The document summarizes a seminar presentation given by Shaik Gouse Ul Azam on the qualification of differential scanning calorimetry (DSC). It introduces DSC, describes its principle, and covers the key aspects involved in qualifying a DSC including design qualification, operational qualification, performance qualification, and installation qualification. Examples of common applications like determining purity and polymorphs are also mentioned.
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DSC Qualification Seminar
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
Qualification of Differential scanning calorimetry (DSC)
A Seminar as a part of curricular for Master of Pharmacy,
I Year - II semester
Presented by
SHAIK GOUSE UL AZAM
(20L81S0708)
Pharmaceutical Analysis
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
Contents:
Introduction
Principle
Instrumentation
Qualification of DSc
Applications
References
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
Introduction:
• Differential scanning calorimetry is a thermoanalytical technique in
which the difference in the amount of heat required to increase
the temperature of a sample and reference is measured as a function
of temperature.
• Both the sample and reference are maintained at nearly the same
temperature throughout the experiment.
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
Principle:
• Most popular thermal technique
• DSc measures the heat absorbs or liberated during the various
transistions in the sample due to temperature treatment
Differential:sample relative to reference
Scanning:temperature is ramped
Calorimeter :measures heat
• Dsc measurements are both qualitative and quantitative and provide
information about physical and chemical changes
• Two types:
Endothermic
Exothermic
4
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
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
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
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
Qualification of Dsc:
8
• qualification is an act or process to assures something complies with
some condition, standard or specific requirements
Design qualification
Operational qualification
Performance qualification
Installation qualification
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
Design qualification
• DQ takes place prior to the purchase decision and defines the
requirement profile of the device.
• This includes the functional and operation specifications as well
as the intended purpose of the instrument and, finally, shows
that the selected instrument is appropriate.
• DQ can be performed by the instrument manufacturer or by the
user. Some laboratories
additionally issue a separate user requirement specification
(URS) list which prepends the DQ. In the URS, future users
specify what they want the instrument to be able to do. 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
Installation qualification
• The DSc should be:
In: A temperature controlled area(150C to 300C is recommended
• A clean environment .
• An area with working and ventilation
ON:A stable, heat-resistant, and fire-resistant work surface.
Near:
• A power outlet (120 volt, 50 or 60 HZ, 15lamps) A step up/down
line transformer may be required. if the unit is operated from a
higher or lower line voltage of your controller.
• A compressed lab air and puge gas supply for use during cooling,
subambient, and high temperature experiments.
10
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
Away from:
Dusty environment.
Exposure to direct sunlight
Direct air drafts (fans air ducts)
Poorly ventilated areas.
Flammable materials
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
Operational qualification
• Operational qualification follows the installation qualification.
It is a documented collection of activities with the objective to
verify that the instrument works correctly in the selected
environment and fulfills.
• The operational specifications given in the Design
Qualification (DQ) and/or the user requirement specifications
(URS).
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
Performance qualification
• The most common procedure is to run an indium standard under and
normal test conditions and measure the heat of fusion valve and melting
onset temperature.
• These value are then compared with literature values and a check made
against accepted limits.
• For many industries limits of +0.50C for temperature or 1% for heat of
fusion may be accepted.
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
• Though tighter limits of +0.30C and 0.1% may also be adopted.
The choice of limits depends on how accurate you need to be.
• Indium is the easiest standard to use because of its stability
and relatively low melting point of 156.60C, which means it can
often be reused. Provided it is not heated above 1800C
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
Applications
• To determine the purity of a sample
• To determine the number of polymorphs and to determine the ratio
of each polymorph.
• To determine the heat of salvation.
• To determine the thermal degradation of a drug or excipients.
• To determine the glass-transition temperature(tg) of a polymer.
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
References
1. D.L. Martin, Rev. Sci. Instrument. (1987) 58
2. R.D. Chirico, S.E. Knipmeyer, A. Nguyen, W.V. Steele, J.
Chem. Thermodyn.(1993)25
3. J.F. Messerly, H.L. Finke, W.D. Good, B.E. Gammon, J.
Chem. Thermodyn. (1988) 20
4. R.D. Chirico, S.E. Knipmeyer, A. Nguyen, W.V. Steele, J.
Chem. Eng. Data (1997) 42
5. R.A. Perkins, H.M. Roder, D.G. Friend, C.A. Nieto de Castro,
Physical (1991) 173
6. G. Ernst, E. Hochberg, J. Chem. Thermodyn. (1989) 21
7. J.P. Hiernaut, C. Ronchi, High Temp.-High Pressures (1989)
21
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