VISCOSITY

MEASUREMENT OF
GLASS

1 Pa-s = 10 P

1 Pa-s = 10 P

EXPERIMENTAL ISSUES
1. elevated temperatures
the materials used in the construction of the apparatus must be
capable of withstanding the required temperatures without
undue deformation under the mechanical or thermal stresses
involved, and without being corroded significantly by the
atmosphere or by the melt.
Your choice:
platinum-rhodium alloys, or else pure ceramics such as
recrystallized alumina.
2. glass melts is highly sensitive to temperature
* provide a furnace chamber with the minimum possible
temperature
variation
throughout
by the sample
* Constancy
to withinthe
1Cvolume
should occupied
be the aim.

3. the measurement of temperature

a. thermocouples so placed as to give the best estimate of the
samples average temperature.
b. Thermocouple wires should enter the furnace cavity long a route
designed to minimize differential thermal gradients and electrical noise
pickup
c. the wires should be sufficiently long to allow proper connection to the
measuring device.
d. thermocouples suffer aging in service to some extent, it is
necessary to calibrate them at intervals against a subsidiary standard
thermocouple reserved for that purpose.
4. Sample preparation and handling
i. avoid clearly visible inhomogeneities or contamination
ii. Excessive heating can cause change of composition due to
volatilization or reaction with the surrounding atmosphere
iii. Grinding a sample to powder while exposed to the usual
laboratory atmosphere could encourage water absorption with
consequent composition change, and is best avoided.

ROTATIONAL VISCOMETERS
range 10 to 105 poise

either the crucible or

the plunger is rotated
and the relationship
between the measured
torque and the
rotational speed gives a
measure of the viscous
drag exerted by the
liquid.

The assembly of crucible and plunger is mounted in a furnace designed to

provide a working volume throughout which the temperature is constant to
better than, say, 1oC
corrosion of the equipment with consequent contamination of the glass sample
is a real possibiliy
Apparatus made from ceramic refractories gave consistently higher
viscosity values. Platinum-rhodium alloys are commonly used

FIBER ELONGATION VISCOMETERS

range 108 to 1013
measuring the rate of extension of a glass fiber suspended vertically in a
suitable furnace

Fiber extension determines the dynamic viscosity of the glass by measuring the
elongation of the sample under uniaxial stress, implicitly assuming that the flow
behavior is Newtonian.
1. Fibers are drawn with diameters between 0.6 and 0.8mm to yield test
samples between 50 and 100mm in length
2. Each end of the sample is fused to a bead about 2mm in diameter to
allow the sample to be suspended in the furnace and coupled to a loading
device.
3. Any surface layer resulting from the drawing process is removed by
etching, and samples with visible imperfections scratches, inclusions, nonconstant diameter must be discarded
4. The sample is mounted as indicated linked by a wire or ceramic coupling
to a thin vitreous silica rod which extends outside the furnace to accept the
weights used for loading

The method is absolute in that the viscosity is calculated directly from

knowledge of the sample geometry, the loading and the measured extension
rate. Provided that the dead weight of the fiber and the effects of surface
tension of the glass may be neglected

the rate of extension of the loaded fiber

dl = l1
l2
where is the dynamic viscosity, m is the mass of the system that loads the fiber,
g is the acceleration due to gravity, l1 is the length of the fiber at the start of a
measurement, l2 is the length of the fiber at the end of the measurement, dt is
the time interval over which the measurement is taken, and A is the surface area
of the fiber specimen (excluding the balls at the ends).

Surface tension () opposes the applied stress (barrier against

increasing
the surface area of the glass when the fiber elongates). So, the
downward
force is a balance between gravitational load and surface tension:
F = (LAg - 2r)
annealing point: elongation rate = 2.5x10-6 l/d2
strain point : rate = 0.0316 x rate at the annealing point

Fiber temperature is monitored by several thermocouples distributed

along the length of that portion of the furnace chamber occupied by
the sample
Measurements may be made with the furnace temperature rising steadily or at
constant temperature
To limit the danger of the fibers necking and producing anomalous results, the
total extension of one particular sample should not exceed 10% over the series
of readings
Littleton softening point, which is a variation on the fiber extension method. Here,
a glass fiber of specified dimensions is subjected to a defined constantly rising
temperature environment and allowed to extend under its own weight. The
measurement depends on establishing the temperature at which
the fiber tip moves downward at a rate of 1mm/minute

BENDING BEAM VISCOMETERS

range 109 to 1015 poise
specimen in the shape of a rod or beam supported near its ends and
loaded midway between the supports.

beams are about 3mm in diameter and the distance between the
supports is about 40mm.

When a load is applied the initial response of the sample is a rapid

elastic deflection, followed by a slower deflection as flow occurs.
Provided the sample is behaving in a Newtonian fashion and the
deflection is sufficiently small, the midpoint deflection rate is
described by

where F is the downward force exerted on the beam, l is the length of

sample between the lower supports, is the dynamic viscosity of the glass,
and Ic is the crosssectional moment of inertia of the beam.
For beams having a rectangular cross section the cross sectional
moment of inertia is given by Ic = h3b/12
where h is the height of the cross section and b is the breadth of the
cross section
When the cross section is circular, the expression becomes Ic = d4/64
where d is the diameter of the cross section.

diameter of the beam is not less than about 10% of the span between the lower
supports and when the total mid-point deflection has not exceeded about 5% of
that span. It is desirable to design the equipment so that the measurement time
is typically in the range 200 to 2000 seconds