CHARACTERIZATION, ANALYSIS AND

TESTING OF POLYMERS
Molecular Weight Analysis

Molecular Structure Analysis

OUTLINE
Thermal Properties Analysis

Physical Properties Analysis

 Molecular Weight Analysis

Melt Flow Index Test

Gel Permeation Chromatography

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Molecular Weight Analysis
Gel Permeation Chromatography

a mode of liquid chromatography in

which the components of a mixture
are separated on the basis of size.

GPC-SEC is mainly used for

samples with a molecular weight
above 2000 although it is also in
use for oligomer separations.

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Molecular Weight Analysis
A GPC/SEC instrument
Gel Permeation Chromatography consists of a pump to push
the solvent through the
instrument
The polymer sample is first
dissolved in a solvent
polymer molecules are
then introduced into the
mobile phase and flow into
the GPC/SEC column
As the components exit the
column and the elution
behavior of the sample is
displayed in a graph, or
CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS
chromatogram.
 Molecular Weight Analysis
Gel Permeation Chromatography
• Running from right going to left,
DATA INTERPRETATION

the molecular weight of the sample

is increasing.
• Detecting the higher peaks in the
right side indicate a low molecular
weight.
• The lower peak would rather mean
that there is a minimal amount of
sample containing higher molecular
weight when compared to the
highest peak.

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Molecular Weight Analysis
Gel Permeation Chromatography
• It has relatively low cost, simplicity, and the ability to provide
accurate, reliable information in a very short time.
• It detects not only resin-based molecules such as polymers,
ADVANTAGES

oligomers, and monomers, but also most additives used in

plastic compounds and even low-level impurities.
• Batch-to-batch uniformity can be checked quickly as a means
of quality assurance.
• Differences in molecular-weight distributions, peak shapes,
shifts, and tailing are readily observable.
• Comparisons of additives and other lower-molecular-weight
species are straightforward.

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Molecular Weight Analysis
Gel Permeation Chromatography
• Inaccuracy due to the backbone or side-chain structures of
analyte polymers differ significantly from those of the
DISADVANTAGES

polymer size standards.

• GPC data can only be acquired for soluble components,
• Inherent shortcomings of the present organic column
packings for GPC are solvent selectivity, temperature
sensitivity, and mechanical instability
• GPC is not efficient for separating polymer molecules
according to molecular characteristics that do not have a
simple correlation with chain size,
• It is useful only for an estimation of molar mass;

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Molecular Weight Analysis
Melt Flow Index Test
a measure of the ease of flow of the
melt of a thermoplastic polymer
It is defined as the mass of
polymer, in grams, flowing in ten
minutes through a capillary of a
specific diameter and length by
a pressure applied via
prescribed alternative
gravimetric weights for
alternative prescribed
temperatures.
CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS
 Molecular Weight Analysis
Melt Flow Index
1. A small amount of the polymer sample is taken in the
specially designed MFI apparatus.
2. The material is packed properly inside the barrel
3. A piston is introduced which acts as the medium that causes
PROCEDURES

extrusion The sample is preheated for a specified amount of

time.
4. After the preheating a specified weight is introduced onto
the piston
5. The weight exerts a force on the molten polymer and it
immediately starts flowing through the die.
6. A sample of the melt is taken after the desired period of time
and is weighed accurately.
CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS
 Molecular Weight Analysis
Melt Flow Index Test
LIMITATIONS
The sample must be “meltable” in
order to be evaluated using the MFI
instrument. of the instrument.

To charge the instrument with

the sample, the sample has to
have a particle size that is on
the order of about 3-mm or less

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Molecular Weight Analysis

FTIR NMR

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Molecular Structure Analysis
Fourier Transform Infrared
Spectroscopy
Infrared radiation (λ = 2.5–25 µm) is
the energy source in infrared
spectroscopy
. Frequencies are reported using a
unit called the wavenumber (v~ = 1/
λ)
Using the wavenumber scale, IR
absorptions occur from 4000 cm–1–400
cm–1.

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Molecular Structure Analysis
Fourier Transform Infrared
Spectroscopy

SAMPLE PREPARATION
PROCEDURES

SPECTROSCOPIC
MEASUREMENT

DETECTION AND
IDENTIFICATION

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Molecular Structure Analysis
Fourier Transform Infrared
Spectroscopy

An FTIR spectrum is obtained from

the spectrophotometer at room
PROCEDURES

temperature using the potassium

bromide (KBr) disc method

the sample is dried and ground

with KBr powder until they are in a
well-mixed, powdered form.

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Molecular Structure Analysis
Fourier Transform Infrared
Spectroscopy

The powder is then pressed at 8

PROCEDURES

tons for 1 min to produce the disc.

The sample is scanned at a

wavenumber range of 4000 to 400
cm−1.

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Molecular Structure Analysis
Fourier Transform Infrared
Spectroscopy
ADVANTAGES

• FTIR frequently suffers from problems associated with sample

preparation.
• Reflectance methods require suitable samples.
• Transmission methods demand samples with sufficient
transparency to allow the penetration of IR beams.

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Molecular Structure Analysis
Fourier Transform Infrared
Spectroscopy
• FTIR is simple, fast, and precise.
• It requires a very small amount of sample for analysis.
DISADVANTAGES

• a valuable tool for in-situ monitoring of chemical reactions.

• useful for determining the functional groups present in a
compound
• most useful for obtaining qualitative information regarding
the average oxidation rate
• infrared radiation absorbs essentially similar frequencies and
intensities called group frequencies

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Molecular Structure Analysis
Nuclear Magnetic Resonance

It determines the physical and

chemical properties of atoms or
the molecules in which they are
contained
It relies on the phenomenon of
nuclear magnetic resonance and
can provide detailed information
about the structure, dynamics,
reaction state, and chemical
environment of molecules

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Thermal Properties Analysis
Differential Scanning Calorimetry

a thermoanalytical
technique in which the
difference in the amount of
heat required to increase
the temperature of a
sample and reference is
measured as a function of
temperature.

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Thermal Properties Analysis
Differential Scanning Calorimetry
the temperature program
for a DSC analysis is
designed such that the
sample holder temperature
increases linearly as a
function of time.
reference sample should
have a well-defined heat
capacity over the range of
temperatures to be scanned
CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS
 Thermal Properties Analysis
Differential Scanning Calorimetry
the sample undergoes a physical
transformation such as phase
transitions, more or less heat
will need to flow to it than the
reference to maintain both at
the same temperature.
It is due to the absorption of
heat by the sample as it
undergoes the endothermic
phase transition from solid to
liquid
CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS
 Thermal Properties Analysis
DSC The peak where
the molecules
are arranged in
very ordered
DATA INTERPRETATION

arrangement

the section The lowest peak

where the in the curve
polymer changes indicating the
in brittle, fragile phase change
property into its from soft solid
viscous and into its liquefied
rubber state form

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Thermal Properties Analysis
Thermogravimetric Analysis
Thermogravimetric analysis
(TGA) is a method of thermal
analysis in which changes in
physical and chemical
properties of materials are
measured as a function of
increasing temperature or
function of time.

TGA can be used to evaluate the

thermal stability of a material

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Thermal Properties Analysis
TGA

• TGA helps to identify a complete polymer decomposition

profile by determining weight losses of different molecular
ADVANTAGES

fragments separating out

• Polymer products based on the different crystallization
behaviors of the various species present can be identified.
• The thermogravimetric technique has a number of
advantages over the more conventional isothermal method of
obtaining kinetic parameters, such as energy of activation
and order of reaction.

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Thermal Properties Analysis
TGA
DISADVANTAGES

• It is a sample-destructive technique.

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Thermal Properties Analysis
Dynamic Mechanical Testing

• A technique used to study and

characterize materials.
• It useful for studying the
viscoelastic behavior of
polymers.
• A sinusoidal stress is applied
and the strain in the material
is measured, allowing one to
determine the complex
modulus.

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Thermal Properties Analysis
Dynamic Mechanical Testing
• The temperature of the
sample or the frequency of the
stress are often varied,
leading to variations in the
complex modulus;
• This approach can be used to
locate the glass transition
temperature of the material,
as well as to identify
transitions corresponding to
other molecular motions.

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

 Physical Properties Analysis

TENSILE STRENGTH TESTING

COMPRESSIVE STRENGTH
TESTING

IMPACT STRENGTH TESTING

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS