Differential thermal analysis

& differential scanning

calorigraphy
 Thermal Analysis Techniques

 A group of techniques in which a physical property

is measured as a function of temperature.

 The sample is subjected to a predefined heating or

cooling program.
 Types of thermal analysis

 TG (Thermo gravimetric) analysis:

weight

 DTA (Differential Thermal Analysis):

temperature

 DSC (Differential Scanning Calorimetry):

temperature
Differential thermal analysis

Definition: DTA is a technique in which the

temperature between sample & thermally inert

reference substance is continuously recorded as a

function of temperature /time.

In DTA both test sample & an inert reference material

(alumina) – controlled heating or cooling programming.

If zero temperature difference b/w sample & reference material

– sample does not undergo any chemical or physical change.

If any reaction takes place temperature difference (∆T) will

occur b/w sample & reference material .

 DTA Principle

Differential thermal analysis is a

technique in which the

temperature of the substance
under investigation is
compared with the
temperature of a
thermally inert material.
 Differential Thermal Analysis
sample holder
sample and reference cells (Al)

sensors
Pt/Rh or chromel/alumel thermocouples one for the
sample and one for the reference joined to
differential temperature controller

furnace
alumina block containing sample and reference cells

temperature controller
controls for temperature program and furnace
atmosphere

Recording system
DTA Instrument
 Differential Thermal Analysis

advantages:

instruments can be used at very high temperatures

instruments are highly sensitive

flexibility in crucible volume/form

characteristic transition or reaction temperatures can be

accurately determined

disadvantages:

uncertainty of heats of fusion, transition, or reaction

estimations is 20-50%
 Applications of Differential thermal
analysis

Qualitative and Quantitative Identification of Minerals:

detection of any minerals in a sample

Polymeric Materials: DTA useful for the characterization of

polymeric materials in the light of identification of thermo

physical , thermo chemical, thermo mechanical and thermo

elastic changes or transitions.

Measurement of Crystalline: measurement of the mass fraction

of crystalline material in semi crystalline polymers.

Analysis of Biological Materials: DTA curves are used to date bone remains or to
study archaeological materials.
 Differential Scanning Calorimetry

this technique is developed by E.S.Watson and

M.J.O’Neill in 1962.

 introduced commercially at the Pittsburgh

Conference on analytical Chemistry and Applied

Spectroscopy.

First Adiabatic differential scanning calorimeter

that could be used in Biochemistry was developed by

P.L.Privalov in 1964.
 Principle

In DSC the heat flow is measured and plotted against

temperature of furnace or time to get a thermogram. This is the

basis of Differential Scanning Calorimetry (DSC).

The deviation observed above the base (zero) line is called

exothermic transition and below is called endothermic transition.

 The area under the peak is directly proportional to the heat

evolved or absorbed by the reaction, and the height of the curve is

directly proportional to the rate of reaction.
DSC Curve
 Heat Flux DSC
•sample holder

•sample and reference are connected by a low-resistance heat

flow path Al or Pt pans placed on constantan disc

•sensors
chromel®-constantan area thermocouples (differential heat flow)

chromel®-alumel thermocouples (sample temperature)

•furnace
one block for both sample and reference cells
•temperature controller

the temperature difference between the sample and reference is

converted to differential thermal power, dDq/dt, which is

supplied to the heaters to maintain the temperature of the sample

and reference at the program value

Heat flux DSC
 Power Compensation DSC
individual
heaters
controller P

 sample holder
sample reference

Al or Pt pans pan pan

 sensors inert gas

vacuum
inert gas
vacuum

thermocouple T=0
Pt resistance thermocouples
separate sensors and heaters for the sample and reference

 furnace
separate blocks for sample and reference cells

 temperature controller
differential thermal power is supplied to the heaters to maintain
the temperature of the sample and reference at the program
value
 Applications of DSC

Protien Stability and Folding

Liquid Biopharmaceutical Formulations

Process Development
Protien Engineering
Rank order Binding
Antibody Domain Studies
acids & micellar
Characterisation of Membranes,lipids,nucleiec systems

Assesment of the effects of structural change on a molecules

stabiity
Measurement of Ultra-light molecular interactions
Assesment of biocomparability during manufracturing.
 Applications of DSC

Polymers:
composition of polymers is determined.
Melting point and lass transition temp can be determined

This can show the polymer degradation by lowering the melting

point(Tm).Molecular weight(low grade –low melting point) can be
determained.
Percentage Crytallinity
Thermal degradation and impurities
Liquid crystals

Oxidative Stability: stability & optimum storage conditions

Drug analysis: widely used in Pharmaceutical industry(defining

processing parameters) and polymer industry(curing process.).

General Chemical analysis: Freezing point depression can be

used as a purity analysis tool.

Functional Applications:
Binding Studies