In this slides contains Differential Thermal analysis (DTA) and Differential Scanning calorimetry (DSC). Presented by : J.Vinay Krishna (Department of industrial pharmacy). RIPER, anantapur.

1. Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721
A Seminar as a part of curricular requirement for
Master of Pharmacy, I Year - I semester
Presented by
J. Vinay Krishna
(20L81S0806)
Dept of. Industrial Pharmacy
Differential Thermal Analysis (DTA)
&
Differential Scanning Calorimetry (DSC)
Under the guidance/Mentorship of
Dr. Hindustan Abdul Ahad M. Pharm., PhD., FAGE
Professor & Head, Department of Industrial Pharmacy,
Program in charge (PG)

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
The Information Provided in this PPT For
Education Purpose Only
2

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
Differential Thermal Analysis (DTA)
 The temperature difference between a sample and an inert reference
material, DT = TS - TR, is measured as both are subjected to identical
heat treatments.
3

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
Differential Scanning Calorimetry (DSC)
 The sample and reference are maintained at the same temperature,
even during a thermal event (in the sample)
 The energy required to maintain zero temperature differential between
the sample and the reference, dDq/dt, is measured

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
 Sample and Reference Placed in Heater
 Constant Heating Rate
⁃ Initial Temp
⁃ Final Temp
⁃ Heating Rate (°C/min)
 Data
⁃ Temp of Sample vs Time (or Temp)
⁃ Temp of Reference vs Time (or Temp)
⁃ Reference should be inert
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DTA

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
 Measures
⁃ Heat of crystallization
⁃ Glass Transition Temperature
6

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
Differential Thermal Analysis
 DTA involves heating or cooling a test sample and an inert reference
under identical conditions, while recording any temperature
difference between the sample and reference.
 This differential temperature is then plotted against time, or against
temperature.
 Changes in the sample which lead to the absorption or evolution of
heat can be detected relative to the inert reference.
7

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

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
Instrumentation
 Sample holder
 Sample and reference cells (Al)
 Sensors Platinum/Rhodium 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
9

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
Differential Thermal Analysis
 Advantages:
 Instruments can be used at very high temperatures.
 Instruments are highly sensitive.
 Flexibility incrucible volume/form.
 Characteristic transition or reaction temperatures can be accurately
determined.
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Disadvantages:
 Uncertainty of heat of fusion,transition, reaction estimations is
20 - 50%.

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
Differential Scanning Calorimetry
 DSC is a thermal analysis method where differences in heat flow
into a substance and a reference are measured as a function of
sample temperature, while both are subjected to a controlled
temperature program.
11

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
 The basic difference between DTA and DSC
 DSC- calorimetric method, energy differences measured.
 DTA- temperature differences measured.
 The applications of both techniques are similar, but DSC is now
more popular.
 DTA is used for higher temperature and qualitative applications.
 DSCis used for calorimetric determinations, sample purity
determinations and kinetics.
12

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
 DSC differs fundamentally from DTA in that the sample and
reference are both maintained at the temperature predetermined by
the program.
• During a thermal event in the sample, the system will transfer heat
to or from the sample pan to maintain the same temperature in
reference and sample pans.
13

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
Differential Scanning Calorimetry –
Principle of Operation
 A sample is placed inside a crucible which is then placed inside the
furnace of the DSC system along with a reference pan which is
normally empty (inert gas may be used).
 By applying a controlled temperature program (isothermal, heating
or cooling at constant rates), phase changes can be characterized
and/or the specific heat of a material can be determined.
 Heat flow quantities are calculated based on calibrated heat flow
characteristics of the cell.
14

15. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721
• Two basic types of DSC instruments:
• Power compensation
• Heat-flux
15

16. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721
Two major types of DSC instruments are available:
 Heat flux device – more popular; more stable baseline and more
durable cell.
Difference in heat flow into s and r is measured with (linear) change in
sample temperature.
 Power compensation device – better resolution; faster heating and
cooling rates. s and r heated by separate heaters to keep same
temperature, as T is changed linearly.
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17. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 17
Power compensation DSC
Heat flux DSC

18. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721
References
• Rieger J. The glass transition temperature Tg of polymers—comparison of
the values from differential thermal analysis (DTA, DSC) and dynamic
mechanical measurements (torsion pendulum). Polymer testing. 2001 Oct
1;20(2):199-204.
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19. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721
Thank
You 19