SECTION -III

POLYMER PROPERTIES
AND
SINGLE-POINT TESTING

Dr. Yasir Qayyum Gill

Assistant professor
Room No. 116
Department of Polymer and Process Engineering
University of Engineering and Technology, Lahore.
yqgill@gmail.com
Mob. 03337067069 1
 TOPICS
• Analytical tests: Density and specific gravity, water absorption,
moisture analysis, sieve analysis, pourability of plastic
materials
• Material characterization tests: melt flow index (MFI), viscometer
• Mechanical tests: Tensile testing, flexural testing, creep and stress
relaxation, impact testing, hardness
• Thermal properties: Heat deflection temperature, Vicat softening
point, melting point, thermal conductivity, thermal expansion,
brittleness temperature
• Electrical properties: Dielectric strength, dielectric constant and
dissipation factor
• Weathering properties: Accelerated weathering and out-door
weathering
• Optical properties: Refractive index, luminous transmittance and
haze, color, gloss
• Chemical properties: Immersion tests, solvent stress-cracking
resistance, environmental stress-cracking resistance
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• Thermal properties
Heat deflection temperature
Vicat softening point
Melting point
Thermal conductivity
Thermal expansion
Brittleness temperature

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 Heat Deflection Test (ASTM D648, ISO 75)
• The heat deflection or distortion test (HDT), like the Flex test, is a 3-point
bending test.

• This test measures the temperature at which a given sample will deform
a specified amount under a prescribed load.
HDT is normally used to define a material’s temperature
resistance and is therefore especially important to thermoformers
as it serves as a guideline for setting mold temperatures.
• The sample is placed in a three-point bending fixture with supports 101.6
mm (4 in.) apart.

• The force is applied to the thickness side of the sample rather than the
width side, as with flexural tests.

• The assembly is placed in an oil bath.

• The sample is then preloaded with the prescribed load.

• The oil medium is heated at a rate of 2 °C/min.

• On heating the sample will soften and begin to deflect.

When deflection reaches 0.25 mm (0.01 in.) the temperature is recorded

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•
and reported as the material’s heat distortion temperature.
Heat Deflection Test (ASTM D648, ISO 75)

The sample dimensions are 50.8 mm  12.7 mm  6.35 mm.

The specified deflection is 0.25 mm (0.01 in.).
Loads are defined as 0.455 MPa (66 psi) and 1.82 MPa.

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 Vicat Softening (ASTM D1525, ISO 306)
The Vicat softening temperature is the temperature at which a
flat needle will penetrate a sample a total of 1 mm under a
given load and heating rate (50 or 120 °C per minute).

• This test is similar to HDT but its applicability is

limited.
• It is primarily used for specific design or quality control
purposes
• The sample is placed flat in an oil bath.
• Acceptable loads are 10 and 50 N, depending on sample
type. Samples may be heated to 50 °C or 120 °C.
• The needle should have a blunt end with a surface area
of 1 mm2.
The temperature at which the needle penetrates the
•
sample 1 mm is recorded.
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Vicat Softening (ASTM D1525, ISO 306)
• The specimen has a minimum thickness and width of 12.7 mm
(0.50 in.) and 3.05 mm (0.12 in.), respectively.

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 Melting Point Determination
• Two basic methods are used for melting point determination.
• For the first method, a Fisher–Johns melting point apparatus is
most commonly used.
The apparatus consists of a
rheostatically controlled heated
block, a thermometer, and a viewing
magnifier.

• A small pellet or a sliver of the plastic

material to be tested is placed on the
electrically heated block along with a
few drops of silicone oil.
• A cover glass is placed over the The expected accuracy of the test
material and the heat is gradually is within ±5°F of the published
increased until the sample material literature value.
melts or softens enough to deform. This method can be used for both
• The meniscus formed by the oil is crystalline and amorphous
viewed through the magnifier. plastics.
• The temperature at which the
meniscus moves is considered the
melting point. 8
Melting Point Determination
• The second method, known as the Kofler method, is used only
for semicrystalline polymers.

It consists of heating the sample by hot-

stage unit mounted under a microscope
and viewing it between crossed
polarizers.

• When crystalline material melts, the characteristic double refraction

from the crystalline aggregates disappears.
• The point at which the double refraction or birefringence (typically a
rainbow color) completely disappears is taken as the melting point of
the polymer. 9
 Differential Scanning Calorimetry, DSC
• (ASTM D3417, D3418)

• In a differential scanning calorimetry test, the heat that flows into or out of a
sample is measured while the temperature the sample is exposed to is programmed.

• The heat flow is a differential that is proportional to the temperature difference

between the sample and a reference.

• When a sample goes through a transition such as from a solid to a melt, or vice
versa, heat is either absorbed or emitted without a corresponding change in the
temperature of the sample. The measured heat flow will show a peak in the curve.

• A small amount of sample, usually 5 to 10

milligrams is sealed in a conductive pan.

• The pan, along with a reference

pan, is placed inside a well-insulated
oven.

• The temperature in the oven

is programmed to heat or cool in a prescribed
manner And the energy required
to heat or cool the sample is measured.

• At transition points, more or less energy is

required, depending on whether the
transition is endothermic (heat absorbing) or
exothermic (heat emitting). 10
• Figure a is an illustration of an endothermic reaction such as a glass transition, showing the
characteristics of the glass transition state.

• The peak in Fig. b illustrates the exothermic reaction, as the material transitions from an
amorphous to a crystalline state as seen with polyethylene terephthalate.

• The crystalline melting point (Fig. c) is endothermic, that is, energy is absorbed.

• When the material degrades, the transition is endothermic, see Fig. d.

• Crystallization from the melt state is exothermic (Fig. e); therefore, energy is given off. Most
chemical reactions are exothermic.
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 THERMAL CONDUCTIVITY
(ASTM C 177, ISO 8302)
Thermal conductivity is defined as
the rate at which heat is transferred
by conduction through a unit cross- The coefficient of thermal conductivity,
sectional area of a material when a sometimes called K factor, is expressed as
temperature gradient exists the quantity of heat that passes through a
perpendicular to the area. unit cube of the substance in a given unit
of time when the difference in temperature
of the two faces is 1°C.
• Plastics have low thermal conductivity.
• Cellular plastics have the lowest thermal conductivity of all materials,
have gained popularity in the field of thermal insulation.
• The outstanding thermal conductivity of cellular plastics is largely
due to the entrapped gases and not to the polymeric material which
serves merely as an enclosure for entrapment of gases.
• As the density of the cellular plastic decreases, the conductivity also
decreases up to a minimum value and rises again due to increased
convection effects caused by a higher proportion of open cells.
• The quantity of heat flow depends upon the thermal conductivity of
the material and upon the distance the heat must flow. 12
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14
THERMAL EXPANSION (ASTM D696,
D864)
The coefficient of thermal
expansion is defined as
the fractional change in
length or volume of a
material for a unit
change in temperature.

• Plastics tend to expand and contract anywhere from six to nine

times more than materials such as metals.
• This difference in the coefficient of expansion develops internal
stresses and stress concentrations in the polymer, and
premature failures occur.
• Special expansion joints, which generally require the use of
rubber gaskets to overcome the expansion of plastics, are
commonly used.
• The use of a filler such as fiber glass lowers the coefficient of
thermal expansion considerably and brings the value closer to
that of metal and ceramics . 15
Coefficient of Linear Thermal Expansion
• The test method requires the use of a fused quartz-tube
dilatometer, a device for measuring changes in length (dial gauge
or LVDT) and liquid bath to control temperature.
• The test is commenced by mounting a preconditioned specimen,
usually between 2 and 5 in. long, into the dilatometer.
• The dilatometer, along with the measuring device, is then placed
below the liquid level of the bath.
• The temperature of the bath is varied as specified. The change in
length is recorded.
• The coefficient of linear thermal expansion is calculated as follows:
∆𝐿
𝑋=
𝐿𝑜 ∆𝑇
• where X = coefficient of linear thermal expansion/°C;
• ΔL = change in the length of the specimen due to heating or
cooling;
• L0 = length of the specimen at room temperature;
• ΔT = temperature difference (°C) over which the change in the
length of the specimen is measured.
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 BRITTLENESS TEMPERATURE
(ASTM D 746, ISO 974)
Brittleness temperature is defined as
1: the temperature at which plastics and elastomers exhibit brittle
failure under impact conditions.
2: the temperature at which 50 percent of the specimens tested exhibit
brittle failure under specified impact conditions.
• At low temperatures, all plastics tend to become rigid and brittle.

• This happens mainly because, at lower temperatures, the mobility of polymer

chains is greatly reduced.

• For amorphous polymers, brittle failure occurs at a temperature well below glass
transition temperature. The polymer tends to get tougher as it reaches the glass
transition temperature.

• For crystalline polymers, the toughness is mainly dependent on the degree of

crystallinity, which generally creates molecular inflexibility resulting in only
moderate impact strength.

• The size of the crystalline structure formed also has significant effect on the
impact strength of the polymer.

• The larger the crystalline structure, the lower the impact strength.

• The polymers exhibiting ductile failure generally show high plastic deformation
characterized by material stretching and tearing before fracturing.
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 Test Apparatus and Procedures
• The test apparatus consists of a
specimen clamp and a striking
member.

• The specimen clamp is designed so

that it holds the specimen firmly as
a cantilever beam.

• The test apparatus most commonly

used is the motor driven brittleness
temperature tester.

• The tester has a rotating striking

tool that rotates at a constant linear
speed of 6.5± 0.5 ft/sec.

• An insulate refrigerant tank with a

built-in stirrer to circulate the heat
transfer medium is used.

• The stirrer maintains the

temperature equilibrium.

• Any type of heat-transfer medium

can be used as long as it remains
liquid at the test temperature. 18
• The test specimens are usually die punched from a sheet. The specimen dimensions are
1 in. long, 0.25 in. wide, and 0.075 in. thick.

• Specimen conditioning is carried out in accordance with the standard conditioning

procedures.

• To perform the test, the specimens are securely mounted in a specimen clamp. The
entire assembly is then submerged in the refrigerant.

• After immersion for a specified time at the test temperature, the striking tool is rotated
to deliver a single impact blow to the specimens. Each specimen is carefully examined
for failure.

• Failure is defined as the division of a specimen into two or more completely separated
pieces or as any crack in the specimen that is visible to the unaided eye.

• The temperature is raised by uniform increments of 2 or 5°C per test and the test is
repeated. This procedure is followed until both the no-failure and all-failure
temperatures are determined.

• The percentage of failures at each temperature is calculated by using the number of

specimens that failed.

• Brittleness temperature is calculated as follows:

𝑺 𝟏
𝑻𝒃 = 𝑻𝒉 + ∆𝑻 −
𝟏𝟎𝟎 𝟐
• where Tb = brittleness temperature (°C); Th = highest temperature at which failure of all
specimens occur (°C); ΔT = temperature increment (°C); S = sum of the percentage of
breaks at each temperature. 19
• Mechanical tests
Tensile testing
Flexural testing
Creep and stress relaxation
Impact testing
Hardness

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Introduction
• Most important properties
• All service conditions
• Majority of end-use applications involve
some degree of mechanical loading.

In practical applications, The material selection for a

plastics are seldom, if ever, variety of applications is quite
subjected to a single, steady often based on mechanical
deformation without the properties such as
presence of other adverse 1. tensile strength
factors such as environment 2. modulus
and temperature. 3. elongation and
4. impact strength.
Since the published values of the mechanical properties of plastics are
generated from tests conducted in a laboratory under standard test
conditions, the danger of selecting and specifying a material from these
values is obvious.
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 Hardness
Hardness is defined as the resistance of a material to
deformation, particularly permanent deformation, indentation,
or scratching.

• Hardness is purely a relative term

and should not be confused with wear
and abrasion resistance of plastic
materials.

• Polystyrene, for example, has a high

Rockwell hardness value but a poor
abrasion resistance.

• Hardness tests can differentiate the

relative hardness of different grades
of a particular plastic.

• However, it is not valid to compare

the hardness of various plastics
entirely on the basis of one type of
test, since elastic recovery along with
hardness is involved.
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Hardness

23
Hardness
• Plastic materials vary considerably with respect to hardness, one type
of hardness test does not cover the entire range of hardness properties
encountered.

• Two of the most commonly used tests for plastics are

1. the Rockwell and
2. the Durometer hardness tests.

• The Rockwell test is used for relatively hard plastics such as acetals,
nylons, acrylics, and polystyrene.

• For softer materials such as flexible PVC, thermoplastic rubbers, and

polyethylene, Durometer hardness is measured.

• The Barcol hardness test was devised mainly for measuring hardness
of both reinforced and nonreinforced rigid plastics.

• Rockwell Hardness (ASTM D 785)

• Durometer Hardness (ASTM D 2240, ISO 868)
• Barcol Hardness (ASTM D 2583) 24
Hardness Scales

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Durometer Hardness (ASTM D 2240,
ISO 868)
• Relative hardness of soft materials.
• Based on the penetration of a specified indentor forced into the material under
specified conditions.
• The Durometer hardness tester consists of a pressure foot, an indentor, and an
indicating device.
• The indentor is spring loaded and the point of the indentor protrudes through
the hole in the base.
• The test specimens are at least 1/4 in. thick and can either be molded or cut
from a sheet.
• Several thin specimens may be piled to form a 1/4 in.-thick specimen but one-
piece specimens are preferred.
• The durometer hardness is read within 1 sec after the pressure foot is in firm
contact with the specimen.
• Two types of durometers are most commonly used—Type A and Type D.
• The basic difference between the two types is the shape and dimension of the
indentor.
• The hardness numbers derived from either scale are just numbers without any
units.
• The Type A durometer is used with relatively soft material and Type D is used
with slightly harder material. 26
Basic Definitions
Stress. The force applied to produce deformation in a unit area of a test
specimen. Stress is a ratio of applied load to the original cross-sectional
area expressed in lb/in.2.

Strain. The ratio of the elongation to the gauge length of the test
specimen, or simply stated, change in length per unit of the original
length (Δl/l). It is expressed as a dimensionless ratio.

Elongation. The increase in the length of a test specimen produced by a

tensile load.

Yield Point. The first point on the

stress–strain curve at which an
increase in strain occurs without
the increase in stress.

Yield Strength. The stress at

which a material exhibits a
specified limiting deviation from
the proportionality of stress to
strain.
Unless otherwise specified, this
stress will be at the yield point. 27
Basic Definitions
• Proportional Limit. The greatest stress at which a material is
capable of sustaining the applied load without any deviation
from proportionality of stress to strain (Hooke’s Law). This is
expressed in lb/in.2.
• Modulus of Elasticity. The ratio of stress to corresponding
strain below the proportional limit of a material. It is expressed
in F/A, usually lb/in.2 This is also known as Young’s modulus. A
modulus is a measure of material’s stiffness.
• Ultimate Strength. The maximum unit stress a material will
withstand when subjected to an applied load in compression,
tension, or shear. This is expressed in lb/in.2.
• Secant Modulus. The ratio of the total stress to corresponding
strain at any specific point on the stress–strain curve. It is also
expressed in F/A or lb/in.2.

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FLEXURAL PROPERTIES (ASTM D 790,
ISO 178)

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FLEXURAL PROPERTIES (ASTM D 790,
ISO 178)

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IMPACT PROPERTIES

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IMPACT PROPERTIES

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