ASTM C1720-11
(Test Method)Standard Test Method for Determining Liquidus Temperature of Immobilized Waste Glasses and Simulated Waste Glasses
Standard Test Method for Determining Liquidus Temperature of Immobilized Waste Glasses and Simulated Waste Glasses
SIGNIFICANCE AND USE
This procedure can be used for (but is limited to) the following applications:
(1) support glass formulation development to make sure that processing criteria are met,
(2) support production (for example, processing or troubleshooting), and
(3) support model validation.
SCOPE
1.1 These practices cover procedures for determining the liquidus temperature (TL) of nuclear waste, mixed nuclear waste, simulated nuclear waste, or hazardous waste glass in the temperature range from 600°C to 1600°C. This method differs from Practice C829 in that it employs additional methods to determine TL. TL is useful in waste glass plant operation, glass formulation, and melter design to determine the minimum temperature that must be maintained in a waste glass melt to make sure that crystallization does not occur or is below a particular constraint, for example, 1 volume % crystallinity or T1%. As of now, many institutions studying waste and simulated waste vitrification are not in agreement regarding this constraint (1).
1.2 Three methods are included, differing in (1) the type of equipment available to the analyst (that is, type of furnace and characterization equipment), (2) the quantity of glass available to the analyst, (3) the precision and accuracy desired for the measurement, and (4) candidate glass properties. The glass properties, for example, glass volatility and estimated TL, will dictate the required method for making the most precise measurement. The three different approaches to measuring TL described here include the following: (A) Gradient Temperature Furnace Method (GT), (B) Uniform Temperature Furnace Method (UT), and (C) Crystal Fraction Extrapolation Method (CF). This procedure is intended to provide specific work processes, but may be supplemented by test instructions as deemed appropriate by the project manager or principle investigator. The methods defined here are not applicable to glasses that form multiple immiscible liquid phases. Immiscibility may be detected in the initial examination of glass during sample preparation (see 9.3). However, immiscibility may not become apparent until after testing is underway.
1.3 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance with the standard.
1.4 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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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: C1720 − 11
StandardTest Method for
Determining Liquidus Temperature of Immobilized Waste
Glasses and Simulated Waste Glasses
This standard is issued under the fixed designation C1720; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope system shall be used independently of the other. Combining
values from the two systems may result in non-conformance
1.1 These practices cover procedures for determining the
with the standard.
liquidus temperature (T ) of nuclear waste, mixed nuclear
L
waste,simulatednuclearwaste,orhazardouswasteglassinthe 1.4 This standard does not purport to address all of the
temperature range from 600°C to 1600°C. This method differs safety concerns, if any, associated with its use. It is the
from Practice C829 in that it employs additional methods to responsibility of the user of this standard to establish appro-
determine T . T is useful in waste glass plant operation, glass priate safety and health practices and determine the applica-
L L
formulation, and melter design to determine the minimum bility of regulatory limitations prior to use.
temperature that must be maintained in a waste glass melt to
2. Referenced Documents
make sure that crystallization does not occur or is below a
particular constraint, for example, 1 volume % crystallinity or 2.1 ASTM Standards:
T . As of now, many institutions studying waste and simu- C162Terminology of Glass and Glass Products
1%
lated waste vitrification are not in agreement regarding this C829PracticesforMeasurementofLiquidusTemperatureof
constraint (1). Glass by the Gradient Furnace Method
D1129Terminology Relating to Water
1.2 Three methods are included, differing in (1) the type of
D1193Specification for Reagent Water
equipment available to the analyst (that is, type of furnace and
E177Practice for Use of the Terms Precision and Bias in
characterization equipment), (2) the quantity of glass available
ASTM Test Methods
to the analyst, (3) the precision and accuracy desired for the
E691Practice for Conducting an Interlaboratory Study to
measurement, and (4) candidate glass properties. The glass
Determine the Precision of a Test Method
properties, for example, glass volatility and estimated T , will
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E2282Guide for Defining the Test Result of a Test Method
dictate the required method for making the most precise
2.2 Other Documents:
measurement. The three different approaches to measuring T
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SRM-773 National Institute for Standards and Technology
described here include the following: (A) Gradient Tempera-
(NIST) Liquidus Temperature Standard
ture Furnace Method (GT),(B) Uniform Temperature Furnace
SRM-674bNIST X-Ray Powder Diffraction Intensity Set
Method (UT), and (C) Crystal Fraction Extrapolation Method
for Quantitative Analysis by X-Ray Diffraction (XRD)
(CF). This procedure is intended to provide specific work
SRM-1976aNISTInstrument Response Standard for X-Ray
processes, but may be supplemented by test instructions as
Powder Diffraction
deemed appropriate by the project manager or principle inves-
Z540.3 American National Standards Institute/National
tigator. The methods defined here are not applicable to glasses
Conference of Standards Laboratories (ANSI/NCSL) Re-
thatformmultipleimmiscibleliquidphases.Immiscibilitymay
quirements for the Calibration of Measuring and Test
be detected in the initial examination of glass during sample
Equipment
preparation (see 9.3). However, immiscibility may not become
apparent until after testing is underway.
3. Terminology
1.3 The values stated in either SI units or inch-pound units
3.1 Definitions:
are to be regarded separately as standard. The values stated in
3.1.1 air quenching—to pour or place a molten glass speci-
each system may not be exact equivalents; therefore, each
men on a surface, for example, a steel plate, and cool it to the
solid state.
ThistestmethodisunderthejurisdictionofASTMCommitteeC26onNuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.13 on Spent Fuel For referenced ASTM standards, visit the ASTM website, www.astm.org, or
and High Level Waste. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved Feb. 1, 2011. Published April 2011. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
C1720–11. the ASTM website.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959. United States
C1720 − 11
3.1.2 anneal—to prevent or remove materials processing 3.1.18 inhomogeneous glass—a glass that is not a single
stresses in glass by controlled cooling from a suitable amorphous phase; a glass that is either phase separated into
temperature, for example, the glass transition temperature (T ) multiple amorphous phases or is crystallized.
g
(modified from Terminology C162).
3.1.19 liquidus temperature—the maximum temperature at
which equilibrium exists between the molten glass and its
3.1.3 annealing—a controlled cooling process for glass
primary crystalline phase.
designed to reduce thermal residual stress to an acceptable
level and, in some cases, modify structure (modified from
3.1.20 melt insoluble—a crystalline, amorphous, or mixed
Terminology C162).
phase material that is not appreciably soluble in molten glass,
for example, noble metals, noble metal oxides.
3.1.4 ASTM Type I water—purified water with a maximum
total matter content including soluble silica of 0.1 g/m,a
3.1.21 mixed waste—waste containing both radioactive and
maximum electrical conductivity of 0.056 µΩ/cm at 25°C and hazardous components regulated by the Atomic Energy Act
a minimum electrical resistivity of 18 MΩ × cm at 25°C (see
(AEA) (3) and the Resource Conservation and Recovery Act
Specification D1193 and Terminology D1129). (RCRA) (4), respectively; the term “radioactive component”
refers to the actual radionuclides dispersed or suspended in the
3.1.5 cleaning glass—glass or flux used to remove high
waste substance (5).
viscosity glass, melt insolubles, or other contamination from
3.1.22 mold—a pattern, hollow form, or matrix for giving a
platinum-ware.
certain shape or form to something in a plastic or molten state.
3.1.6 crystallize—to form or grow, or both, crystals from a
Webster’s
glass melt during heat-treatment or cooling.
3.1.23 nuclear waste glass—a glass composed of glass-
3.1.7 crystallization—the progression in which crystals are
forming additives and radioactive waste.
first nucleated and then grown within a host medium.
3.1.24 observation—the process of obtaining information
Generally, the host may be a gas, liquid, or another crystalline
regarding the presence or absence of an attribute of a test
form. However, in this context, it is assumed that the medium
specimen or of making a reading on a characteristic or
is a glass melt.
dimension of a test specimen (see Terminology E2282).
3.1.8 crystallization front—the boundary between the crys-
3.1.25 phase separated glass—a glass containing more than
talline and crystal-free regions in a test specimen that was
one amorphous phase.
subjected to a temperature gradient heat-treatment.
3.1.26 preferred orientation—when there is a stronger ten-
3.1.9 furnace profiling—the process of determining the
dencyforthecrystallitesinapowderoratexturetobeoriented
actual temperature inside of a furnace at a given location; this
more one way, or one set of ways, than all others. This is
involves different processes for different types of furnaces.
typically due to the crystal structure. IUCr
3.1.10 glass—aninorganicproductoffusionthathascooled
3.1.27 primary phase—the crystalline phase at equilibrium
to a rigid condition without crystallizing (see Terminology
with a glass melt at its liquidus temperature.
C162); a noncrystalline solid or an amorphous solid (2).
3.1.28 radioactive—of or exhibiting radioactivity; a mate-
3.1.11 glass ceramic—solid material, partly crystalline and
rial giving or capable of giving off radiant energy in the form
partly glassy (see Terminology C162).
of particles or rays, for example, α, β, and γ,bythe
disintegration of atomic nuclei; said of certain elements, such
3.1.12 glass sample—the material to be heat-treated or
asradium,thorium,anduraniumandtheirproducts. American
tested by other means.
6 7
Heritage Webster’s
3.1.13 glass specimen—the material resulting from a spe-
3.1.29 Round-Robin—aninterlaboratoryandintralaboratory
cific heat treatment.
testing process to develop the precision and bias of a proce-
3.1.14 glass transition temperature (T )—on heating, the
g
dure.
temperatureatwhichaglasstransformsfromasolidtoaliquid
3.1.30 section—a part separated or removed by cutting; a
material,characterizedbytheonsetofarapidchangeinseveral
slice, for example, representative thin section of the glass
properties, such as thermal expansivity.
specimen. Webster’s
3.1.15 gradient furnace—a furnace in which a known tem-
3.1.31 set of samples—samples tested simultaneously in the
perature gradient is maintained between the two ends.
same oven.
3.1.16 hazardous waste glass—a glass composed of glass
3.1.32 simulated nuclear waste glass—a glass composed of
forming additives and hazardous waste.
glass forming additives with simulants of, or actual chemical
3.1.17 homogeneous glass—a glass that is a single amor- species, or both, in radioactive wastes or in mixed nuclear
phous phase; a glass that is not separated into multiple wastes, or both.
amorphous phases.
Webster’s New Universal Unabridged Dictionary, 1979.
IUCr Online Dictionary of Crystallography, 2011.
3 6
The boldface numbers in parentheses refer to a list of references at the end of American Heritage Dictionary, 1973.
this standard. Webster’s New Twentieth Century Dictionary, 1973.
C1720 − 11
3.1.33 standard—to have the quality of a model, gage, 3.2.22 SEM—scanning electron microscope or scanning
pattern, or type. Webster’s electron microscopy
3.1.34 standardize—to make, cause, adjust, or adapt to fit a 3.2.23 SRM—Standard Reference Material
standard (5); to cause to conform to a given standard, for
3.2.24 T —temperature where glass contains 1 volume%
1%
example, to make standard or uniform. Webster’s
of a crystalline phase
3.1.35 surface tension—a property, due to molecular forces,
3.2.25 T —primary UT measurement above T
a L
by which the surface film of all liquids tends to bring the
3.2.26 T —primary UT measurement below T
c L
contained volume into a form having the least possible area.
3.2.27 T —glass transition temperature
g
3.1.36 test determination—the value of a characteristic or
3.2.28 T —liquidus temperature
dimension of a single test specimen derived from one or more
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observed values (see Terminology E2282).
3.2.29 TLM—transmitted light microscopy
3.1.37 test method—a definitive procedure that produces a
3.2.30 T —melting temperature for glass preparations
M
test result (see Terminology E2282).
3.2.31 UF—uniform temperature furnace
3.1.38 test observation—see observation.
3.2.32 UT—uniform temperature
3.1.39 test result—the value of a characteristic obtained by
3.2.33 WC—tungsten carbide
carrying out a specific test method (see Terminology E2282).
3.2.34 XRD—X-ray diffraction
3.1.40 uniform temperature furnace—afurnaceinwhichthe
temperature is invariant over some defined volume and within
4. Summary of Test Method
some defined variance.
4.1 This procedure describes methods for determining the
3.1.41 vitrification—the process of fusing waste with glass
T of waste or simulated waste glasses.Temperature is defined
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making chemicals at elevated temperatures to form a waste
as the maximum temperature at which equilibrium exists
glass (see Terminology C162).
between the molten glass and its primary crystalline phase. In
3.1.42 volatility—the act of one or more constituents of a
other words, T is the maximum temperature at which a glass
L
solid or liquid mixture to pass into the vapor state.
melt crystallizes. Fig. 1 illustrates an example T for a simple
L
two-component liquid on a binary phase diagram.
3.1.43 waste glass—a glass developed or used for immobi-
lizing radioactive, mixed, or hazardous wastes. 4.1.1 (A) Gradient Temperature Furnace Method (GT)—
This method is similar to Practice C829, “Standard Practices
3.2 Abbreviations:
for Measurement of Liquidus Temperature of Glass by the
3.2.1 AEA—Atomic Energy Act
Gradient Furnace Method,” though it has been modified to
3.2.2 ANSI—American National Standards Institute
meet the specific needs of waste and simulated waste glass
3.2.3 ASTM—American Society for Testing and Materials measurements. The most pronounced differences between this
method and the Practice C829 “boat method” are the sample
3.2.4 CF—crystal fraction extrapolation
preparation and examination procedures.
3.2.5 C —crystal fraction in a sample or specimen
F
4.1.1.1 Samples are loaded into a boat, for example, plati-
3.2.6 EDS—energy dispersive spectrometry
num alloy (Fig. 2) with a tight-fitting lid, and exposed to a
3.2.7 η—viscosity linear temperature gradient in a gradient furnace (Fig. 3) for a
fixedperiodoftime.Thetemperature,asafunctionofdistance,
3.2.8 FWHM—full width of a peak at half maximum
d, along the sample, is determined by its location within the
3.2.9 GF—gradient temperature furnace
GF, and the T is then related to the location of the crystalli-
L
3.2.10 GT—gradient temperature
zation front in the heat-treated specimen (Fig. 4).
4.1.1.2 Following the heat-treatment, the specimen should
3.2.11 HF—hydrofluoric acid
be annealed at or near the glass transition, T , of the glass (this
g
3.2.12 HLW—high-level waste
should be previously measured or estimated) to reduce speci-
3.2.13 ID—identification
men cracking during cutting and polishing.
3.2.14 NBS—National Bureau of Standards 4.1.1.3 The specimen should then be scored or marked to
signifythelocationsonthespecimenlocatedatdifferentdepths
3.2.15 NCSL—National Conference of Standards Laborato-
into the gradient furnace, that is, locations heat-treated at
ries
specific temperatures.
3.2.16 NIST—National Institute for Standards and Technol-
4.1.1.4 If the specimen is optically transparent, it can be
ogy (formerly NBS)
observed with transmitted light (that is, transmitted light
3.2.17 OM—optical microscope or optical microscopy
microscopy or TLM) or reflected light microscopy (RLM) to
look for bulk or surface crystallization, respectively. If the
3.2.18 PDF—powder diffraction file
specimen is not optically transparent or is barely optical
...
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