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RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 1
Differential Scanning Calorimeter
Instrumentation
A Seminar as a part of curricular requirement
for I year M. Pharm I semester
Presented by
N. Poojitha
(Reg. No. 20L81S0308)
Under the guidance
Dr. Nawaz Mahammad
M. Pharm, Ph.D
Associate Professor
Dept. of Pharmaceutics
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 2
• Introduction of DSC
• Principle of DSC
• Instrumentation of DSC
• References
Contents
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 3
Introduction of DSC
• The technique was developed by E.S. Watson and M.J. O Neill in
1960, and introduced commercially at the Pittsburgh Conference on
Analytical Chemistry and Applied Spectroscopy in 1963.
• This technique is used to study what happens to polymers/samples
upon heating.
• It is used to study thermal transitions of a polymer/sample (the
changes that take place on heating)
• The differential scanning calorimeter does all of the above functions
and heats the sample with the linear temperature.
• Both the sample and reference are maintained at nearly the same
temperature through out the experiment in DSC
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 4
Principle of DSC
• It is a technique in which the energy necessary to establish a zero
temperature difference between the sample & reference material is
measured as a function of temperature.
• Here, sample & reference material are heated by separate heaters in
such a way that their temp are kept equal while these temp. are
increased or decreased linearly.
• During heating two types of reactions can be take place one is the
endothermic and the other is the exothermic.
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 5
Endothermic reaction:
• If sample absorbs some amount of heat during phase transition then
reaction is said to be endothermic.
• In endothermic reaction more energy needed to maintain zero temp
difference between sample & reference.
• E.g. Melting, boiling, sublimation, vaporization
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 6
Exothermic reaction:
• If sample released some amount of heat during phase transition,
then reaction is said to be exothermic.
• In exothermic reaction, less energy needed to maintain zero temp
difference between sample & reference.
• E.g crystallization, degradation, polymerization
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 7
DSC Graph
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 8
DSC Instrumentation
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 9
• Two basic types of DSC instruments: Heat flux DSC, Power
compensated DSC
Types of DSC Instuments
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 10
1.Heat-flux DSC
• Sample Holder :
 PLATINUM, ALUMINIUM, STAINLESS STEEL
• SENSORS:
 Temperature Sensors
 Usually thermocouples, which are same for the sample are reference
• Furnace:
 One block for both sample and reference cells.
• Temperature:
 The temperature difference between the sample and reference is
converted to differential thermal power, which is supplied to the heaters
to maintain the temperature of the sample and reference at program
value.
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 11
2.Power Compensated DSC
• Sample Holder :
 PLATINUM, ALUMINIUM, STAINLESS STEEL PANS
• SENSORS:
 Pt resistance thermocouple
 Separate sensors and heaters for the sample and reference sample.
• Furnace:
 Separate blocks for sample and reference cells.
• Temperature:
 Differential thermal power is supplied to the heaters to maintain the
temperature of the sample and reference at the program level.
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 12
DSC attached to Computer
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 13
• P. J. Elving & I. M. Kolthoff, Chemical analysis, Vol. 19, P134, 1964.
• Wang L, Wang B, Lin Q. Demonstration of MEMS-based differential
scanning calorimetry for determining thermodynamic properties of
biomolecules. Sensor Actuat B-Chem 2008;134:953– 958
• Masri MS, Reuter FW, Fiedman M. Interaction of wool with metal
cations. J Appl Polym Sci 1974;18:675–681
• Hohne G, Hemminger W, Flammersheim H-J. Differential Scanning
Calimetry: An Introduction for Practitioners. Berlin, Germany:
Springer-Verlag, 1996 .
• Instrumental methods of analysis- Willards,7th edition, CBS
Publications ;237-332. 11/12/2019
References
RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 14

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Differential Scanning Calorimeter Instrumentation.(DSC)

  • 1. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 1 Differential Scanning Calorimeter Instrumentation A Seminar as a part of curricular requirement for I year M. Pharm I semester Presented by N. Poojitha (Reg. No. 20L81S0308) Under the guidance Dr. Nawaz Mahammad M. Pharm, Ph.D Associate Professor Dept. of Pharmaceutics
  • 2. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 2 • Introduction of DSC • Principle of DSC • Instrumentation of DSC • References Contents
  • 3. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 3 Introduction of DSC • The technique was developed by E.S. Watson and M.J. O Neill in 1960, and introduced commercially at the Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy in 1963. • This technique is used to study what happens to polymers/samples upon heating. • It is used to study thermal transitions of a polymer/sample (the changes that take place on heating) • The differential scanning calorimeter does all of the above functions and heats the sample with the linear temperature. • Both the sample and reference are maintained at nearly the same temperature through out the experiment in DSC
  • 4. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 4 Principle of DSC • It is a technique in which the energy necessary to establish a zero temperature difference between the sample & reference material is measured as a function of temperature. • Here, sample & reference material are heated by separate heaters in such a way that their temp are kept equal while these temp. are increased or decreased linearly. • During heating two types of reactions can be take place one is the endothermic and the other is the exothermic.
  • 5. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 5 Endothermic reaction: • If sample absorbs some amount of heat during phase transition then reaction is said to be endothermic. • In endothermic reaction more energy needed to maintain zero temp difference between sample & reference. • E.g. Melting, boiling, sublimation, vaporization
  • 6. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 6 Exothermic reaction: • If sample released some amount of heat during phase transition, then reaction is said to be exothermic. • In exothermic reaction, less energy needed to maintain zero temp difference between sample & reference. • E.g crystallization, degradation, polymerization
  • 7. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 7 DSC Graph
  • 8. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 8 DSC Instrumentation
  • 9. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 9 • Two basic types of DSC instruments: Heat flux DSC, Power compensated DSC Types of DSC Instuments
  • 10. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 10 1.Heat-flux DSC • Sample Holder :  PLATINUM, ALUMINIUM, STAINLESS STEEL • SENSORS:  Temperature Sensors  Usually thermocouples, which are same for the sample are reference • Furnace:  One block for both sample and reference cells. • Temperature:  The temperature difference between the sample and reference is converted to differential thermal power, which is supplied to the heaters to maintain the temperature of the sample and reference at program value.
  • 11. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 11 2.Power Compensated DSC • Sample Holder :  PLATINUM, ALUMINIUM, STAINLESS STEEL PANS • SENSORS:  Pt resistance thermocouple  Separate sensors and heaters for the sample and reference sample. • Furnace:  Separate blocks for sample and reference cells. • Temperature:  Differential thermal power is supplied to the heaters to maintain the temperature of the sample and reference at the program level.
  • 12. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 12 DSC attached to Computer
  • 13. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 13 • P. J. Elving & I. M. Kolthoff, Chemical analysis, Vol. 19, P134, 1964. • Wang L, Wang B, Lin Q. Demonstration of MEMS-based differential scanning calorimetry for determining thermodynamic properties of biomolecules. Sensor Actuat B-Chem 2008;134:953– 958 • Masri MS, Reuter FW, Fiedman M. Interaction of wool with metal cations. J Appl Polym Sci 1974;18:675–681 • Hohne G, Hemminger W, Flammersheim H-J. Differential Scanning Calimetry: An Introduction for Practitioners. Berlin, Germany: Springer-Verlag, 1996 . • Instrumental methods of analysis- Willards,7th edition, CBS Publications ;237-332. 11/12/2019 References
  • 14. RIPER AUTONOMOUS NAAC & NBA (UG) SIRO- DSIR Raghavendra Institute of Pharmaceutical Education and Research - Autonomous K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 14