Differential scanning calorimetry (DSC) is a thermal analysis technique that measures the heat flow into or out of a sample as it is heated, cooled, or held at constant temperature. DSC was developed in 1962 and measures the difference in heat flow between a sample and an inert reference as they are subjected to a controlled temperature program. DSC can be used to analyze physical and chemical changes in materials by measuring the heat effects associated with phase transitions, crystallization, melting, and chemical reactions as a function of temperature.
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DSC for Pharmaceutical Analysis
1. DIFFERENTIAL SCANNING CALORIMETRY (DSC)
PCH 803 ASSIGNMENT
By
OGOH, ADAKOLE AUGUSTINE
Group 1
M.Sc. Students
Department of Pharmaceutical chemistry
University of Jos, Jos
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3. INTRODUCTION
THERMAL ANALYSIS
During the past few years, the methods of thermal analysis have been widely
accepted in analytical chemistry.
The term thermal analysis incorporates those techniques in which some
physical parameter of the system is determined and/or recorded as a function
of temperature (Willard et al, 2012)
Thermal analysis has been used to determine the physical and chemical
properties of polymers, electronic circuit board, geological materials and
coals (Willard et al, 2012)
A number of physical and chemical effects can be produced by temperature
changes , and method for characterizing these alteration upon heating or
cooling a sample material are referred as thermal analysis.
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4. THERMAL ANALYSIS cont’d
A physical and chemical changes a sample undergoes when heated are
characteristic of the material being examine.
By measuring the temperature at which such reactions occur and the heat
involved in the reaction, the compounds present in such material can be
characterized
The physical and chemical changes that take place when unknown sample is
heated provide the information that enables identification of the material
The majority of the known inorganic compounds have been so
characterized.
Common method of thermal analysis are DSC, DTA and TMA.
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5. METHOD OF THERMALANALYSIS
S/N NAME OF
TECHNIQUE
INSTRUMENT
EMPLOY
PARAMETER
MEASURED
GRAPH
1 Thermogravimetry Thermobalance Mass Mass vs Temperature
2 Differential Thermal
Analysis (DTA)
DTA apparatus ∆T ∆T VS Temperature
3 Dilatometry (TMA) Dilatometer Volume or
length
Volume or length vs
Temperature
4 Emanation Thermal
Analysis (ETA)
ETA apparatus Radioactivity
(E)
E vs Temperature
5 Differential Scanning
Calorimetry (DSC)
Differential
scanning
calorimeter
dH/dt dH/dt vs Temperature
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6. DIFFERENTIAL SCANNING CALORIMETRY (DSC)-
HISTORY
This technique is developed by E.S Watson and M. J. O’Neill in 1962
It was introduced commercially at the Pittsburgh conference on Analytical
Chemistry and Apply Spectroscopy
First adiabatic differential scanning calorimeter that could be used in
biochemistry was developed by P.L. Privalov in 1964
The term DSC was coined to describe this instrument, which measures
energy directly and allows precise measurements of heat capacity
(Wunderlich, 1990)
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7. DIFFERENTIAL SCANNING CALORIMETRY (DSC)
Differential scanning calorimetry (DSC) is one of the thermo-analytical
techniques
A calorimeter measures the heat into or out of a sample
A differential calorimeter measures the heat of sample relative to a reference.
A differential scanning calorimeter does all of the above and heats the sample
with a linear temperature ramp (Freire, 1995)
DSC is a technique in which the difference in the amount of heat required to
increase the temperature of a sample and reference are measured as function
of temperature
Both the sample and reference are maintained at nearly the same temperature
throughout the experiment
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9. INTRODUCTION CONT’D
Generally, the temperature program for a DSC analysis is designed such that
the sample holder temperature increases linearly as a function of time
Only a few mg of material are required to run the analysis
DSC is the most often used thermal analysis method, primarily because of its
speed, simplicity, and availability
It is mostly used for quantitative analysis
The reference is an inert material material such as alumina or just an empty
aluminium pan
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10. BACKGROUND THEORY
Since the Differential Scanning Calorimeter is at constant pressure, the heat
flow is equivalent to enthalpy changes:
(dq/dt)p=dH/dt
Here dH/dt is the heat flow measure in mcalsec.
The heat flow difference between the sample and reference is:
∆dH/dt= ( dH/dt)sample – (dH/dt)reference
The heat change can be either positive or negative.
In an endothermic process, such as most phase transition, heat is absorbed
and therefore, the heat that flow to the sample is higher than that to the
reference.
In an exothermic process,such as crystallization,oxidation reactions and
some decomposition reactions,the opposite is true and dH/dt is negative
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11. REFERENCES
Thermal Methods. In: Chatwal GR, Anand SK. Instrumental Methods of
Chemical Analysis. Fifth Edition: Himalaya Publication House, 2002.
P.2.701 2.749-2.751
Thermal Analysis. In:Willard HH, Merritt LL, Dean JA, Settle FA.
Instrumental Methods of Analysis. Seventh edition: CBS publishers,2012.p.
761.
Freire E. Differential scanning calorimetry. Methods Mol Biol. 1995; 40:
191-218.
Thermal Methods. In: Skoog DA, Holler FJ, Crouch SR. Instrumental
Analysis. India edition: Cengage Learning, 2011.p. 982,983,984
Wunderlich, B. (1990). Thermal Analysis. New York: Academic Press.
pp. 137–140.ISBN 0-12-765605-7.
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