THERMAL METHODS OF ANALYSIS
Thermal method of analysis:
comprise a group of techniques in which a
physical property of a substance is measured as a
function of temperature while the substance is
subjected to a controlled temperature
programme.
Classification of thermo-analytical
techniques:
Techniques most commonly used in pharmacy:
1. Thermo-microscopy 2. Differential thermal
analysis
3. Differential scanning
calorimetry 4. thermo-gravimetry
Developed by Austrian pharmacognosist Ludwig Kofler and his
wife Adelheid Kofler and continued by Maria Kuhnert-
Brandstätter.
This technique is also known as hot-stage microscopy.
Technique involves the observation of sample through
a microscope fitted with a stage that can be heated or
cooled at a controlled rate. Modern hot stages can
cover the range of -180 to 600 C.
DIFFERENTIAL THERMAL ANALYSIS
Speakers:
Anam hassan
Bushra khan
DEFINITION
Differential thermal analysis is
the measurement of the
difference in temperature
between a sample and a
reference as heat is applied to
the system.
DTA GRAPH
FACTORS AFFECT RESULT IN DTA
Sample weight
Heating rate
Particle size
Atmospheric condition
INSTRUMENTATION
Apparatus for DTA consists of:
Sample & reference holder
A furnace
A detector
An amplifier
A recorder
APPLICATIONS
Qualitative and quantitative
identification of minerals.
Analysis of biological material
To determine M.P, B.P, decomposition
temperature of organic compounds.
Widely used for the quality control of
a large number of substances like
cement, glass, soil etc.
Also used for the thermal stability of
inorganic compounds and complexes.
DIFFERENTIAL SCANNING
CALORIMETERy
SPEAKERS:
HIRA ARSHAD
AMMARA FAROOQUI
TERMS TO KNOW:
CALORIMETER
DIFFERENTIAL CALORIMETER
DIFFERENTIAL SCANNING CALORIMETER
Heat the sample with linear temperature ramp
PRINCIPLE
The measuring principle is to compare the rate of
heat flow to the sample and to an inert material
which are heated or cooled at the same rate.
DSC GRAPH
FACTORS AFFECTING DSC
Sample shape
Carnoba Wax Polymer Blend
Polymorphism of
Phenobarbitol
Sample Size
Other Factors
Furnace heating rate
Sensitivity of recording mechanism
Particle size
Nature of sample
Thermal conductivity
INSTRUMENTATION
TYPES OF DSC INSTRUMENTS
Power compensation DSC Heat-flux DSC
Pt resistance thermocouples Chromel-alumel
thermocouples
Separate sensors & heaters Sample & reference are
for the sample & reference connected by a low-
resistance heat flow path
separate blocks for sample one block for both sample &
and reference cells reference cells
APPLICATIONS
Qualitative analysis
Quantitative analysis
Detection of impurities
Heat of fusion and extent of crystallinity can also be
determined.
To study and characterize polymers and their
identification
Discriminate several commercial polymers in a
mixture.
Determine melting and boiling points more
accurately
Determine moisture content (moisture presence
causes peaks regarding dehydration).
Use to study phase transition
Decomposition of inorganic metals like alloy etc.
Physical changes of excepients during storage of dosage
form
DSC with the support of X-ray diffraction and IR
spectroscopy are used as screening technique for the
compatibility testing of a drug with excepients.
SPEAKERS:
“…. a technique in which the
mass of a substance is
measured as a function of
temperature, while the
substance is subjected to a
controlled temperature
programme.”
3 Essential parts of thermo balance which are as follows:
A furnace is an enclosed structure used for
heating materials to very high temperatures.
A microbalance is capable of
making precise measurements
of weight of objects of
relatively small mass.
Recorder is use to record the data in computer in
graphical form for further interpretation.
GAS IN BALANCE
WEIGHT
CONTROLLER
GAS-TIGHT
ENCLOSURE
SAMPLE
HEATER
SAMPLE TEMP.
POWER FURNACE TEMP.
TEMPERATURE PROGRAMMER
The plot also shows the derivative of the
TG curve, or the DTG curve, which is
often useful in revealing extra
detail, such as the small event around
400°C.
