Mohsin Alam 1
Melt Flow Index
Melt Flow Index
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ASTM D 1238

It is defined as the rate of flow of plastic material
through a standard die under the specified
conditions of temp. & pressure. It is expressed in
gms /10 minutes. For different plastic, temp. &
pressures are different.

The amount of thermoplastics resin, measured in
grams, which can be forced through a specified
orifice within ten minutes when subjected to a
specified force.


It helps o distinguish between different grade of

High molecular weight polymer is more resistance
to flow than low molecular wt.

High flow grade material gives better gloss than
low MFI.
Capillary Type
Melt Flow Index Test (MFI)
Definition: Rate of extrusion of a resin in molten condition
under specified temperature and pressure through a specified
size of die in 10 min is defined as melt flow index. The unit of
MFI is g/10min.

The reported melt index values help to distinguish between
the different grades of a polymer.

A high molecular ­weight material is more resistant to flow
than a low molecular­weight material
•It can also be useful for other purposes like studying the
relative thermal effect with respect to barrel residence time on
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Test Methods: ASTM D 1238, ISO 1133, DIN 53735
Test Specimen: The test specimen should be in the form of
powder, granules, strips or film or moulded slugs.
Test Apparatus:
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Test Procedure: Place the thermometer on the hold provided.
The set temperature stabilizes for 5 min. than charge the
material using tool without any air gap. Then apply the load
over the piston. Allow some time for material to melt and
soften and purge the material upto the lower mark of the
piston. Then start the stopwatch and start cutting off the
extrudate depending upon the flow.
Calculations: 30 Sec., 1 min, 3 min, or 6 min intervals and
tabulate the weight of the extrudate.
Flow rate = (m/t) x 600
Where m = mass of extruded, t = time of piston travel for
length L. (sec), 600 = conversion factor to convert in sec.
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Material Temperature Load, Kg
Acetal (Homo & Copolymer) 190 2.16/1.05
PMMA 230 1.2/3.8
ABS 200 and 230 5.0 and 3.8
Cellolose esters 190 and 210 0.325/2.16/21.6
Nylon66 275 0.325
Nylon6 235 1.0/2.16/5.0
PCTFE 265 12.5
PE 125 0.325/2.16
190 0.325/2.16/10/2.16
310 12.5
PC 300 1.2
PP 230 2.16
PS or HIPS 190 5.0
200 5.0
230 1.2/3.8
Polyterepthalate 210 2.16
250 2.16
285 2.16
PPS 315 5.0

Table: Temperature and load for MFI test
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Factors Influencing:
1. Preheat Time. If the cylinder is not preheated for a specified
length of time. This causes the flow rate to vary considerably.
2. Moisture. Moisture in the material, especially a highly
pigmented one, causes bubbles to appear in the extrudate. The
weight of the extrudate is significantly influenced by the
presence of the moisture bubbles.
3. Packing. The sample resin in the cylinder must be packed
properly by Pushing the rod with substantial force to allow the
air entrapped between the resins Pellets to escape. Once the
piston is lowered, the cylinder is sealed of air can escape. This
causes variation in the test results.
4. Volume of Sample. In order to achieve the same response
curve. Repeatedly, the volume of the sample in the cylinder
must be kept constant. Any change in sample volume causes
the heat input from the cylinder to the material significantly
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Physical form of test materials Preferably pellets or performs
(thermoplastics) samples charges – 2.0 – 8 g
Test equipment Extrusion plastometer
Test Condition Dead load on piston varying from polymer
to polymer and Temperature varying from
polymer to polymer
Measuring range Test observation are made between two
specified scribe marks on the piston
Measurement Extrude cut at uniform time intervals are
taken and weighed

Melt flow index as the weight of extrudate
(average in 10 min is calculated and

Summary of test specimen for MFI
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Capillary Rheometer (Viscometer) Test
Definition: The flow rates are measured at a single shear
stress and a shear rate performed at one set of
temperature and geometric conditions.
The capillary rheometer measures apparent viscosities or
melt index over an entire range of shear stresses and
shear rates encountered in compression molding,
calendaring, extrusion, injection molding and other
polymer melt processing operation.
Significance and Use:

The melt flow index measurements takes accounts of
the behavior of polymer at only one point, it is quite
possible for two materials with the same melt index
values to behave completely different at shear rate and
shear stress.
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Molecular characteristics, shear instability, degradation due
to mechanical and thermal effects and evaluation of additives
(processing aids) on processing of polymer can be studied.

Commercially available capillary rheometers are capable of
operating at shear rates up to 25000 S
, which is within the
range of shear rates, encountered in actual processing.
Rheometers up to a shear range 10
have been developed.

Rheological data generated can be very useful in optimizing
processing: conditions and improving product quality.
Material, output and problems related to processing like die
swell, melt fracture etc. can also be studied.

Molecular characteristics, shear instability, degradation due
to mechanic thermal effects and evaluation of additives
(processing aids) on process ability of polymers can be
Md. Mohsin Alam 10

The capillary rheometer is consisting of an electrically
heated cylinder, a pressure ram, temperature controller, timer
and interchangeable capillaries. The plunger can be moved at
a constant velocity that translates to a constant shear rate.
The forces to move the plunger at this speed is recorded
which determines the shear stress.

The sample material is placed in the barrel of the extrusion
assembly, brought to temperature and force out through a
capillary. The forces required moving a load cell detect the
plunger at each speed.
Test Method: ASTM D 3835­93a Test specimen:
The specimen may be in any form that can be introduced into
the bore of the cylinder such as powder, beds, pellets, strips
or film. In case of preformed plugs, any application of heat to
the sample must be kept to a minimum and shall be held
constant for the entire specimen.
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Table-4: Recommended Test Temperature for different thermoplastics
Material Typical Test Temperature °C
Acetal 190
Acrylics 230
Acrylonitrile-butadiene-styrene 200
Cellulose esters 190
Nylon 235 – 275
Polychlorotrifluoroethylene 265
Polyethylene 190
Polycarbonate 300
Polypropylene 230
Polystyrene 190 – 230
Poly (vinyl chloride) 170 – 205
Poly (butylenes terephthalate) 250
Thermoplastic elastomers (Unsaturated) 150 – 210
Thermoplastic elastomers (Saturated) 150 – 210

Test Apparatus:
The capillary rheometer is consisting of an electrically heated
cylinder, a pressure ram, temperature controller, timer and
interchangeable capillaries. The plunger can be moved at a
constant velocity that translates to a constant shear rate. The
forces to move the plunger at this speed be recorded which
determines the shear stress.
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Select test temperature shear rates and shear stress
accordance with material specification

Replace the die and piston in the barrel and allow the
assembled apparatus to reach thermal equilibrium.

The sample material is placed in the barrel of the extrusion
assembly, brought to temperature and force out through a
capillary. The charging of materials should be done within 2

Place the piston movement until the full melt time reached.
Reactivate the piston to start extrusion. After reached steady
state operation, record the force and collect the data. The
data can be collected by

Run a constant rate test (or a constant shear stress test)

Run a multiple rate of multiple stress level test
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( )

Where, γ = shear rate (sec
); Q = flow rate (in
( . )
Shear stress
Pa s
Shear rate

Apparent melt viscosity (poise)
( )
R l
Where, τ = shear stress (psi); F = Load on the ram (lbs); r =
radius of capillary orrifcae (in); R= radius of the barrel (in); l =
length of capillary orriface (in).
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Shear stress versus shear rate and melt viscosity versus
shear rate curves can be plot for the capillary viscometer as
given in Fig
0 1 0 2 0 3 0
4 0
1 0
2 0
3 0
4 0
5 0
6 0
7 0
8 0
9 0
1 0 0
P c f o r f a t e s t s h e a r r a t e
F a t e s t S h e a r R a t e
S l o w e s t S h e a r R a t e
L e n g t h / D i a m e t e r R a t i o

Fig. 12: The true graph for capillary viscometer
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Factors Influencing and Correction factor:
Capillary Calibration: The apparent viscosity varies with the
fourth power of r, it is desirable to know this value within
t0.00762 mm.
Piston friction: The frictional force is negligible compared to
the pressure drop through the capillary. The frictional force
should be subtracted from force reading.
Polymer back flow: The clearance between the plunger and
the barrel may permit a small amount of melt to flow along
with the piston instead of through the capillary. Due to this
the true shear rate to be lower than that calculated from the
piston velocity.
Melt compressibility: As the hydrostatic pressure diminishes
along with the capillary, the fluid density decreases and the
flow rate increases. This results in an increase in shear rate.
If the compressibility of the material is known can be
Md. Mohsin Alam 16
Barrel Pressure Drop: Under isothermal condition, the
pressure drop of Newtonian materials varies:
P L r
¸ _

¸ _
÷ ÷

¸ ,
¸ ,
Determining True Shear Stress: To obtain true shear stress,
perform the following procedure: using a minimum of two
dies having same entrance angle and same diameter (D) of
different capillary length (L). At least one L/D ratio should be
less than 16 and one should be more than 16. Obtain the true
shear stress using the following equation
( ) ( )
4 4
c c
− −
· ·
Where, τ = Ture shear stress, P = Melt pressure
Pc = the intercept between shear rate, D = dia meter
L = Die length, Ab = Cross section area, Fc = Bagley plot
Where L
refers to the rheometer barrel
length and L
to the capillary length.
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Test Specimen Forms – Granules, powder, strips etc.
Important equipment dimensions
Barrel diameter 6.350 – 12.700 t 0.007mm
Capillary (Die)
(i) Diameter is such that barrel to capillary
diameter ratio is between 3 to 15
(ii) length to diameter ratio of capillary
between 4 to 40

(iii) Piston – 0.0254t 0.007mm clearance
between piston land and barrel
Measurements At specified temperature and steady state
operation (constant application of forces;
the forces on piston, material output and its
times are recorded.
Test run Time ~ 10 min
Conclusions Consistency in melt viscosities or viscosity
change with time is calculated and reported.

Summary of test specification for measurement of
rheological properties using capillary rheometer
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Rotational Rheometer
Rotational viscometer consists of two basic parts separated
by the fluid being tested. The parts may be concentric
cylinder (cup and bob), plats, a low angle cone and a plate, or
disk, paddle or rotor in a cylinder. Rotation of one part
against the other produces a shearing action on the fluid. The
torque required to produce a given angular velocities
resulting from a given torque is a measure of the velocity.
Rotational viscometers are more versatile than capillary
viscometers. They can be used with a wide range of materials
since opacity, settling and non­Newtonian behavior do not
cause difficulties.
Cone and Plate Geometry
Parallel Plate Geometry
Co­axial Viscometer
Concentric Cylinder Viscometer
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Cone and Plate Geometry
1. The principle of the cone and plate rheometer is, it
consists of flat circular plate and liner concentric cones
are rotated relative to each other.
2. The test material is placed in the space between the plate
and cone. The major advantage of the instrument is
constant shear rate application on the test fluid,
requirement of small sample size and hence less heat
built up at high shear rates than with a concentric cylinder
3. The disadvantage other than low shear rate range of the
test is the tendency for the development of secondary
flows in the polymer, which affects the accuracy of the
Md. Mohsin Alam 20 Cone and Plate Geometry
For Newtonian fluid, the basic
equations for the cone and plate
rheometer are:
π ω
· ·
R = Radius distance of the sample in cone and plate
α = Angle in radian which cone makes with the flat plate
M = Torque required to rotate the cone relative to the plate of an
angular frequency of ω
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Parallel Plate Geometry
1. Parallel plate geometry consists of a stationary and a
rotating flat circular plate wherein a thin layer of the
sample is placed between them for the test.
2. The gap width can be varied in this viscometer. This is an
advantage when suspension or dispersion with large
particles or with a tendency to fly out the gap.
3. However, the velocity, the shear rate, varies with the
distance from the center of the plate. This makes viscosity
data more difficult to evaluate.
4. Maximum shear rate at plate rim) is given by
γ ·
Where, R is the radius of the plate and
h the distance between the two plats. The velocity given by:
3 ln
1 3
2 ln
M d M
R d
π γ γ
· +
¸ ]
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22 Co­axial Viscometer
It consists of two cylinders, one within the other (cup and bob)
with the sample between them.
2 2
1 1
i o
M kM
ω π ω
¸ _
¸ _
· − ·
¸ ,
¸ ,
Where, M is the torque on the inner cylinder, h is the length
of the inner cylinder, ω is the relative angular velocity of
the cylinder in radius per seconds R
the radius of the inner
cylinder wall, R
the radius of the outer cylinder wall and k
an instrument constant.
The shear rate can be given by
( ) ( )
( )
2 2
2 2
2 /
i o
o i
r R R
γ ·

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Where r is any given radius. The shear stress is given
r h
Co­axial Viscometer
The viscosity of Newtonian liquid
may be determined from the above
equation or from slope of a shear
stress –shear rate plot. Non­
Newtonian fluid gives intercepts and
curves with such plots.
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Concentric Cylinder
1. The test material (fluid state) is placed in the annular
spaces between two cylinders.
2. The cylinder is rotated at a constant speed, while a
transducer measures the torque acting on it.
3. The major advantage of concentric cylinder geometry is
that a nearly constant shear rate is maintained
throughout the entire volume of fluid being tested.
4. This is important in the case of non­Newtonian fluid
since viscosity may be strongly dependent upon the rate
of shear. The relationship of viscosity (η) to the ratio of
‘τ’ and ‘γ’ is shown below:
Where K is the instrument constant.

Md. Mohsin Alam 25
Brookfield Viscometer
The viscosity defines the flow behaviour of plastisol
under low shear. This viscosity relates to the
conditions encountered in pouring, casting, molding
and dipping process. The Brookfield instrument is a
commercially used rotating spindle type viscometer.
The suitability of a dispersion resin for given
application process is dependent upon its viscosity
characteristics. The test standard for viscosity
measurement of plastisols / organosols, epoxy resin
and emulsion etc.
Test Methods:
ASTM D­2393, ASTM D 1824 and ISO 2555.
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1. Select the spindle in middle or upper portion of
viscometer dial at the highest rotational speed to be
used. Insert the spindle approximately at 45° angle.
Move the sample so as to center the spindle, adjust the
depth to the immersion mark.
2. Start the viscometer at its lowest speed. Allow it to run 2
min. record the scale reading during the next rotation.
3. Placing it in a constant temperature bath at the
specified test temperature preconditions the sample.
The proper size spindle is allowed to rotate in the
sample for 30 sec. The instrument is stopped through
the use of a clutch and the reading is taken from the
dial. The test is repeated until a constant reading is
obtained. Record the sample temperature at the
conclusion of viscosity reading. Md. Mohsin Alam 27
Range (cP) Spindle Speed (rpm) Factor
100­400 1 20 5
400­800 1 10 10
800­1600 2 20 20
1600­3200 2 10 40
3200­4000 3 20 50
4000­8000 4 20 100
8000­16000 4 10 200
16000­20000 3 4 250
20000­40000 4 4 500
40000­80000 4 2 1000
80000­160000 5 2 2000
160000­200000 6 4 2500
200000­400000 6 2 5000
400000­800000 7 4 10000
800000­2000000 7 2 20000

Conversion table from centipoises to factor
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Torque Rheometer (ASTM D­2396 )
A torque rheometer measures flow properties of
materials in a miniature form of typical processing
equipment. The capabilities of the sensors used with a
torque rheometer are as follows:
1. (i) An internal mixer with roller blades measures flow
properties of resin
2. (ii) A single­screw extruder with different types of dies
providing a measures of the absolute viscosity of the
3. (iii) A twin­screw extruder, which provides information
on compounding characteristics of resins.
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The ability of PVC granules to accept a plasticizer and
become a dry free flowing powder is related to the
internal pore structure of the resin, resin temperature,
plasticizer temperature and the plasticizer used. The abs
option of plasticizer in PVC can be detect using this
Test Method: ASTM: D2396­94
Test Specimen: The specimen should be in powder form
and plasticizer will be liquid form.
Conditioning: Maintain the PVC and plasticizer at 23 t 1°C
and 50 t 5% relative humidity for all time after mixing and
throughout the period of determination.
Md. Mohsin Alam 30
Test Apparatus:
A torque rheometer is a device consisting of a drive, a
torque (viscosity) measuring system, a sensor, a
temperature control unit and a data recorder. The sensors
available are batch mixers, single/twin­screw extrusion
sensor with post­extrusion line and continuous mixing,
compounding and extrusion sensors with post extrusion
systems. The sigma Mixture is shown in Figure
Md. Mohsin Alam 31

A sample of material to be tested is placed in the
mixing head where it is subjected to shear by means of
two rotating blades.

These methods determine the powder mixing
characteristics of the polyvinyl chloride. The test requires
the use of a torque rheometer measuring head as shown
in fig. The mixture is heated either electrically or oil
circulating heat transfer jacket. In order to obtain
consistency, a standard formulation is established as
PVC resin : 225 g t0.1g
Filler : 15.75 g t0.1g
Basic Lead carbonate : 22.50 g t0.1g
DOP plasticizer : 117.00g t0.1g
Md. Mohsin Alam 32

Because of lot­to­lot variations in the quality of
plasticizer, and basic lead carbonate, it is recommended
that the laboratory maintain a large enough inven­tory of
these additives to establish control standards. A standard
powder­mix curve should also be generated using
standard additives and kept on file for com­parison
Temperature : 88 t 1°C
Mixer Speed : 63 t 1 rpm
Material Weight : 380g t 10g

The sample material is also subjected to high
temperatures. The dynamometer is suspended freely
between two bearing blocks.

The shear rate, measured by the angular velocity of the
rotors, is set according to a tachometer.
Md. Mohsin Alam 33

All ingredients except the plasticizer are weighed into the
container and mix thoroughly. The mixer is preheated and
allowed to run at a specified speed for 30 min to obtain
equilibrium conditions. All dry additives are added to the
mixer and allowed to mix for 5 min. next, the plasticizer is
poured quickly into the mixer and mixing is continued for
10 min. beyond the dry point.

The torque rheometer serves dual purpose of providing
constant torques drive for the extruder screw and
simultaneously recording the torque on the screw. The
instrument responds to the reaction torque encountered by
rotating the extruder screw. The instrument accommodates
a number of interchangeable mixer and extruder

The measuring head rotors encounter a resistance torque
from the test material that causes the dynamometer to
rotate in the opposite direction.

The measuring head is either electrically or oil heated.
Md. Mohsin Alam 34
Case Study for PVC
Test Condition
Speed : 60 rpm, Mix Temperature : 180°C­195°C, Start Temperature :
180°C, Test Time : 55 Min, Sample Weight : 60 gm
Md. Mohsin Alam 35
9.3.2 Flow Properties of Thermosetting Materials
Factor Affecting Flow:
1.    Resin Type: All resin flow differently because of basic
differences in the structure of the polymer e.g. melamine
formaldehyde exhibit longer flow than urea formaldehyde.
2.       Type of filler: The small particle size filler e.g. wood
floor, mica, and minerals creates less turbulence and less
frictional drag during mold filling. The size of the glass fibre
and long fibre can adversely affect the flow.
3.   Storage Time: All resins have a natural tendency to
polymerize in storage, causing partial precure, which reduces
36 Md. Mohsin Alam Cup Flow (ASTM D 731) Definition: The measurement of the molding index
of thermosetting plastics ranging in flow from soft to stiff
by selection of appropriate molding pressure within the
range from 4.1 to 31.9 MPa Significance: This test is specifically designed for
thermosetting molding compounds. This test is primarily
useful for determining the minimum pressure required to
mold a standard cup and the time required to close the
mold fully. The material is molded using a mould of
specified cup­shaped cavity dimensions. The method
provides the guide for evaluating the mold ability of
thermosetting powders. Test Methods: ASTM D 731
37 Md. Mohsin Alam Test Apparatus: The test apparatus shown in
38 Md. Mohsin Alam Procedure:
1.       The rate of flow is sensitive to the condition of the
mold surface. First two reading has to be discarded and after
two successive reading the mold flow can be accepted. The
preferred mold temperature is given below:
Phenolics: 165 t 1 °C
Melamine: 155 t 1 °C
Urea: 150 t 1 °C
Epoxy: 150 t 1 °C
Diallyl phthalates: 150 t 1 °C
Alkyd: 150 t 1 °C
39 Md. Mohsin Alam
# Take the weight and begin the test with proper load to
close the mold to the fin thickness specified for the type of
material. The load can be applied to the mold is as given
Total Load Molding Pressure (MPa)
1112 4.6
1601 6.6
1124 9.0
1686 13.6
2248 18.0
3372 21.2
4496 36.3
11120 45.4
40 Md. Mohsin Alam
# If a 2248 N load applied to make initial cup and required
fin thickness is obtained, the next lower load 1686N is
applied as indicated above. If the mold close to the
required thickness again then next 1124 N load applied. If
the mold then does not close, the ‘molding index’ is close
to 1686 N load.
# The time of flow in seconds shell be measured from that
the hydraulic gage indicates an applied load of 454 kg to
the instant that the fin has reached 0.20 mm I thickness for
material with an izod impact strength of 27 J/m of notch.
41 Md. Mohsin Alam Spiral Flow Definition: The spiral flow of a thermosetting molding
compounds is a measure of the combined characteristics of
fusion under pressure, melt viscosity and gelation rate under
specific condition. Significance: This is a high shear­rate test for
thermoplastics and is widely accepted in the molding industry
and quality control test. The test is performed on an injection­
molding machine under specified condition and using a spiral­
flow mould. Test Method: ASTM D 3123­98
42 Md. Mohsin Alam Procedure
Molding condition:
1. Temperature: A temperature of 150t3°C shall be maintained
on the mold and transfer plunger.
2. Transfer Pressure: The actual pressure applied to the
compounds at the base of the pot shall be 6.90t0.17MPa.
3. Charges Mass: The mass of the compounds shall be
determined empirically so that the thickness of the molded
compounded on the top of the sprue plate of the mold.
4.  Transfer plunger speed: The transfer plunger speed
without load shall be controlled between 25 and 100 mm/s.
5. Pressure Cure Time: sufficient cure time shall be used to
facilitate easy removal of spiral from the mold.
43 Md. Mohsin Alam
MFI of polypropylene (g/10min at 230°C
and 2.16 Kg load
Spiral flow (cm
) at 260°C barrel
temperature, 700 kg/cm
1.7 25.0
3.0 32.0
5.6 36.0
10.0 46.25 Disc Flow Test
Resin Temperature (°C t5°C) Pressure (MPa t10%)
Polyester 120 1.4
Epoxy 160 1.4
Silicones 175 1.4 – 6.9

1 2
( )
w w
Flow percent

1 3
( 4 )
w w
Flow percent

Spiral flow data of polypropylene.
44 Md. Mohsin Alam
9.3.3 For Elastomer
For vulcanisable compound a measure of the time to
the incipient vulcanisation and rate of curing can be
determined for elastomeric material using Mooney
viscosity. Mooney Viscosity Definition:
Mooney viscosity is defined as the shearing torque
resisting rotation of a cylindrical metal disk (or rotor)
embedded in rubber within a cylindrical cavity. Test Method: ASTM D 1646, ISO 289
45 Md. Mohsin Alam Significance:
1.       By this method molecular mass and viscosity can
be determined because rubber is non­newtonian fluid.
2. These mooney viscosities of polymers will normally
relate to how they will be processed. Lower Mooney
viscosity materials (30 to 50) will be used in injection
molding, while higher Mooney products (60 to 80) can
be more highly extended and used in extrusion and
compression molding.
3. The onset for vulcanization can be detected by
increase in viscosity. The curing rate also can be
detected for rubbers.
4. Test Apparatus:
46 Md. Mohsin Alam
Type Rubber Test Temperature °C Running Time (Min)
NBS 388 100t0.5 or 125t0.5 8
100t0.5 4
BIIR, CIIR, IIR 100t0.5 or 125t0.5 8
EPDM, EPM 125t0.5 4
Synthetic Rubber black
master batches
100t0.5 4
Compounded stock
reclaimed material
100t0.5 4 Procedure:
1. Select the rotor to be used and select the test
temperature table given below:
1. Adjust the torque indicator to the zero reading while
viscometer running in the unloaded condition with the
rotor in place.
2. Remove the hot rotor and place the test piece and
replace the viscometer and start the viscometer and
47 Md. Mohsin Alam
Scorch assessed by plasticity test on rubber sample
when sample heated and an increase in stiffness with
heating time was observed (The results shown in Fig.).
Rate of cure is still assessed by vulcanising samples for
various times and following the change in tensile
properties, hardness, set, swelling etc
Determinations of scorch and cure characteristics
48 Md. Mohsin Alam
Md. Mohsin Alam 49

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