Lesson 3: Characterization, Analysis, Testing Flashcards
is the analytical branch of polymer science.
Polymer characterization
is a technique used to determine the molecular properties, structure, and behavior of polymers.
Polymer characterization
➢Characterization techniques are typically used to determine
molecular mass, molecular structure, morphology,
thermal properties, and mechanical properties.
The ____ of a polymer differs from typical molecules, in
that polymerization reactions produce a distribution of molecular
weights and shapes.
molecular mass
The distribution of molecular masses can be summarized by the
number average molecular weight, weight average molecular weight,
and polydispersity.
➢There are four molecular weight
averages in common use:
number-average molecular
weight, Mn; the weight-average
molecular weight, Mw; the z-average molecular weight, Mz; and the viscosity-average molecular weight, Mv
If all species in a polymer sample have the same molecular weight, the polymer is
monodisperse
➢The ratio Mw/Mn is called the ____ is commonly used as a simple measure of the polydispersity of the polymer sample.
polydispersity index (PDI)
➢The molecular weight of polymers can be determined by a
number of physical and chemical methods.
- end group analysis
- measurement of colligative properties
- light scattering
- Ultracentrifugation
- dilute solution viscosity
- gel permeation chromatography (GPC).
➢The ____ is a chemical method use for calculating the number-average molecular weight of polymer samples whose molecules contain reactive functional groups at one end or both ends of the molecule.
end-group analysis
➢This method is limited to the determination of polymers with a molecular weight of less than about 20,000.
End-group Analysis
Method of _____ analysis
✓Titrimetric method
✓Nuclear magnetic resonance (NMR)
✓mass spectrometry
✓vibrational spectrometry, like infrared and raman spectroscopy.
End grp analysis
➢End-group analysis is not applicable to
polymers that lack reactive or easily detectable end-groups.
high molecular weights
➢Properties of solutions that depend on the number of molecules present and not on the kind of molecules are called
colligative properties
colligative properties include
boiling point elevation, freezing point depression, and osmotic pressure.
Boiling Point Elevation or
Ebulliometry
In applying this method, the boiling point of a solution of known concentration is compared to that of the solvent at the same pressure
Boiling Point Elevation
✓Boiling point of the solution is ____ than the pure solvent. This phenomenon is used to determine the molecular weight of polymers
higher
_____, like end-group analysis, is
limited to low-molecular-weight polymers.
Ebulliometry
It works by analyzing the melting behavior of a substance as it is frozen. By measuring the time it takes for a specific substance to melt at a certain temperature, its molecular weight can be calculated.
Cryoscopy (Freezing Point Depression)
Like ebulliometry, the cryoscopic method is also limited to relatively low-molecular-weight polymers
with Mn up to ___.
50,000
____ is the most important among all colligative properties for the determination of molecular weights of synthetic polymers.
Osmotic pressure
____ is a technique for the determination of molecular masses of polymers by means of osmosis. The phenomenon of osmosis describes the attempt of solvent molecules to go through a ___ into a solution.
Membrane osmometry, semipermeable membrane
Membrane osmometry is useful to determine Mn about ____ and less than _____
20,000-30,000 g/mol, 500,000 g/mol
The main drawbacks to ____ are that it is time consuming and sensitive to changes in the
atmospheric pressure.
ebulliometry
It is not suitable for use with volatile substances or highly reactive chemicals due to the risk of explosion.
Ebulliometry
One disadvantage for ___ is that the process can be time-consuming, as it requires a sudden freezing and slow thawing process.
cryoscopy
Another disadvantage of this process can be sensitive to impurities in the monomer solutions, which can lead to
defective polymer formation
Cryoscopy
_____ is simple but takes several hours to few days in diffusion of solvent through the semipermeable membrane. It is a very slow process and the time taken to attain equilibrium is extremely
high.
Membrane osmometry
Membrane osmometry is useful in themolecular weight range of
30,000 to 1,000,00
The measurement of ___ by polymer solutions is an important technique for the determination of weight-
average molecular weight, Mw. It is an absolute method of molecular weight measurement.
light scattering
___ is a technique that measures the intensity of the scattered light to obtain the average molecular weight Mw of a macromolecule like a polymer or a
protein in solution.
Static light scattering
In a ___ measurement, a coherent laser beam is used to analyze a sample.
static light scattering
One of the great advantages of ___ is that it provides information about macromolecules without any calibration with polymer.
standards.
light scattering
The drawback is that it is non-selective and thus requires
purified extracts without co-eluting contaminants in order to generate
useful data.
Light scattering
✓Requires a solvent with a different refractive index compared to the solute (usually this is fine for most biomacromoleculesin aqueous buffers).
Light-Scattering Method
➢___ is defined as the measure of the opposing force of material to
flow.
Viscosity
➢____ gives the relationship between viscosity and
average molecular weight:
Mark-Houwink equation
➢ It is the most common type of
viscometer that is used for the
determination of viscosity of polymer solution.
Ubbelohde viscometer
✓One disadvantage is that viscometry is generally limited to measuring materials in the ___ state
liquid or semi-liquid
Higher concentration
leads to a ___ viscosity measurement.
higher
➢ ____ is an extremely powerful method for determining the
complete molecular weight distribution and average molecular weights.
Gel permeation chromatography (GPC)
It is essentially a process for the separation of polymer molecules according to their size.
Gel permeation chromatography (GPC)
GPC is also known as
gel filtration, gel exclusion chromatography, size-exclusion chromatography (SEC), and molecular sieve chromatography.
mitations/Disadvantages
✓ There is a limited number of peaks that can be resolved within the short time scale of the GPC run. GPC requires around at least a __ difference in molecular weight for a reasonable resolution of peaks to occur.
10%