Thermal analysis and its applications

1. - Aaditya Thole

2. › Thermal analysis is a branch of materials science where
the properties of materials are studied as they change
with temperature.

3. METHOD ABBREVIATION PROPERTY MEASURED
DIFFERNTIAL THERMAL
ANALYSIS
DTA TEMEPERATURE
DIFFERENCE
DIFFERNETIAL SCANNING
CALORIMETRY
DSC ENTHALPY
THERMOGRAVIMETRIC
ANALYSIS
TGA MASS
DYNAMIC MECHANICAL
ANALYSIS
DMA DEFORMATION
DIELECTRIC THERMAL
ANALYSIS
DEA DEFORMATION
EVOLVED GAS ANALYSIS EGA GASEOUS
THERMO-OPTICAL
ANALYSIS
TOA OPTICAL PROPERTIES

4. › Differential scanning calorimetry, or DSC, is 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.
› Both the sample and reference are maintained at nearly the same
temperature throughout the experiment.

5. DSC
Heat capacity
Glass transition
temperature
Temperature
of
crystallization
Temperature of
melting

6. In Pharmaceutical Industry
Detection of polymorphism
Quantification of polymorph
Detection of metastable
polymorph
Fingerprinting of wax
Detection of isomerism
Percentage crystallinity
determination
Amorphous content in
excipient
APPLICATIONS
Protein stability and
folding
Process development
Antibody domain studies
Rank order binding
Protein engineering
Characterisation of
membrane, lipids and
micellar systems

7. › Glass transition temperature is the temperature at which higher
molecular weight materials(polymers) transforms from glassy state
to a viscous and rubbery state.

8. › DTA is a technique in which the difference in temperature between a
substance and a reference material is measured as a function of
temperature while the substance and reference material are
subjected to a controlled temperature program.

9. › To study phase transitions and phase diagram.
› To fingerprint substances
› To determine M.Pt., B.Pt., decomposition temperatures of
organic compounds

10. › To characterize inorganic materials
› The peak at 113°C corresponds to a solid-phase change from the
rhombic to the monoclinic form, while the peak at 124°C corresponds
to the melting point of the element.
› Liquid sulphur is known to exist in at least three forms, and the peak
at 179°C
› apparently involves a transition among these.
› The peak at 446°C corresponds to the boiling point of sulphur.

11. To quantitatively analyze polymer
mixtures
› This is a thermogram of a physical
mixture of seven commercial
polymers.
› Each peak corresponds to the
characteristic melting point of one
of the components.
› Poly tetrafluoroethylene (PTFE)
has an additional low temperature
peak, which arises from a
crystalline transition.

12. › Quantitative analysis of Compounds
› Determination of Structural and Chemical
› changes occurring during heat treatments.
› Quality Control of Cement, glass, textiles, soils,
explosives and resins

13. › TGA measures the amount and the rate of weight change
of a material with respect to temperature or time in
controlled environments.

14. › Determination of the bound and unbound water in the suspension
of Milk of Magnesia (MoM), used as a laxative.
› In an overview of thermal analysis testing it is always preferable to
do a TGA experiment on unknown samples before doing a DSC
experiment (especially for pharmaceuticals).
› Decomposition of pharmaceuticals renders products which are
insoluble and generally sticky on the inside of a DSC cell.
› These products will lower the life use of a DSC cell. Therefore,
know the decomposition temperatures of all drugs and heat in a
DSC evaluation to 50°C below those temperatures.

15. › Evaporation of free (unbound) water begins at room
temperature due to dry gas flowing over the sample.
› Decomposition can have multiple stages (weight
losses)but the presence of multiple weight loss steps can
also indicate the presence of multiple components in the
sample.

16. THANK YOU