CHARACTERIZATION, ANALYSIS AND

TESTING OF POLYMERS

Molecular Weight Analysis

Molecular Structure Analysis

Thermal Properties Analysis

Physical Properties Analysis

OUTLINE

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

Gel Permeation Chromatography

A
GPC/SEC
instrument
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

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

As the components exit the

column and the elution
behavior of the sample is
displayed in a graph, or
chromatogram.

Molecular Weight Analysis

Gel Permeation Chromatography

DATA INTERPRETATION

Running from right going to left,

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

ADVANTAGES

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,
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

DISADVANTAGES

Inaccuracy due to the backbone or side-chain structures of

analyte polymers differ significantly from those of the
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

PROCEDURES

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
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
CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

NMR

Molecular Structure Analysis

Fourier Transform Infrared
Spectroscopy
Infrared radiation ( = 2.525 m) is
the
energy
source
in
infrared
spectroscopy
. Frequencies are reported using a
unit called the wavenumber (v~ = 1/
)
Using the wavenumber scale, IR
absorptions occur from 4000 cm1400
cm1.

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

Molecular Structure Analysis

Fourier Transform Infrared
Spectroscopy
SAMPLE PREPARATION

PROCEDURES

SPECTROSCOPIC
MEASUREMENT
DETECTION
IDENTIFICATION

AND

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

Molecular Structure Analysis

Fourier Transform Infrared
Spectroscopy

PROCEDURES

An FTIR spectrum is obtained from

the spectrophotometer at room
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

PROCEDURES

The powder is then pressed at 8

tons for 1 min to produce the disc.
The sample is scanned at a
wavenumber range of 4000 to 400
cm1.

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

DISADVANTAGES

FTIR is simple, fast, and precise.

It requires a very small amount of sample for analysis.
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

DATA INTERPRETATION

the section
where the
polymer changes
in brittle, fragile
property into its
viscous and
rubber state

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS

The peak where

the molecules
are arranged in
very ordered
arrangement

The lowest peak

in the curve
indicating the
phase change
from soft solid
into its liquefied
form

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

ADVANTAGES

TGA helps to identify a complete polymer decomposition

profile by determining weight losses of different molecular
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
TESTING

STRENGTH

IMPACT STRENGTH TESTING

CHARACTERIZATION, ANALYSIS AND TESTING OF POLYMERS