Qualification of DSC

In this slide contains QUALIFICATION OF DSC
Presented by: SHAIK GOUSE UL AZAM (Department of pharmaceutical analysis ).RIPER, anantapur

1. 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. Contents: Introduction Principle Instrumentation Qualification of DSc Applications References 2

3. 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. 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

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8. 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. 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. Installation qualification The DSc should be: In: A temperature controlled area(15 C to 30 C 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. Away from: Dusty environment. Exposure to direct sunlight Direct air drafts (fans air ducts) Poorly ventilated areas. Flammable materials 11

12. 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. 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 +0.5 C for temperature or 1% for heat of fusion may be accepted. 13

14. Though tighter limits of +0.3 C 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 156.6 C, which means it can often be reused. Provided it is not heated above 180 C 14

15. 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. References D.L. Martin, Rev. Sci. Instrument. (1987) 58 R.D. Chirico, S.E. Knipmeyer, A. Nguyen, W.V. Steele, J. Chem. Thermodyn.(1993)25 J.F. Messerly, H.L. Finke, W.D. Good, B.E. Gammon, J. Chem. Thermodyn. (1988) 20 R.D. Chirico, S.E. Knipmeyer, A. Nguyen, W.V. Steele, J. Chem. Eng. Data (1997) 42 R.A. Perkins, H.M. Roder, D.G. Friend, C.A. Nieto de Castro, Physical (1991) 173 G. Ernst, E. Hochberg, J. Chem. Thermodyn. (1989) 21 J.P. Hiernaut, C. Ronchi, High Temp.-High Pressures (1989) 21 16