ASTM C829-81(2005)
(Practice)Standard Practices for Measurement of Liquidus Temperature of Glass by the Gradient Furnace Method
Standard Practices for Measurement of Liquidus Temperature of Glass by the Gradient Furnace Method
SIGNIFICANCE AND USE
These practices are useful for determining the maximum temperature at which crystallization will form in a glass, and a minimum temperature at which a glass can be held, for extended periods of time, without crystal formation and growth.
SCOPE
1.1 These practices cover procedures for determining the liquidus temperature (Note 0) of a glass (NOTE 0) by establishing the boundary temperature for the first crystalline compound, when the glass specimen is held at a specified temperature gradient over its entire length for a period of time necessary to obtain thermal equilibrium between the crystalline and glassy phases. Note 0These terms are defined in Definitions C 162.
1.2 Two methods are included, differing in the type of sample, apparatus, procedure for positioning the sample, and measurement of temperature gradient in the furnace. Both methods have comparable precision. Method B is preferred for very fluid glasses because it minimizes thermal and mechanical mixing effects.
1.2.1 Method Aemploys a trough-type platinum container (tray) in which finely screened glass particles are fused into a thin lath configuration defined by the trough.
1.2.2 Method Bemploys a perforated platinum tray on which larger screened particles are positioned one per hole on the plate and are therefore melted separately from each other.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:C829–81 (Reapproved 2005)
Standard Practices for
Measurement of Liquidus Temperature of Glass by the
Gradient Furnace Method
This standard is issued under the fixed designation C829; 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 2.2 Other Document:
NIST Certificate for Liquidus Temperature, SRM 773
1.1 These practices cover procedures for determining the
liquidus temperature (Note 1) of a glass (Note 1) by establish-
3. Significance and Use
ing the boundary temperature for the first crystalline com-
3.1 Thesepracticesareusefulfordeterminingthemaximum
pound, when the glass specimen is held at a specified tempera-
temperature at which crystallization will form in a glass, and a
ture gradient over its entire length for a period of time
minimum temperature at which a glass can be held, for
necessarytoobtainthermalequilibriumbetweenthecrystalline
extended periods of time, without crystal formation and
and glassy phases.
growth.
NOTE 1—These terms are defined in Definitions C162.
4. Apparatus
1.2 Two methods are included, differing in the type of
4.1 The apparatus for determining the liquidus temperature
sample, apparatus, procedure for positioning the sample, and
shall consist essentially of an electrically heated gradient
measurement of temperature gradient in the furnace. Both
furnace, a device for controlling the furnace temperature,
methods have comparable precision. Method B is preferred for
temperature measuring equipment, and other items listed.
veryfluidglassesbecauseitminimizesthermalandmechanical
4.1.1 Furnace:
mixing effects.
4.1.1.1 MethodA—Horizontaltemperaturegradient,electri-
1.2.1 Method A employs a trough-type platinum container
cally heated furnace, tube type, as illustrated in Fig. 1, Fig. 2,
(tray) in which finely screened glass particles are fused into a
and Fig. 3 and described in A1.1.
thin lath configuration defined by the trough.
4.1.1.2 Method B—An alternative furnace detail employing
1.2.2 Method B employs a perforated platinum tray on
pregrooved Al O cores and dual windings, as illustrated in
which larger screened particles are positioned one per hole on
2 3
Fig. 4 and Fig. 5, and described in A1.2.
the plate and are therefore melted separately from each other.
4.1.1.3 Equivalenttemperaturegradientconditionsmayalso
1.3 This standard does not purport to address all of the
be obtained with furnaces having multiple windings equipped
safety concerns, if any, associated with its use. It is the
with separate power and control, or a tapped winding shunted
responsibility of the user of this standard to establish appro-
with suitable resistances. For high precision, temperature
priate safety and health practices and determine the applica-
gradients in excess of 10°C/cm should be avoided.
bility of regulatory limitations prior to use.
4.1.2 Furnace Temperature Control:
2. Referenced Documents
4.1.2.1 Method A—A suitable temperature controller shall
2.1 ASTM Standards: be provided to maintain a fixed axial temperature distribution
over the length of the furnace.
C162 Terminology of Glass and Glass Products
4.1.2.2 MethodB—Arheostat shall be used to supply power
1 to the outer winding.Aseparate rheostat and controller shall be
These practices are under the jurisdiction of ASTM Committee C14 on Glass
and Glass Products and are the direct responsibility of Subcommittee C14.04 on used for the inner core winding. The basic furnace temperature
Physical and Mechanical Properties.
level is achieved by controlling power to both inner and outer
Current edition approved Sept. 1, 2005. Published November 2005. Originally
core windings. The slope of the gradient is achieved by
approved in 1976. Last previous edition approved in 2000 as C829-81(2000). DOI:
adjusting power input to the outer core winding only. The
10.1520/C0829-81R05.
From NBS Research Paper RP2096, Vol 44, May 1950, by O. H. Grauer and
established temperature gradient is then maintained by control-
E. H. Hamilton, with modification and improvement by K. J. Gajewski, Ford Motor
ling power to the inner core winding only.
Co., Glass Research and Development Office (work unpublished).
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
Standards volume information, refer to the standard’s Document Summary page on Available from National Institute of Standards and Technology (NIST), 100
the ASTM website. Bureau Dr., Stop 3460, Gaithersburg, MD 20899-3460
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C829–81 (2005)
NOTE 1—See A1.1 for further description.
1. Outer shell (stainless steel) 7. Outer protection tube
4 5
2. End plate (Transite) 8. Sil-O-Cel insulation
3. End plate (quartz) 9. Control thermocouple (platinum/rhodium)
4. Stand 10. Heating element wire
5. Inner protection tube 11. Specimen tray
6. Heating element tube
FIG. 1 Liquidus Furnace (Method A)
Material: 26-gage stainless steel
FIG. 2 Liquidus Furnace Shell (Method A)
Millimetres
No. of Turns
A: 6 turns—4.8-mm spacing
B: 13 turns—9.5-mm spacing
C: 5 turns—6.4-mm spacing
D: 24 turns—4.8-mm spacing
FIG. 3 Recommended Liquidus Furnace Winding (Method A)
4.1.3 Temperature-Measuring Equipment— Furnace tem- perforated plate. A solid-state digital thermometer capable of
peratures shall be measured with calibrated Type R or S the measurement accuracy specified may be used for tempera-
thermocouples in conjunction with a calibrated potentiometer, ture measurement.
or other comparable instrumentation, capable of measurements 4.1.4 Microscope—Amicroscopecapableofresolutionofat
within 0.5°C. In addition to control thermocouples, Method A least 5 µm at 1003 is required. A petrographic microscope is
requires an unshielded supported thermocouple for insertion preferredforeaseofcrystalidentificationunderpolarizedlight.
into the furnace chamber to determine temperature gradients, 4.1.5 Additional Equipment for Method A:
and Method B requires five thermocouples mounted in the 4.1.5.1 Laboratory stand to support thermocouple horizon-
specimen support fixture as shown in Fig. 6. An alternative tally (see Fig. 7).
method is to attach (spot weld) the thermocouples to a fixed 4.1.5.2 Trough-type platinum boats (see Fig. 8 and Annex
platinum or platinum alloy plate which supports the tray or A2).
C829–81 (2005)
NOTE 1—See A1.2 for further description.
1. Stainless steel shell 7. Inner heating element tube
2. End plates (Transite ) 8. Perforated platinum tray
3. End seals (Fiberfrax ) 9. Mullite tube of riding device
4. Insulating cover (Fiberfrax ) 10. Alumina spacers
5. Refractory or Sil-O-Cel insulation 11. Controlling thermocouple
6. Outer heating element tube
FIG. 4 Liquidus Furnace (Method B)
FIG. 5 Liquidus Furnace Heating Cores (Method B)
NOTE 1—Hottest thermocouple positioned at forward edge of cut-away section of mullite tube.
FIG. 6 Specimen Support Fixture (Method B)
4.1.5.3 Reshaping die for trough-type boats (see Fig. 8). 4.1.5.8 Graduated measuring rod.
4.1.5.4 Stainlesssteelmortarandpestle.(Thestainlesssteel 4.1.5.9 Stainless steel tongs.
must be magnetic.) 4.1.5.10 Other minor items as described in the text.
4.1.5.5 Sieve, U.S. Standard, No. 20 (850-µm) with receiver 4.1.6 Additional Equipment for Method B:
pan. 4.1.6.1 Riding device for simultaneously holding and posi-
4.1.5.6 Small horseshoe magnet. tioning multiple thermocouples and a perforated platinum tray.
4.1.5.7 Glass vials with covers. This device is provided with leveling screws, a means for
C829–81 (2005)
that their centers are at the predetermined gradient temperature
level corresponding to the liquidus temperature, if known.
Record the location of the trays in the furnace. Either the
single- or the double-core furnace may be used. Modify the
double-core furnace design to accommodate two samples by
providingtworidingdevicesandmeansforinsertionfromboth
ends of the furnace.
6.2 Method B—Use one or two perforated specimen trays
that are free of cracks, pits, or adhering glass. Using the
pointed stainless steel tongs or tweezers, select chips of the
FIG. 7 Thermocouple and Support (Method A)
sample from the No. 12 (1.70-mm) sieve and place one in each
of the drilled holes in each tray. Position a tray in the cut-away
section of the mullite tube on the riding device with the double
lateraladjustment,andapositivestopforpreciselylocatingthe
row of holes forward (toward the hot end), and the forward end
boat and thermocouples within the furnace. The device shown
of the tray indexed precisely over the most forward of the five
in Fig. 9 meets these requirements.
thermocouples against the forward edge of the cut-away
4.1.6.2 Perforated platinum trays (see Fig. 10 and Annex
section, as shown in Fig. 4. An alternative method is to move
A2).
thefurnaceintopositionaroundafixedtray.Onesampleinone
4.1.6.3 Stainless steel mortar and pestle.
tray supported by one riding device may be tested in the
4.1.6.4 Sieves, U.S. Standard, No. 8 (2.36-mm) and No. 12
double-core furnace. Two samples may be tested simulta-
(1.70-mm) with receiver pan.
neously by modifying the furnace design to provide for
4.1.6.5 Glass vials with covers.
insertion from both ends. Carefully feed the riding device
4.1.6.6 Stainless steel pointed tongs.
containing the tray into the furnace until the prepositioned stop
4.1.6.7 Other minor items as shown in illustrations and
plate is contacted. Close the end opening of the furnace around
described in the text.
the riding device with suitable insulation.
5. Preparation of Test Specimens
6.3 Treatment Time—Leave the specimens in the furnace
5.1 Select a mass of glass of approximately 70 g. Break the until equilibrium between the crystal and glassy phases is
sample into pieces of a size that will fit into the mortar. Clean established. The time required is a function of the glass
the sample with acetone, rinse with distilled water, and dry. composition. Twenty-four hours is sufficient for many glasses,
Clean the mortar and pestle, sieve, and magnet in the same butsomeglassesmaytakedaystoreachequilibrium.Complete
manner (Note 2). Crush the sample, using the mortar and crystallization of the specimen indicates insufficient tempera-
pestle, by using a hammer or other suitable means. ture in heat treatment. Total lack of crystallization indicates
insufficient time or excess temperature.
NOTE 2—From this point on, contact with bare hands or other source of
6.4 Temperature Gradient—Determine the temperature gra-
contamination must be avoided.
dients over the lengths of the specimens at the end of the
5.2 Method A—Pour the crushed sample onto a No. 20
heating period just prior to removal from the furnace.
(850-µm) sieve. Retain the material not passing the sieve and
6.4.1 Single-Core Furnace—Establish a temperature profile
repeat the crushing procedure until all the glass has been
over the length of each tray by using a traveling unshielded
reducedtoasizetopassthroughthesieveintothereceiverpan.
Type R or S thermocouple supported horizontally as near the
With the test specimen still in the pan, move the magnet
top of the trays as practical and centered over their widths.
throughout the specimen to remove magnetic fragments that
Start the probe at the hotter end of each tray, toward the center
may have been introduced during crushing. If not to be tested
of the furnace, and make successive temperature readings
immediately, place the specimen in a covered glass vial or
along the tray length at ⁄2-in. (12.7-mm) intervals. Allow the
other suitable container.
thermocouple temperature to stabilize in each position as
5.3 Method B—Pour the crushed sample onto a No. 8
indicated by constancy of temperature over a period of time.
(2.36-mm) sieve fitted over a No. 12 (1.70-mm) sieve and
Record the temperature of each thermocouple position to the
receiver pan. Retain only that part of the sample not passing
nearest 1°C as related to tray position, and plot as in Fig. 11.
throughtheNo.12sieve.ThatglassretainedontheNo.8sieve
6.4.2 Double-Core Furnace—Obtain the temperature pro-
may be recrushed if necessary to increase the No. 12 sieve
file as related to tray position from readings of the five Type R
sample size. Discard the fines passing through to the receiver
or S thermocouples mounted in fixed positions in the riding
pan. If not to be tested immediately, place the specimen in a
device.
covered glass vial or other suitable container.
6.5 Method A:
6. Procedure
6.5.1 Remove the specimens from the furnace, free from the
6.1 Method A—Fill to one-half to three-quarters full two trays, cool, and examine under a microscope for evidence of
specimen trays that are free of cracks, pits, or adhering glass crystallization. If the single-core furnace has been used for the
with the crushed glass specimen. Distribute evenly over the heat treatment, grasp the trays with smooth-faced forceps and
length of each tray. Place the filled trays in the furnace, one on drag outside the furnace onto a heat-resistant flat surface. If the
either side of the maximum temperature point, and locate so double-core furnace has been used, retract the riding device
C829–81 (2005)
FIG. 8 Platinum Tray and Reforming Die (Method A)
NOTE 1—See A1.2 and Fig. 4 for legend.
FIG. 9 Riding Device (Method B)
from the furnace, remove the tray, and place it on the tray. Repeat the inward and outward bending as needed to
heat-resistant flat surface. Immediately upon removal and separate the specimen from the tray. Finally, bend the sides of
before the glass specimen hardens, bend the sidewalls of the the tray to nearly their original shape, and invert the tray to
tray slightly inward at 1-in. (25.4-mm) intervals along its remove the specimen.Tapping the top of the tray on a hard, flat
length. After the specimen has solidified, but is still quite hot, surface is usually required to remove the specimen. Immedi-
bend the sidewalls outward to separate the specimen from the ately return the hot specimen to its original position in the tray
C829–81 (2005)
FIG. 10 Platinum Tray for Holding Glass (Method B)
FIG. 11 Liquidus Furnace Temperature Gradient
to avoid thermal shock breakage and to preserve orientation. prisms with a full-
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