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Differential Scanning Calorimetry (DSC)

Differential Scanning Calorimetry (DSC) is a thermal analysis technique that measures heat flow associated with phase transitions in materials, widely used in various industries including pharmaceuticals and food science. It operates by comparing the heat flow of a sample to a reference under controlled temperature changes, detecting endothermic and exothermic transitions. DSC has several types, including Heat-Flux and Power-Compensated DSC, and offers advantages such as high sensitivity and a wide temperature range, though it has limitations like the need for calibration and thermal stability of samples.

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9 views5 pages

Differential Scanning Calorimetry (DSC)

Differential Scanning Calorimetry (DSC) is a thermal analysis technique that measures heat flow associated with phase transitions in materials, widely used in various industries including pharmaceuticals and food science. It operates by comparing the heat flow of a sample to a reference under controlled temperature changes, detecting endothermic and exothermic transitions. DSC has several types, including Heat-Flux and Power-Compensated DSC, and offers advantages such as high sensitivity and a wide temperature range, though it has limitations like the need for calibration and thermal stability of samples.

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maryamsandhu769
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Differential Scanning Calorimetry

(DSC)
Differential Scanning Calorimetry (DSC) is a thermal analysis technique used to
measure the heat flow associated with phase transitions (e.g., melting,
crystallization, glass transition) in materials as a function of temperature or time.
It is widely used in pharmaceuticals, polymers, food science, and material science
to study thermal properties.

Principle
DSC measures the heat flow difference between a sample and a reference material
when both are subjected to a controlled temperature program.

• Endothermic transitions (heat absorbed): Melting, glass transition,


dehydration.

• Exothermic transitions (heat released): Crystallization, oxidation,


polymerization.

DSC measures the heat flow difference between a sample and a reference as they
undergo controlled temperature changes. This allows detection of thermal
transitions such as melting, crystallization, glass transitions, and chemical
reactions.

Types of DSC:

1. Heat-Flux DSC: A single furnace heats both pans. The heat flows through
a thermally conductive disk (e.g., platinum, aluminum) connecting the
sample and reference.

2. Power-Compensated DSC: Separate heaters for the sample and reference


pans allow independent power adjustments to maintain temperature
equilibrium.
3. Instrumentation
1. Sample and Reference Crucibles (Pans)

• Sample Pan: Holds the material under study (e.g., polymer, drug,
metal).

• Reference Pan: Contains an inert material (e.g., empty pan or


alumina) to provide a baseline.

• Both pans are placed symmetrically within the furnace.

2. Furnace Assembly

• Heat-Flux DSC: A single furnace heats both pans. The heat flows
through a thermally conductive disk (e.g., platinum, aluminum)
connecting the sample and reference.

• Power-Compensated DSC: Separate heaters for the sample and


reference pans allow independent power adjustments to maintain
temperature equilibrium.

3. Temperature Sensors

• Thermocouples: Measure the temperature of the sample (Ts) and


reference (Tr).

• In heat-flux DSC, the temperature difference (ΔT=Ts−Tr) is


proportional to heat flow.

• In power-compensated DSC, thermocouples ensure Ts=Tr by


adjusting heater power.

4. Heaters (Power-Compensated DSC)

• Individual heaters for the sample and reference pans.


• The power difference required to maintain equal temperatures is
recorded as the heat flow signal.

5. Temperature Controller:

• Regulates the furnace heating/cooling rate (e.g., 10 °C/min).

6. Cooling System:

• Liquid nitrogen or mechanical refrigeration for rapid cooling.

7. Purge Gas System:

• Inert gas (e.g., nitrogen, argon) flows through the furnace to prevent
oxidation or control atmosphere.

8. Data Acquisition System:

• Converts ΔT (heat-flux DSC) or power difference (power-


compensated DSC) into heat flow (dq/dt).

• Draws a plot of heat flow (mW) vs. temperature (°C) or time.


Applications:

1- Pharmaceutical Industry

a) Polymorphism Detection – Identifies different crystalline forms of drugs.


b) Glass Transition Temperature (Tg)– The temperature at which
amorphous polymers transition from a rigid, glassy state to a more flexible,
rubbery state. t determines amorphous vs. crystalline nature of drugs.
c) Purity Analysis – Higher purity shows sharp melting points. Assesses drug
purity, polymorphism, and stability.

2- Polymer Industry

a) Crystallinity & Melting Point–Determines degree of polymer


crystallinity. Determines glass transition temperature (Tg), melting points
(Tm), crystallization, and curing kinetics.
b) Thermal Stability–Evaluates degradation temperatures.
c) Crosslinking & Curing – Used in thermoset resins and adhesives.

3- Food Science

a) Fats & Oils Characterization – Determines melting profiles in chocolate,


margarine.
b) Protein Denaturation –To study protein stability in dairy and meat
products.

4- Material Science & Metallurgy

i) Phase Transitions – Studies phase changes in alloys, ceramics.


ii) Oxidation Stability – Determines thermal degradation temperatures.

iii) Materials Science: Studies phase transitions, thermal stability, and


composition.
Comparison with Other Techniques:

• TGA: Measures mass loss (complements DSC by identifying


decomposition).

• DTA: Measures temperature differences (less quantitative for enthalpy


than DSC).

Advantages

1- High sensitivity and accuracy.


2- Small sample size required.
3- Wide temperature range (from -150 °C to 1600 °C in some
instruments).
4- Applicable to various materials (polymers, metals, pharmaceuticals,
etc.).

Limitations

1- Requires calibration for accuracy.


2- Limited information on kinetic parameters.
3- Samples must be thermally stable to avoid decomposition.

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