last accurate standard measurement made with the balance must be marked appropriately. Have balance
calibrated on an annual basis.
11.2.3 Water Purification System—Calibrate at least annually following the manufacturer’s instructions. Standardize with the 10
MΩ·cm at 25°C resistivity calibration cell (or equivalent) on the water purification system (see Test Methods D1125).
11.2.4 Calipers—Calibrate with traceable standards at least annually.
11.2.5 Image Analysis System—Calibrate with a micrometric calibration ruler designed for image analysis calibration.
12. Procedure for Conducting the Vapor Hydration Test
12.1 Amount of Water Needed—In order to conduct reliable VHTs, the amount of water added to the vessel must be sufficient
to saturate the vessel’s volume at the test temperature and provide excess water that can condense on the test specimen surface
without sufficient water to reflux during testing. The amount of water needed for saturating a 22 mL vessel was calculated assuming
ideal conditions, H O, N , and O . It consists of an amount of water needed to saturate the vessel at a given temperature
2 2 2
C1663 − 18
(determined from steam tables) plus an additional 0.05 mL of excess water needed for each specimen with dimensions of 10.0 by
10.0 by 1.5 mm (surface area 260 mm ). The volume of the specimen assembly (specimen, support rod, and chemically inert wire)
was not accounted for in steam saturation calculations. Similar calculations should be performed if using vessels with different
volumes.
12.2 Test Set-Up:
12.2.1 Verify that the convection oven is at the desired temperature and temperature-monitoring device has been calibrated.
12.2.2 Verify that the stainless steel test vessels have been cleaned according to Section 10. The vessels must have a unique
number permanently affixed to the vessel cap and bottom.
12.2.3 Wind the threads of the vessel closure fittings with PTFE tape to prevent binding of the closure threads (roughly 2 wraps).
12.2.4 Verify that a calibrated balance accurate to 60.01 g is available.
12.2.5 Verify that a pipette and fresh DIW are available.
12.2.6 Verify that a torque wrench is available and set to the desired setting between 20.3 N·m and 23.0 N·m (15.0 ft·lbft·lbf
to 17.0 ft·lb).ft·lbf).
12.2.7 Verify that the stainless steel support rods have been cleaned and thoroughly rinsed with ethanol according to Section
10.
12.2.8 Verify that the required data sheet and test parameters for the VHT are available, see Appendix X1 for an example data
sheet.
12.2.9 Verify that the test specimens are prepared according to Section 9.
12.3 Test Start-Up Procedure:
12.3.1 Record the following information on a VHT Data Sheet: (1) Test number, (2) Test temperature, (3) Planned test duration,
(4) Vessel and cap identification number, and (5) Sample/specimen identification.
12.3.2 Wear non-talc gloves (or equivalent covering if in remote environment) and use tweezers when tying the specimen as
shown in Fig. 1.
12.3.3 Place the support with specimen in proper position inside the assigned vessel as shown in Fig. 2.
12.3.4 Place a clean PTFE gasket (or equivalent) inside a vessel cap.
NOTE 2—The PTFE gasket should be replaced by a different material in those cases where high radiation fields and long test times are expected to
introduce sufficient fluorine onto the test specimen to influence test result.
12.3.5 Place vessel bottom, cap and vessel closure (not assembled) on a balance accurate to 60.01 g and record the mass.
12.3.6 Using a pipette, add the targeted amount (in mL) of fresh DIW (See Table 1 as example for 22 mL vessel with one
sample) sample. The exact volume can be determined as the maximum volume that does not result in solution reflux (see 13.6.1)
to the vessel and record the mass. Verify that the amount of water added is the difference between dry assembly and assembly
including water.
12.3.7 Place the assembly in an appropriate device/stand for holding vessels during tightening and tighten with torque wrench
to between 20.3 N·m and 23.0 N·m (15.0 ft·lb to 17.0 ft·lb).
12.3.8 Record the oven temperature and calibration status of the temperature monitoring device on the data sheet.
12.3.9 Place the test vessel inside the oven and record the time and date on the data sheet.
12.4 During Test:
12.4.1 It is allowed, but not required, to check the test vessels for fluid leakage during testing (for example, after one day) by
quickly removing the vessel from the oven, weighing it on a calibrated balance, and returning it to the oven. This is particularly
important in long-term tests when water loss has been found to be significant. Record the results on the data sheet.
12.4.2 Record the temperature during the test period in 0.5 h intervals with a calibrated measurement device.
12.5 Test Termination:
FIG. 1 Glass Specimen Suspended with Thin Pt Wire
(roughly 0.2 mm diameter)
C1663 − 18
FIG. 2 Apparatus for Conducting Vapor Hydration Tests
TABLE 1 Vapor Pressure and Amounts of Water Needed for the
VHT with 22 mL Vessels for Temperatures from 5°C to 300°C
NOTE 1—The table should be used as a guide to determine the mass of
water necessary to perform a test.
A A
T [°C] P [MPa] H O [g] T [°C] P [MPa] H O [g]
2 2
5 6.1E-04 0.05 110 1.4E-01 0.07
10 8.8E-04 0.05 115 1.7E-01 0.07
15 1.2E-03 0.05 120 2.0E-01 0.08
20 1.7E-03 0.05 125 2.3E-01 0.08
25 2.4E-03 0.05 130 2.7E-01 0.09
30 3.2E-03 0.05 140 3.6E-01 0.10
35 4.3E-03 0.05 150 4.8E-01 0.11
40 5.7E-03 0.05 160 6.2E-01 0.13
45 7.4E-03 0.05 170 8.0E-01 0.15
50 9.6E-03 0.05 180 1.0E+00 0.18
55 1.2E-02 0.05 190 1.3E+00 0.21
60 1.6E-02 0.05 200 1.6E+00 0.25
65 2.0E-02 0.05 210 1.9E+00 0.29
70 2.5E-02 0.05 220 2.3E+00 0.35
75 3.1E-02 0.06 230 2.8E+00 0.42
80 3.9E-02 0.06 240 3.4E+00 0.49
85 4.8E-02 0.06 250 4.0E+00 0.59
90 5.8E-02 0.06 260 4.7E+00 0.70
95 7.0E-02 0.06 270 5.5E+00 0.83
100 8.5E-02 0.06 280 6.4E+00 0.98
105 1.0E-01 0.07 300 7.5E+00 1.39
A
“NBS/NRS Steam Tables,” Lester Haar et al, Hemisphere Publishing Corp., 1984,
pp. 9–14.
12.5.1 Record the temperature, date and time out of the oven on the data sheet when the test is complete.
12.5.2 Place a piece of refractory block on a calibrated balance accurate to 60.01 g and tare the balance.
12.5.3 Remove the test vessels, one at a time, and place on the refractory piece on the balance. Record the mass of each test
vessel. The difference in mass between test initiation and termination indicates the amount of water evaporated during the test.
12.5.4 Place the vessel in cold water (roughly 20 mm deep) for approximately 20 min. For temperatures higher than 200°C ice
water is recommended.
12.5.5 Place assembly in an appropriate device/stand for holding vessels during loosening. Loosen and remove the closure
fitting.
C1663 − 18
12.5.6 Open the vessel, remove the test specimen, allow specimen to dry. It is recommended that the time between terminating
the test and opening the vessel does not exceed 30 min due to the potential hygroscopic nature of the specimen’s surface.
12.5.7 Record observations pertaining to specimen(s) surface, drying pattern, secondary phase development, and overall
integrity of the specimen(s).
12.5.8 Place the specimen(s) into the pre-labeled container(s). Labels should include test number (indicating the type of sample
tested), test temperature, and test period.
12.5.9 Note the presence or absence of fluid remaining on the bottom of the test vessel and on specimens.
12.5.10 Measure and record the approximate pH of the fluid in the test vessel with pH paper capable of indicating pH in the
range from 5 to 10.
13. Interpretation of Results
13.1 Specimen Analyses for Alteration Products:
13.1.1 Specimens can be analyzed for the presence of secondary phases by visual observation and OM; type of secondary
phases by XRD, OM, SEM/EDS, microprobe/WDS, or TEM/EDS, or combinations thereof; remaining glass layer thickness by
OM/IA or SEM/EDS (see Section 13.3); alteration layer thickness by SEM/IA or OM/IA (see section 13.4), and extent of corrosion
(see section 13.5). The thickness of these layers may be used to estimate the amount of glass altered. Section 13.2 describes the
advantages and disadvantages of the two methods for sample analyses and suggests how to select between the two methods.
13.2 Selection of Method for Sample Analyses:
13.2.1 To determine the amount of glass or glass ceramic converted into alteration products, it is possible to measure the
remaining glass thickness or the thickness of alteration layers. Generally, the method with the highest precision is preferred. Jiricka
et al, 2001 (6) performed detailed analyses of the relative merits of each technique. In measuring the alteration layer, the layer
density is typically lower than that of the glass or glass ceramic and varies widely with glass or glass ceramic composition and
test condition; additionally, the alteration layers are non-uniform in thickness and density. In measuring the remaining glass or glass
ceramic thickness, the measurement of a relatively small difference in thickness can have low measurement precision. The exact
thickness at which the precision of remaining glass or glass ceramic measurement becomes preferable depends on the precision
of the specific equipment used to measure samples. An example calculation to determine the appropriate method of sample
analyses follows.
13.2.2 To illustrate the method for selecting sample analyses techniques we use a specimen reported by Vienna et al, 2001
(4)—HLP-51 glass tested at 300°C for 2 days. An optical micrograph of the cross section of this specimen is shown in Fig. 3. For
measurement of this sample, we can choose between OM and SEM, and measurement of remaining glass or glass ceramic
thickness or alteration products thickness. Ten measurements of the remaining glass or glass ceramic thickness return a thickness
of 0.39 6 0.06 mm. The precision of the OM/IA was determined to be 0.003 mm while the precision of the SEM/IA method (not
shown) was found to be 1 %, relative, or 0.004 mm for a measurement of 0.4 mm. In this case, the precision of remaining glass
or glass ceramic thickness measurement by both methods are roughly equal and an order of magnitude less than the variation in
the sample. So, either method could be performed without impacting measurement precision. The other key decision is the
measurement of remaining
...