Polymer Testing Lab Manual Finalized
Polymer Testing Lab Manual Finalized
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Outcome Based Education Statements
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PSO3: capable of taking up research/ higher education in premier institutes and employment
in polymer industries viz. rubbers, plastics, composites, adhesives, paints, etc.
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CONTENTS
Sl. No. NAME OF THE EXPERIMENT Page No.
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EXPERIMENT – 1
HARDNESS
AIM: To determine Durometer Hardness for different polymers in accordance with ASTM
D 2240.
SCOPE: This test method covers two types of durometers, shore A and D. The procedure
for determining the indentation hardness of homogeneous materials ranging from soft
vulcanized rubber to some rigid plastics.
Type A is used for soften materials and Type D is used for harder materials.
This test method permits hardness measurements on either initial indentation or indentation
after specified periods of time or both.
This test method is based on the penetration of a specific indentor forced into the
material under specific conditions. The indentation hardness is inversely related to the
penetration and is dependent on the elastic modulus and viscoelastic behaviour of the
material. The shape of the indentor and the force applied to it influence the results. This test
is intended for quality control purposes.
APPARATUS:
1. Presser Foot with a hole of diameter between 2.5 and 3.2 mm centered at least 6mm
from any edge of the foot.
2. Indentor formed from hardened steel rod with a diameter between 1.15 and 1.40 to
the shape and dimensions as shown in figure (1) and (2).
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Note: 1) Not to scale
2) All dimensions are in mm
3. Indicating device on which the amount of extension of the point of indentor is read in
terms of graduations ranging from zero for full extension of 2.46 to 2.54 mm to 100
for zero extension obtained by placing presser foot and indentor in firm contact with a
flat piece of glass.
4. Protector for indentor
5. Calibrated spring for applying force to the indentor in accordance with one of the
following equations:
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Force ( N) = 0.4445 HD ----------------------- (1)
Force ( N) = 0.550+0.075 HA ---------------------- (2)
Where,
HD is the hardness reading on a type D durometer
HA is the hardness reading on a Type A durometer
SPECIMEN: The test specimen shall be at least 6 mm in thickness. The lateral dimensions
of the specimen shall be sufficient to permit measurements at least 12 mm from any edge. A
suitable hardness determination cannot be made on a rounded, uneven or rough surface. Plied
pieces may also be used.
PROCEDURE:
• Calibrate the durometer by using standard check gage. If there is any error, note down
the zero correction.
• Place the specimen on a hard, horizontal surface.
• Hold the durometer in a vertical position with point of indentor at least 12 mm from
any edge of the specimen.
• Apply presser foot to the specimen as rapidly as possible without shock
• Apply just sufficient pressure to obtain firm contact between presser foot and
specimen.
• Read the scale within 1 sec the presser foot is in firm contact with the specimen,
unless the maximum reading indicator type Durometer is used. If a reading after a
time interval is specified, hold the presser foot in contact with the specimen without
change in position of pressure and read the scale after the period specified.
Durometers having only a maximum indicator cannot be used to obtain
hardness values at various time intervals, nor in testing vinyl plastics which require
the reading to be taken at 15 s.
When values less than 20 are obtained with type D durometer, the
measurement be made with type A durometer. And when values above 90 are
obtained with type A durometer, the measurements be made with type D durometer.
Values below 10 Shore A are inexact and should not be reported.
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• Make five measurements at different positions on the specimen at least 6 mm apart
and determine the median value or arithmetic mean.
REPORT:
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EXPERIMENT – 2
SCOPE: This test method is the metric counterpart of test method D638. This covers the
determination of tensile properties of plastics of any thickness up to 10mm. however, for
sheeting and film of less than 1 mm thickness test method D882 is preferred.
1. Tensile testing machine or UTM of constant rate of grip separation type comprising of
fixed member, movable member, grips, drive mechanism, load and extension
indicators.
2. Plotter and Micrometer.
TEST SPECIMEN:
The dimensions of dumbbell shaped test specimen for sheet, plate and molded plastics are
given in Table 1 and the speed of testing is given in Table2.
i. Rigid and semirigid plastics: The type M-I is preferred where sufficient material
having thickness of 10 mm or less is available. Type M-III shall be used where
limited material having a thickness of 4 mm or less is available or where a large
number of specimens are to be exposed in a limited space (aging tests etc.). Type M-II
should be used when direct comparisons are required between materials in different
rigidity cases (that is nonrigid and semirigid).
ii. Nonrigid plastics: Type M-I must be used for 4 to 10mm thickness materials and type
M-II shall be used for materials with a thickness of 4mm or less.
iii. Reinforced composites: Type M-I specimen shall be used.
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TABLE 1: SPECIMEN DIMENSIONS (mm)
For Type M-I, having an overall width of 20 mm, an overall length of 215 mm is preferred.
Thickness, T shall be 3±0.4 mm for all types of molded specimens where possible.
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PROCEDURE:
• Measure the width and thickness of specimens with a suitable micrometer to the
nearest 0.02 mm at several points along their narrow sections within the gage
boundaries. Record the minimum values of cross-sectional area so determined.
• Mark gauge length on the specimen.
• Set the grip separation speed of the machine as indicated in Table 2. Fix the specimen
straight between the grips.
• Tighten the grips evenly and firmly to the extent necessary to prevent slippage of the
specimen during test and not to the point where the specimen would be crushed.
• Start the machine and record the load-extension curve
• Record the load and extension at yield and break point.
• Discard specimens that break at some obvious fortuitous flaw or that do not break
between gauge marks.
• Test at least 5 specimens for each sample. Calculate the arithmetic mean of all values
obtained and report it as average value of particular property.
CALCULATION:
Load (N)
1. Tensile stress (MPa) = --------------------------------------------- -----------------
Original minimum cross-sectional area (mm2)
*If the specimen gives a load at yield higher than the load at break, calculate “Percent
Elongation at yield”, otherwise, calculate “Percent Elongation at break”,
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5. Young’s modulus: Calculate the Modulus of Elasticity (Young’s Modulus) by
extending the initial linear portion of the load-extension curve and diving the
difference in stress corresponding to any segment of section on this straight line by
the corresponding difference in strain.
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Sl. Thicknes Width c/s Grip Gage Load Load Extn. Extn. Tensile % % Young’s
No. s (mm) area separation length at at At At strength elongation Elongation modulus
(mm) (mm2) speed (mm) break break yield break (Mpa) at yield at break (Mpa)
(mm/min) (N) (N) (mm) (mm)
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EXPERIMENT-3
SIGNIFICANCE AND USE: The value of this test method is used mainly in the areas
of quality control and materials specification.
SCOPE:
In ASTM D 256, following types of test methods are described:
Test method A(Izod type): The specimen is held as a vertical cantilever beam and is
broken by a single swing of the pendulum with the line of initial contact at a fixed
distance from the specimen clamp and form the centerline of the notch and on the same
face as the notch. The notch produces a stress concentration which promotes a brittle,
rather than a ductile fracture.
Test method B (Charpy type): The specimen is supported as a horizontal simple beam
and is broken by a single swing of the pendulum with the impact line midway between
the supports and directly opposite the notch.
Test method C: is same as method A but includes a determination of the energy expended
in tossing a portion of the specimen. The value reported is called “estimated net izod
impact strength”. Test method C is preferred over method A for materials that have an
izod impact strength of less than 27j/m of notch. For materials higher than this value, the
differences between test methods A and C become unimportant.
Test method D: provides a measure of notch sensitivity of a material. The stress
concentration at the notch increases with decreasing radius. This effect is obtained by
testing specimens with different notch radii.
Test method E: It is similar to method A, except that the specimen is reversed. The striker
of the apparatus impacts the specimen on the face opposite the notch. It is used to give an
indication of the unnotched impact strength of plastics.
In test methods A,C,D and E, the type of failure is recorded as one of the 4 coded
categories defined as follows:
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C complete break
H hinge break: an incomplete break such that one part of the specimen cannot support
itself above the horizontal when the other part is held vertically.
P partial break: an incomplete break that does not meet the definition for a hinge break
but has fractured at least 90% of the distance between the vertex of the notch and the
opposite side.
NB non break: fracture extends less than 90%.
TEST SPECIMEN:
The dimensions and geometry of Izod type test specimen is as shown in figure 3 .
The width shall be between 3.17 and 12.7 mm for molded specimens. For sheet materials
and molded specimens the width shall be the thickness.
22.5±0.5
D
E
PROCEDURE:
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• Before testing the specimen, with excess energy indicating pointer in its normal position
but without specimen, release the pendulum from its normal position and note the
reading as A.
• Measure the width (thickness) of each specimen in the region of the notch with a
micrometer to the nearest of 0.025mm and record it.
• Position the specimen in the apparatus and clamp the vise.
• Release the pendulum and record the excess energy remaining in the pendulum after
breaking the specimen.
• Subtract the correction from the indicated impact reading to obtain the energy delivered
to the specimen.
• Divide the net value so found by the measured width of the specimen to obtain its impact
strength in joules per meter of width.
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EXPERIMENT- 4
AIM: To determine impact resistance of plastic film by measuring the kinetic energy lost by
a free falling dart that passes through the film in accordance with ASTM D 4272
PRINCIPLE:
The velocity of a freely falling dart of specified shape that has passed through a
sheet of plastic film is determined by means of a photoelectric speed trap. The kinetic energy
corresponding to this energy is calculated and compared with the kinetic energy of the same
dart measured without a plastic film. The loss in kinetic energy, suffered by that dart that
ruptured the film is used as an index of impact resistance.
APPARATUS:
The apparatus consists of following components:
Specimen clamp: consists 2 piece annular specimen clamps having inside diameter of 127
mm. the lower stationary half of the clamp shall be mounted rigidly so that the plane of the
specimen is horizontal. The upper or movable part of the clamp shall be designed to maintain
positive and plane contact with the lower clamp when in position. Suitable clamps shall be
provided to hold the film firmly in place during test.
Rubber gasket: of 3.1 mm thick, 127 mm inside diameter and 152 mm outside diameter with
50 to 60 Shore A hardness, may be affixed to the specimen contact surfaces of both clamps.
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Electromagnet: capable of supporting a two kg weight for use in supporting and releasing the
dart assembly. It shall be equipped with a centering device to ensure reproducible drop and a
suitable source of electric power which may be interrupted to energize and de-energize the
electromagnet.
Positioning device: Means shall be provided for positioning the dart at a drop height of 0.660
m from the impinging surface of the dart head to the surface of the test specimen.
Time counter: with a sensitivity to measure in 10-5 s.
Light sensitive speed trap: to activate the time counter device.
Cushioning and shielding device: to avoid damaging the impinging surface of the dart.
Collar: with inside diameter of approximately 7 mm with set screw for securing collar to dart
shaft.
Darts: shall have hemispherical head fitted with a 6.4 mm diameter shaft at least 115 mm
long to accommodate removable incremental weights. Dart shall be 38±0.13 mm in diameter
hemispherical head. Dart weight equals 227 g. Five dart weights each 227 g are provided.
Stem diameter of 9.52 mm has been found satisfactory to resist bending.
Micrometer: accurate to ±0.0025 mm for measuring specimen thickness.
TEST SPECIMENS: The minimum size is 165 by 152.5 mm. the sample shall be of free of
pinholes, wrinkles, folds or any other obvious imperfections.
PROCEDURE:
• Turn on the computer and power supply for the light-sensing unit and allow to warm
up in sufficient time to reach equilibrium.
• Make sure that the dart retrieval drawer (cushioning) is in its place.
• Without prior knowledge of the impact resistance of the film tested, use a 908 g dart
weight at 0.660 m height.
• Position the dart vertically in the holding device. Allow a few seconds for any
vibration to subside.
• Release the dart and record the free fall time. Repeat this for five more times.
Average the five measured times and record it as t1. The time reading of each of the
five free-falls should be within ±30 µs of the average.
• Measure and record the thickness of the film to the nearest 0.0025 mm. Reject
samples that vary by more than 15% from the nominal or a average thickness.
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• Place the specimen over the bottom part of the clamp, making sure that it is
uniformly flat, free of wrinkles, folds etc.
• Place the top part of the clamping ring on the specimen and tighten it with the help of
wing nuts such that the film is firmly held and there is no slippage.
• Position the dart vertically with the electromagnet. Wait a few seconds for any
vibrations to subside.
• Set the counter to zero by pressing the reset button.
• Release the dart by pressing the start button.
• Note down the counter reading for the dart fall and record it as t2.
• Calculate the energy to rupture for the film sample as the average of the five energy
values for the test specimens.
CALCULATION:
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DERIVATION OF FORMULA:
If the time of the free-fall to travel between 2 light sensing elements is t1, the distance
traveled is d, and the velocity entering the speed trap is v1, then:
d = ½ gt12 + v1t1
v1 = (d/t1) – (gt1/2)
if the time of the dart to travel between the sensing elements after breaking the film
is t2 then:
d = ½ gt22 + v2t2
We define the impact energy as the kinetic energy lost in breaking the film as
follows:
m 1 1 g2
= ----- d2 ----- - ----- + ----- (t12- t22)
2 t12 t22 4
RESULT:
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EXPERIMENT - 5
AIM: To determine flexural properties of plastics including high modulus composites and
electrical insulating materials in the form of rectangular bars in accordance with ASTM D
790.
SCOPE: This test method is generally applicable to rigid and semirigid materials. However,
flexural strength cannot be determined for those materials that do not break for that do not
fail in the outer fiber. Two methods are described as follows:
1. Test method I : A 3 point loading system utilizing center loading on a simply
supported beam.
2. Test method II: A 4 point loading system utilizing 2 load points equally spaced from
their adjacent support points, with a distance between load points of either one third
or one half of the support span.
The basic difference between two test methods is in location of the maximum
bending moment and maximum axial fiber stresses. The maximum axial fiber stresses occur
on a line under the loading nose in Test method I and over the area between the loading nose
in the Test method II.
Materials that do not fail at the point of maximum stress under Test method I
should be tested by Test method II.
Either test method can be used with two procedures that follow:
1. Procedure A: is designed principally for materials that break at comparatively small
deflections. The rate of straining at the outer fibers is 0.01 mm/mm-min.
2. Procedure B: is designed particularly for those materials that undergo large deflections
during testing. The strain rate is 0.10 mm/mm-min. for some materials the increase in
strain rate provided under procedure B may induce the specimen to yield or rupture or both
within the required 5% strain limit. Beyond 5% strain, this test methods are not applicable.
Comparative tests may be run according to either test method or procedure,
provided that test method or procedure is found satisfactory for the material being tested.
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SIGNIFICANCE AND USE:
Flexural properties are useful for quality control and specification purposes.
Flexural properties may vary specimen depth, temperature, atmospheric conditions and the
difference in rate of straining as specified in procedures A and B.
APPARATUS:
• Testing machine (UTM) that can be operated at constant rates of crosshead motion
with load and deflection indicating device.
• The loading nose and supports shall have cylindrical surfaces. In order to avoid
excessive indentation or failure due to stress concentration directly under the loading
nose, the radius of the nose and supports shall be at least 3.2 mm.
TEST SPECIMEN:
The specimens may be cut from sheets, plates or molded to the desired finished
dimensions. For flat wise tests the depth of the specimen shall be the thickness of the
material.
The recommended specimen for molding material is 127 by 12.7 by 3.2 mm tested
flatwise and support span to depth ratio (L/D) is 16 to 1. For composite materials, the
dimension of specimen shall be 130 by 13 by 6.4 mm.
PROCEDURE:
Test Method I:
• Measure the width and depth (thickness) of the specimen to the nearest of 0.03 mm
at the center of the support span.
• Determine the support span to be used and set the support span to within 1% of the
determined value. The support span to depth ratio shall be chosen such that failures
occur in the outer fibers, due only to the bending moment. As a general rule, support
span to depth ratios of 16:1 are satisfactory when the ratio of tensile strength to shear
strength is less than 8:1, but the support span to depth ratio must be increased to 32:1
or 40:1 for composite laminates having relatively low shear strength in the plane of
the laminate and relatively high tensile strength parallel to the support span. The
laminate and relatively high tensile strength parallel to the support span. However,
for some highly anisotropic composites shear deformation can significantly influence
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modulus measurements, even at 40:1 ratio. Hence, for these materials 60:1 is
recommended.
• Calculate the rate of crosshead motion as follows:
R = ZL2/6d
Where, R= rate of cross head motion, mm/min,
L= support span, mm
d = depth of beam, mm
Z= rate of straining of the outer fiber, mm. (Z shall be 0.01 for smaller deflection
materials and 0.10 for comparatively larger deflection materials).
• Set the machine for the calculated rate.
• Align the loading nose and support so that the axes of the cylindrical surfaces are
parallel and the loading nose midway between the supports.
• Center the specimen on the supports, with the long axis of the specimen
perpendicular to the loading nose and supports.
• Apply the load to the specimen at the specified crosshead rate.
• Take simultaneous load-deflection data.
• The specimen is deflected until rupture or 5% strain is attained, whichever occurs
first. Terminate the test if the maximum strain in the outer fiber has reached 5%. The
deflection at which this strain occurs is calculated as follows:
D= rL2/6d
Where, D = mid span deflection, mm r = strain (0.05 mm/mm)
L= support span, mm d= depth of specimen, mm.
• At least 5 specimens shall be tested for each sample. Arithmetic mean of all values
obtained shall be calculated to 3 significant figures and reported as the “average
value” for the particular property.
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Sl. Material Depth d Width Support L/d Strain Rate of Load at Load at Deflection Deflection Flexural Flexural % % Flexural
No (mm) b span ratio rate cross head yield break (N) at yield at break strength yield strain Modulus
(mm) length used (mm/ motion (N) (mm) (mm) (MPa) strength at Strain (MPa)
(mm) mm- (mm/min) (MPa) yield at
min) break
1
2
25
3
4
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CALCULATION (FORMULAE):
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EXPERIMENT – 6
ABRASION RESISTANCE OF PLASTICS
TEST SPECIMEN: The test specimen shall be of 50.8 by 76.2 (±0.4) mm in dimension.
PROCEDURE:
• Determine the density of the material to be tested.
• Fill the abrasive container with the grit and adjust the rate of feed to 44±2 g/min.
• Weigh the test specimen to the nearest 0.01 g (W1) and attach to the specimen plate
holder by means of the end clamp provided.
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• Place the weight on the specimen shaft, brush off grit under the specimen.
• Run the machine for 1000 revolutions.
• Remove the mounted specimen, clean with a filtered air blast and reweigh (W2).
• Calculate the abrasion loss. The average of the 6 measurements shall be taken as the
abrasion loss for the material.
OBSERVATION:
1.
2.
3.
4.
5.
CALCULATION:
Calculate the abrasion resistance or the abrasion loss in volume at 1000 revolutions, as
follows:
Where,
W1 = initial weight, g
W2 = weight after abrasion, g
D = density of the material being abraded, g/cm3.
RESULT:
The abrasion loss (volume loss per 1000 revolutions) of ________ material is _______ cc.
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EXPERIMENT – 7
APPARATUS:
Dielectric breakdown voltage tester with following capabilities:
Voltage source: Capable of maintaining the test voltage until dielectric breakdown occurs.
Two electrodes and an output current capacity of 40 mA is usually satisfactory. The power
rating for most tests will vary from 0.5 kVA for testing low testing low capacitance
specimens at voltages up to 100 kV. Equip the voltage source with a circuit-breaking device
that will operate within 3 cycles. The device shall disconnect the voltage-source equipment
from the power service and protect it from overload as a result of specimen breakdown
causing an overload of the testing apparatus. If prolonged current follows breakdown it will
result in unnecessary burning of the test specimens, pitting of the electrodes.
Voltage measurement: A voltmeter must be provided.
TEST SPECIMEN:
When flat-faced electrode is to be used, thin materials such as film, sheet etc. may be used. It
may be convenient to use specimens large enough to permit making more than one test on a
single piece
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PROCEDURE:
1. Switch on the apparatus
2. Measure the thickness of the specimen.
3. Place the specimen on flat surface of the electrode and hold the other electrode on the
specimen.
4. Select the suitable current capacity.
5. By pressing the (red) knob in the top electrode, apply the voltage in any one the
following methods.
1. Method A, short-time test: Apply voltage uniformly to the test electrodes from zero
at one of the following rates* until breakdown occurs.
*Rates: 100,200,500,1000,2000,5000 V/s ±20%
When establishing a rate initially, select a rate that will give an average time to
breakdown of between 10 and 20 s. For many materials a rate of 500 V/s is used. If
the time to breakdown cannot be adhered to, the time shall be made a part of the
report.
2. Method B, step-by step test: Apply voltage to the electrodes at the preferred starting
and in steps and duration until breakdown occurs.
3. Method C, slow rate-of-rise test: Apply voltage to the test electrodes from the
starting voltage and at one of the following rates*
*Rates: 1,2,5,10,12.5,20,25,50,100 V/s ±20%
Unless otherwise specified, use the short-time test.
(Dielectric failure or dielectric breakdown consists of an increase in conductance,
limiting the electric field that can be sustained. This is evidenced during test by abrupt
rupture through the thickness of the specimen, which can be seen and heard, and which
results in a visible puncture and decomposition of the specimen in the breakdown area.
If the breaker is set for too high a current, or it the breaker malfunctions, excessive
burning of the specimen will occur.)
4. Note down the breakdown voltage in Voltmeter.
5. Divide the breakdown voltage by the thickness of the specimen to give dielectric
strength in k V/mm or V/mil at breakdown.
6. Make 5 breakdown for a particular material and report the average value.
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OBSERVATION:
1. A(manual)
2. “
3. “
4. “
5. “
RESULT:
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EXPERIMENT – 8
PRINCIPLE:
Vicat softening point is defined as the temperature at which a flat ended needle of 1 sq.mm
circular cross section will penetrate a thermoplastic specimen to a depth of 1 mm under
specified load and uniform rate of temperature raise.
Data obtained by this method may be used to compare the heat softening qualities of
thermoplastic materials. This test is useful in the areas of quality control, development and
characterization of materials.
Immersion bath: for heat transfer liquid with stirrer and heaters with controller to permit
manual or automatic control of the selected bath temperature raise.
Heat transfer liquid: Liquids such as silicone oils, glycerine, ethylene glycol and mineral oil
shall be used as heat transfer media. The liquid chosen should not affect the material being
tested.
Specimen support: A suitable stand or support for the specimen to be placed in the bath.
Needle: Flat ended, circular cross section of 1 + 0.05 or -0.02 mm2 with flat tip and a length
of 5 to 12.5 mm is used.
Weights: A set of weights of suitable sizes so that the net load on the needle point is equal to
1000+ 40 or – 0g when the apparatus is assembled.
Penetration measurement device: A dial gage or any other device capable of measuring
differences of 0.01 mm or better may be used.
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Temperature measuring device: A thermometer or thermocouple adequate to cover the
range being tested may be used.
TEST SPECIMEN:
Use at least two specimens to test each sample. Flat specimen with minimum thickness of 3
mm and at least 12 mm square is used.
PROCEDURE:
OBSERVATION:
2.
RESULT:
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EXPERIMENT – 9
PRINCIPLE:
A bar of rectangular cross section is tested as a simple beam with the load applied at its center
to give maximum fibre stress of 455 kPa or 1820 kPa. The specimen is immersed in a heat
transfer medium with a means of raising the temperature at 2 ± 0.20C/min. the temperature is
recorded when the test bar has deflection 0.25 mm, which is the HDT of the test specimen.
APPARATUS:
The equipment essentially consists of the following:
Immersion bath: for heat transfer liquid with stirrer and heaters with controller to permit
manual or automatic control of temperature raise at a uniform rate of 2 ± 0.20C/min.
Heat transfer liquid: Liquids such as silicone oil, mineral oil shall be used as heat transfer
media. The liquid chosen should not affect the material being tested.
Specimen supports: A suitable stand with two metal supports for the specimen which is 100
mm apart, allowing load to be applied on top of the specimen vertically and midway between
the supports
Deflection measurement device: A dial gage or any other device capable of measuring
differences of 0.01 mm or better may be used.
Temperature measuring device: A thermometer or thermocouple adequate to cover the range
being tested may be used.
Weights: A set of weights of suitable sizes so that the specimen can be loaded to a maximum
fiber stress of 1820 or 455 ± 2.5 % kPa. The weight of the rod and force exerted by the spring
or dial gage is determined and included as part of the total load.
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P= 2Sbd2/3L and P’ = P/9.80665 …………..(1)
Where,
P = load, N
S = maximum fiber stress in the specimen, N/mm2
b = width of specimen, mm
d = depth of specimen, mm
L= width of span between supports, mm
and P’ = load in kgf, when P is in N
TEST SPECIMEN:
The dimensions of test specimen shall be 127 mm in length, 13 mm in depth by any width
from 3.17 to 13 mm. test at least two specimens from each sample and report the average
value.
PROCEDURE:
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OBSERVATIONS:
RESULT:
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EXPERIMENT-10
AIM: To determine Melt Flow Index for different grades of a Polymer as per the standard
ASTM D1238
APPARATUS REQUIRED:
MFI Tester (Plastometer), Die, Weighing balance, funnel, stop clock, a tool
for cutting off the extruded sample, piston , die retainer plate, screw driver or tester, weights
(1.2,2.16,3.8,5.0,10.0 Kgs) etc.
THEORY:
MFI is the weight in grams of the molten polymer extruded through a standard die in 10
minutes under prescribed conditions of temperature, load and piston position in the barrel.
SIGNIFICANCE:
This test method serves to indicate the uniformity of the flow rate of the polymer as
made by an individual process.
The flow rate obtained with the extrusion plastometer is not a fundamental property of
polymer. It is an empirically defined parameter critically influenced by the physical
properties and molecular weight of the polymer and the conditions of measurement. Since
the rheological characteristics of polymer melts depend on a number of variables, the test
results may not correlate directly with processing behavior.
APPARATUS:
The description of different parts of the apparatus is given below:
Cylinder: The dimensions of the cylinder are as given below:
Diameter : 50.8mm
Length : 162 mm
Hole Diameter : 9.5504± 0.0076 mm
A plate is attached to the bottom of the cylinder to retain the die. A hole in this plat centered
under the die and countersunk from below, allows free passage of the extrudate. This cylinder
is vertically fitted to a support.
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Die: The outside of the steel die is such that it will fall freely to the bottom of the 9.5504mm
diameter hole in the cylinder. The length of the die is 8.000 ± 0.025 mm and the diameter of
the smooth straight bore is 2.0955 ± 0.0051 mm.
Piston: The piston is made of steel with an insulating bushing at the top as a barrier to heat
transfer from the piston to the weight. The piston is scribed with the reference marks 4 mm
apart in such fashion that when the lower mark coincides the top of the cylinder, the bottom
of the piston is 48 mm above the top of the die.
Heater and Temperature controller: The apparatus is provided with electric heater to
maintain the temperature within ± 0.2 0C. A thermocouple with temperature indicator cum
controller is provided. Two temperature setting knobs are provided for coarse and fine setting
of the temperature.
TEST SPECIMEN:
The specimen may be in any form that can be introduced into the bore of the
cylinder for example, powder, granules, pellets etc.
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EXPERINMENTAL PROCEDURE:
1. Select the condition of temperature and load from Table 3 such that flow rates will
fall between 0.15 to 50 g/ 10 min. Ensure that the barrel is cleaned.
2. Set the temperature as given in Table1. Once the temperature is attained, push the die
retainer plate in forward direction and insert the die and piston. The temperature of
the barrel with piston and die in place should have been at the test temperature for
about 15 minutes before the test is begun.
3. Charge the material. The weight of the material is as given in Table 2.
4. Material is compressed by using hand pressure on the piston.
5. 6 to 8 minutes after completing the introduction of the sample, during which time the
temperature should have returned to that selected, the selected load is placed on the
piston.
6. The piston is allowed to descend under gravity pressure or pushed down faster using
hand pressure, until a bubble free extrudate is extruded and the lower mark is 5 to
10mm above the top edge of the cylinder. The extrudate is cut off and discarded.
7. The piston with load is then allowed to descend under gravity. Only when lower mark
has reached the top edge of the cylinder, the time is recorded and the extrudate portion
cut off simultaneously with the cutting tool.
8. Successive cut offs are then collected in order to ensure the extrusion rate at time
intervals depending on the flow rate as given in Table 2.
9. Stop cutting when upper mark of the piston stem reaches the top edge of the cylinder.
Any cut off containing visible air bubble is discarded.
10. By pulling back the retainer plate, the die and remainder of the material in the barrel
has to be removed. Clean the barrel and piston with cloth and die with die cleaning
tool when it is hot.
11. Weigh the extrudate to the nearest 1 mg when cool. If the difference between
maximum and minimum value of the individual weighing exceeds 10% of the
average, the result is discarded and the test is repeated.
39
TABLE 1 STANDARD TEST CONDITIONS
Condition
Sl. No. Material (Temp(0C) /Load(kg)
1 Acetals (Copolymer and Homopolymer) 190/2.16 190/1.05
2 Acrylics 230/1.2 230/3.8
3 Acrylonitrile-butadiene-styrene 200/5.0 230/3.8
4 Cellulose esters 190/0.325 190/2.16
190/21.6 210/2.16
5 Nylon 275/0.325 235/1.0
235/2.16 235/5.0
6 Polycholortrifluorethylene 265/12.5
7 Polyethylene 125/0.325 125/2.16
190/0.325 190/2.16
190/21.6 190/10.0
310/12.5
8 Polycarbonate 300/1.2
9 Polypropylene 230/2.16
10 Polystyrene 200/5.0 230/1.2
230/3.8 190/5.0
11 Polyterphthalate 250/2.16 210/2.16
285/2.16
12 Poly(vinyl acetal) 150/2.16
13 Poly(phenylene sulfide) 315/5.0
14 Thermoplastic Elastomer-ether-ester 190/2.16 220/2.16
230/2.16 240/2.16
40
TABLE 2 STANDARD TEST CONDITIONS, SAMPLE WEIGHT AND TESTING TIME
OBSERVATIONS:
CALCULATION:
600 X M
MFI (g/10min) = ---------------- -------------------------------- (1)
t
Where, M is mass of the extrudate in g and
t is cut off time interval in seconds.
RESULT:
The MFI (T 0C, L kgs) of ________ material is ________ g/10 min.
41
EXPERIMENT – 11
AIM: To determine initial tear resistance of plastic film and sheeting as per the standard
ASTM D1004.
SIGNIFICANCE AND USE:
The data of this test method furnish comparative information for ranking the tearing
resistance of plastic specimens. The resistance to tear of plastic film while partly
dependent upon thickness has no simple correlation with specimen thickness. Hence,
tearing forces measured cannot be normalized over a wide range of specimen thickness.
Data from this test method are comparable only from specimens which vary by no more
than ±10% from the nominal or average thickness of all specimens tested.
APPARATUS:
A power driven machine of constant rate of grip separation type, dial thickness gauge, die
for cutting specimens, grips that minimizes both slippage and uneven stress distribution on
the specimens shall be used.
TEST SPECIMENS: The shape and dimensions of test specimen is as shown below:
101.60
900
19.05
12.7 rad
Rad 25.4
26.95 23.85
3) Tolerance is ± 0.051 mm
42
PROCEDURE:
1. Cut the specimen from film or sheet using the die. The 900 angle should be honed
sharp with no radius or have a minimum practical radius. The cutting edge of the die
shall be kept sharp and free from nicks to avoid leaving ragged edges on the
specimen.
2. Measure the thickness of the specimen to the nearest of 0.0025 mm at several points
and record the average thickness.
3. Set the jaw separation (distance between grips) to 25.4 mm
4. Place the specimen in the grips of the testing machine. Grips lined with thin rubber, or
No. 80 emery cloth may be used.
5. Apply the load at 51 mm/ min rate of grip separation.
6. After complete rupture of the specimen, record the maximum tearing load. At least 10
specimens in case of isotropic and 20 specimens in case of anisotropic material (10
parallel with and 10 normal to the principal axis of anisotropic or maximum
orientation) shall be tested.
Note: Resistance to tear may be expressed in pounds per mile of specimen thickness where
correlation for the particular material being tested has been established. However, it should
be realized that comparison between films of dissimilar thickness may not be valid.
43
EXPERIMENT – 12
THEORY: This test method covers the determination of the force necessary to propagate a
tear in plastic film and thin sheeting (thickness of 1 mm (0.04 in.) or less) by a single-tear
method. The method is not applicable for film or sheeting material where brittle failures
occur during testing.
1. This test method is of value in rating the tear-propagation resistance of various plastic
films and thin sheeting of comparable thickness.
2. This test method shall be used for specification acceptance testing only after it has
been demonstrated that the data for the particular material are acceptably
reproducible.
3. The data obtained by this test method furnish information for ranking the tear-
propagation resistance of plastic films and sheeting of similar composition. Actual use
performance may not necessarily correlate with data from this test method. Sets of
data from specimens of dissimilar thickness are usually not comparable.
A B 50mm
75mm
25mm
44
PROCEDURE:
RESULT:
Maximum tear propagation force of _____ film having thickness ______ mm is ______ N.
45
EXPERIMENT – 13
PRINCIPLE:
Specific gravity and density determinations are performed by “Archimedes principle”. This
principle states that every solid body when immersed in a fluid apparently loses weight by an
amount equal to the fluid it displaces.
Multiply the specific gravity of the sample to the density of the liquid used, to give
density of the sample being tested.
The specific gravity or density of a solid is a property that can be measures conveniently to
identify a material, to follow physical changes in a sample, to indicate degree of uniformity
among different sampling units or to indicate the average density of a large item.
APPARATUS:
1. Analytical balance: A balance with a precision within 0.1 mg and equipped with a
stationary support for the immersion vessel above the balance pan.
2. Holder/sinker: Two numbers of holders for both floating and nonfloating solids.
This shall be corrosion resistant.
3. Immersion vessel: a glass beaker beaker may be used for holding water.
4. Thermometer: A thermometer with an accuracy of ± 10C is required.
46
TEST SPECIMEN: The test specimen shall be single piece of the material weighing
approximately 1 to 50g.
PROCEDURE:
CALCULATION:
W1
1. Specific gravity = --------------------
(W1- W2)
47
EXPERIMENT – 14
48
Gag Load at %
c/s Load at Elongation Tensile 300%
Sl. Thickness Width length 300% elongation
Sample area break at break strength Modulus
No. (mmm) (mm) Lo elongn at
(mm2) (N) (mm) (MPa) (MPa)
(mm) (N) break
1.
2.
3.
4.
49
5.
Distance
between bench Distance between bench
Sl. Gag length Tensile set after break
Sample marks after 10 marks 10 minutes afrer break Tensile set (%)
No. Lo (mm) (%)
minutes (mm)
retraction (mm)
PROCEDURE:
1. Determination of tensile strength, modulus, ultimate elongation:
1. Cut the specimens from the sheet
2. Mark the specimen with bench marker for a distance of 25 ± 0.25 mm
3. Measure the thickness one at the center and one at each end of the reduced section
(with in gage length) of the specimen. If the differences between maximum and
minimum exceeds 0.08 mm discard the specimen.
4. Place the specimen in the grips of the testing machine.
5. Set the grip separation speed to 500 ± 50 mm/min and start the machine.
6. Note the distance between two bench marks.
7. Record the force at specified elongation and at the time of rupture in Table 5.
2. Determination of Tensile set:
1. Place the specimen in the grips of the testing machine.
2. Separate the grips at a uniform rate, requiring 15 s to reach the specified
elongation. Hold it for 10 minutes.
3. Release quickly without allowing it to snap back, and allow it to rest for 10 min.
4. Measure the distance between bench marks and record it in Table 6.
5. For determining set after break, 10 min. after the specimen is broken, fit the two
pieces carefully together so that they are in contact over the full area of the break.
6. Measure the distance between bench marks and record it in Table 6.
CALCULATION:
51
EXPERIMENT – 15
AIM: To determine impact resilience of solid rubber from measurement of the vertical
rebound of a dropped mass in accordance with ASTM D 2632.
PRINCIPLE:
Resilience is determined as the ratio of rebound height to drop height of a metal plunger of
prescribed weight and shape which is allowed to fall on the rubber specimen.
2. This test method is used for development and comparison of materials. It may not
directly relate to end-use performance.
SCOPE:
1. This test method covers the determination of impact resilience of solid rubber from
measurement of the vertical rebound of a dropped mass.
2. This test method is not applicable to the testing of cellular rubbers or coated fabrics.
3. A standard test method for impact resilience and penetration of rubber by a rebound
pendulum is described in Test Method D1054.
APPARATUS:
Rebound resilience tester which includes means for suspending plunger of 28 ± 0.5 g
weight at a given height and a scale for measuring rebound height. The drop height should
be 400 ± 1 mm above the specimen surface and the resilience scale should be marked in 100
equally spaced divisions. The plunger fall and rebound is guided by a vertical rod with
minimum friction.
52
TEST SPECIMEN:
The standard specimen shall have a thickness of 12.5 ± 0.5 mm. the specimen shall be cut
such that, the point of plunger impact is a minimum distance of 14 mm from the edge of the
specimen. (Specimen size : 36 X 36 X 12.5 mm3)
PROCEDURE:
1. Level the instrument and raise the plunger to the top of its guide rod.
2. Position the resilience scale so that its full weight rests upon the specimen. Lock it in
this position.
3. Release the plunger, making sure that it slides freely on its guide.
4. Do not record the first 3 rebounds. Record the height of each of the next 3 rebounds.
Since the resilience scale is divided into 100 parts, the rebound height is equal to the
resilience in percent.
5. Test 3 specimens from each sample and report the average of 3 results.
RESULT:
53
EXPERIMENT – 16
AIM: To determine dynamic fatigue resistance of rubber in accordance with ASTM D 430.
SCOPE:
This test method covers testing procedures that estimate the ability of soft rubber compounds
to resist dynamic fatigue. No exact correlation between these test results and service is given
or implied because of varied nature of service conditions. Data obtained by this test
procedure can be used for the comparative evaluation of rubber compounds.
APPARATUS: There are 3 test methods using the following types of apparatus:
1. Method A- Scott Flexing Machine: is used for test of type I.
2. Method B- De Mattia Flexing Machine: is used for test of type II
3. Method C- E.I. Dupont de Nemours and co. Flexing Machine: is adapted to tests of
either type I and II.
25
75 75
rad 2.39±0.03
6.35±0.13
PROCEDURE:
55
3. Run the test for a known predetermined number of cycles, after which make the
grading comparison. Compare by judging visually the length, depth and number of
cracks. The standard comparison scale shall consist of 11 specimens equally graded
and numbered from No. 0, showing no cracking, to No. 10 which is completely
cracked through.
RESULT:
56
EXPERIMENT – 17
AIM: To determine crack growth of vulcanized rubber subjected to repeated bend flexing as
per the standard ASTM D 813.
SCOPE:
This test is particularly applicable for synthetic rubber compounds which resist the initiation
of cracking due to flexing when tested in De Mattia type machine (ASTM D 430) and the
small cuts or tears in service may propagate rapidly. Because of this characteristic of
synthetic compounds particularly those of SBR type, this method in which the specimens are
artificially punctured in the flex area and the cut length is measured at frequent intervals to
determine the cut growth rate.
APPARATUS:
De Mattia Flexing Machine with specifications as described in test method ASTM D 430,
measuring scale, piercing tool to make artificial crack at the center of groove of the specimen.
TEST SPECIMEN: The shape and dimensions of test specimen is shown in fig. (6).
PROCEDURE:
1. Make an artificial cut on the center of the groove of test specimen. The piercing tool
shall be maintained perpendicular to both the transverse and longitudinal axes and the
cut accomplished by a single insertion and withdrawal of the tool. The dimensions of
the tool are given in the standard. While cutting, the tool shall completely penetrate
the specimen and project at least 3.2 mm through the specimen. The initial cut
produced by the punctured spear is 2 ± 0.1 mm in width.
2. Clamp the specimens in the grips of the machine such that the circular groove shall
become outer surface. The positions of stationary and movable grip shall be adjusted
so that during each stroke of the machine the grips approach each other to a distance
of 19.0 ± 0.1 mm and separate at a distance of 75.9 + 0.3 or -0.0mm.
3. Start the machine and record the time. Stop the machine at 1000 cycle periods (the
number of flexing cycles is calculated by multiplying the observed time in minutes by
the machine rate (ie.300 cpm).
57
4. Measure the length of the developed crack to the nearest 0.3 mm with an accurate
scale.
5. Continue the test until a crack at least 12.5 mm in length developed. Continuation to
break may be desirable for aged specimens or when operating at elevated
temperatures.
RESULT:
The crack growth data may be reported in any one of following 3 ways:
1. As the number of cycles required to reach the specified crack growth length for
example, from 2 to 20mm or,
2. As the average rate of crack growth over the entire test period, or,
3. As the rate of cracking in millimeters per kilocycles during a portion of the test for
example, (a) 2 to 4mm (b) 4 to 8 mm or (c) 8 to 12mm.
58
EXPERIMENT – 18
TEAR RESISTANCE OF RUBBER
AIM: To determine Tear Resistance of vulcanized rubber as per the standard ASTM D 624.
SCOPE
1. This test method describes procedures for measuring a property of conventional
vulcanized rubber and thermoplastic elastomers called tear strength.
2. The values stated in SI units are to be regarded as the standard. The values given in
parentheses are for information only.
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 and health practices and determine the applicability of regulatory limitations
prior to use.
APPARATUS: UTM, dial thickness gauge, die for cutting test specimen, razor blade
etc.
TEST SPECIMEN:
There are 3 specimen shapes as follows:
1. Die A: A razor nicked crescent specimen
2. Die B: A razor nicked crescent specimen with tab ends (ISO/34 configuration)
3. Die C: An unnicked 900 angle specimen.
The thickness of the specimen should not fall outside the limits of 1.3 to 3.2 mm.
59
PROCEDURE:
1. Cut the specimen from the sheet such that the grain direction is long way of the
specimen.
2. Make a single slit or nick at the center of the inner concave edge (for Die A and B) of
the specimen. The cutting shall be done by a safety razor blade clamped in a holder
with the extension of the blade beyond the surface of the holder regulated by a depth
gage to produce a slit of 0.50 ± 0.05 mm in depth. Die C specimens are not nicked.
3. Measure the thickness in three places across the width of the specimen, near its center
and record the median measurement.
4. Clamp the specimen in the grips of the testing machine and align with the center of
the ends.
5. Separate the grips at a rate of 500 ± 50 mm/min.
6. Record the highest force and calculate the tear strength (resistance) as follows:
Sl. No. Sample Thickness (mm) Maximum load (N) Tear Strength (N/mm)
1
2
3
60
EXPERIMENT – 19
SPECIFIC GRAVITY OF RUBBER
AIM: To determine specific gravity of rubbers using direct reading specific gravity balance.
1. With needle and sinker in position slide the 2 weights to the bottom of the long arm.
2. Adjust the base level screw until pointer reads 1.00
3. Place the 3 calibration weights on the needle above sinker.
4. Adjust the sliding weights on long arm until the pointer is exactly on mark ‘A’,
5. Remove one weight from the sinker. Now the pointer should read 3.00 ± 0.02.
6. Remove the second weight from the sinker. The pointer should now read 1.50 ± 0.005
PROCEDURE:
1. Make sure that the pointer is moving freely in its pivots screw. The screw should be
tightened only to the extent of free movement of pointer.
2. Fill the glass beaker with distilled water and keep it on the platform and see that the
lower needle is fully immersed in water.
3. Adjust the sliding weights of long arm until the pointer reads 1.00 accurately.
4. Remove the beaker from the platform.
5. Fix the sample in the needle.
6. Adjust the sliding weight on the long arm until the pointer coincides accurately with
the mark ‘A’ on the dial scale.
7. Raise the beam to lift the test piece and place the beaker of distilled water on the
platform.
8. Raise the platform and beaker until the test piece is immersed fully in water without
bubbles. Ensure that the specimen does not touch the slides or bottom of the beaker
and that the sinker does not make contact with the water during test.
9. Read the scale which directly gives the specific gravity of sample being tested.
RESULT: Specific gravity of ________ rubber sample is ________
61
EXPERIMENT- 20
APPARATUS:
Du Pont Croydon Abrasion Tester which carries a standard abrasive disc mounted on a
vertical flat wheel which is rotated at a speed of 35±5 rpm about the axis of the lever arm by
means of an electric motor. The torque in the lever arm is balanced by means of a weight
bucket. A lever arm with specimen holders is mounted on a rod. A wire with a known weight
for holding the specimens against the abrasive disc is attached to the far end of the rod.
PROCEDURE:
1. Weigh the test specimen and record its weight as W1. At a time 2 specimens from the
same sample shall be tested.
2. Fix the specimens in its holders.
3. Press the lever arm and rod such that the specimens are in firm contact with abrasive
disc. Suspend the weight to the far end of the rod which passes through a pully for
holding the specimens in firm contact with the disc during test.
4. Start the machine. The abrasive surface is continuously cleaned by means of air jets.
5. After specified number of revolutions or time, stop the machine.
6. Weigh the sample and record the weight as W2.
7. Determined the density of sample in g/cc and record it.
CALCULATION: Calculate and report the Abrasion resistance of given rubber sample in
any of the following ways:
62
*Since all tests are comparative, a standard compound is included so that the result can be
expressed as Abrasion Resistance Index i.e. Abrasion resistance relative to that of a standard
compound.
OBSERVATION:
63
EXPERIMENT- 21
FLAMMABILITY TEST
AIM: To determine Rate of Burning and/or Extent and Time of Burning of Plastics in a
Horizontal Position according to ASTMD 635
SCOPE:
1. This fire-test-response test method covers a small-scale laboratory screening procedure
for comparing the relative linear rate of burning or extent and time of burning, or both, of
plastics in the form of bars, molded or cut from sheets, plates, or panels, and tested in the
horizontal position.
2. This standard is used to measure and describe the response of materials, products, or
assemblies to heat and flame under controlled conditions, but does not by itself
incorporate all factors required for fire hazards or fire risk assessment of materials,
products, or assemblies under actual fire conditions.
APPARATUS
Test Chamber, enclosed laboratory hood, or chamber free of induced or forced draft
during test, having an inside volume of at least 0.5 m3. An enclosed laboratory hood with
a heat-resistant glass window for observing the test and an exhaust fan for removing the
64
products of combustion after the tests is recommended. The atmosphere in and around the
test chamber shall be maintained between 15 to 35°C and 45 to 75 % relative humidity.
Laboratory Burner, constructed in accordance with Specification D 5025.
Gas Supply, a supply of technical-grade methane gas with suitable regulator and meter
for uniform gas flow. Natural gas mixtures having an energy density of approximately
37MJ/m3 have been found to provide similar results.
Timing Device, accurate to 0.5 s.
Scale graduated in millimeters.
Conditioning Room or Chamber
Flexible Specimen Support Fixture, used to facilitate the testing of specimens that
sag and touch the wire gauze.
TEST SPECIMEN:
65
12.7mm. Ensure that the edges are smooth and the radii of the corners do not exceed
1.2mm.
Condition the specimens for atleast 48 hrs at temperature 23 ±2⁰cand relative humidity
of 50±5 percent. Each specimen is marked across its width with two lines , 25.4mm and
101.6mm from one end.
SPECIMEN:
25.4mm
12.7mm
76.2mm
127mm
PROCEDURE:
Where t is time in seconds for the flame to travel 25.4mm mark to 101.6mm mark
66
QUESTION BANK
1. Define the following
a) Hardness
b) Tensile strength
c) Flexural strength
d) Abrasion resistance
e) Resilience
f) Tear strength
g) Impact strength
h) VSP
i) HDT
j) MFI
k) Dielectric strength
l) Specific gravity and density
m) Conditioning
n) Flame resistance.
2. Write ASTM standard for the following tests
a) Hardness
b) Tensile strength
c) Flexural strength
d) Abrasion resistance
e) Resilience
f) Tear strength
g) Impact strength
h) VSP
i) HDT
j) MFI
k) Dielectric strength
l) Specific gravity and density
m) Flame resistance.
67
3. Effect of different test variables on results of
a) Hardness
b) Tensile properties
c) Flexural properties
d) Abrasion resistance
e) Resilience
f) Tear strength
g) Impact strength
h) VSP
i) HDT
j) MFI
k) Dielectric strength
l) Specific gravity and density
m) Flame resistance testing.
4. Test specimen preparation methods for different tests
5. Advantages and disadvantages of the specimen preparation techniques
6. Different methods of conditioning
7. Samples dimensions and shape of the samples for different tests for ex: mechanical ,
thermal, electrical and other physical properties
8. Formulae used for calculations and units used for expressing test results for the
properties mentioned in 3.
9. Scope and Significance of the different test methods.
10. Behavior of plastic and rubber material on tensile, flexural and compression load.
11. Different types of Flame resistance methods
68
Work sheet
69
Work sheet
70