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DIFFERENTIAL SCANNING CALORIMETRY (DSC)
PCH 803 ASSIGNMENT
By
OGOH, ADAKOLE AUGUSTINE
Group 1
M.Sc. Students
Department of Pharmaceutical chemistry
University of Jos, Jos
1
OUTLINE
 INTRODUCTION
 Thermal analysis
 History
 Method of thermal analysis
 BACKGROUND THEORY
 REFERENCES
2
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.
3
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.
4
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
5
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)
6
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
7
PICTURAL REPRESENTATION
8
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
9
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
10
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.
11
THANK YOU
12

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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 1
  • 2. OUTLINE  INTRODUCTION  Thermal analysis  History  Method of thermal analysis  BACKGROUND THEORY  REFERENCES 2
  • 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. 3
  • 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. 4
  • 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 5
  • 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) 6
  • 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 7
  • 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 9
  • 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 10
  • 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. 11