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Optimization of Freeze Drying
Optimization of Freeze Drying
Optimization of Freeze Drying
Oxidation
Or
Crystallization Decomposition
Heat Flow → exothermic
Melting
Glass
Cross-Linking
Transition
(Cure)
Composite graph
Temperature
Standard DSC of Frozen Sucrose Solution
MDSC® of Frozen Sucrose Solution
Note: Heating
Rate 0.5C/min
Structural Comparison of Frozen Sucrose
Solution During Slow Cooling and Heating
Understanding Structural Differences Between
Quenched and Slow-Cooled Sucrose-Water Solution
5 0.2
Quench Cooled
4
3 -0.1
Quench Cooled
-0.2
2
Slow Cooled
Heat Capacity Signals
-0.3
Both Steps Due to Tg
Amorphous Sucrose
1 -0.4
-60 -50 -40 -30 -20
Temperature (°C) Universal V3.8A TA Instruments
One Experiment on Same Sample Shows Metastability of
Quench-cooled 40% Sucrose-water Solution
Measuring Time-Dependence of Processes
with Modulated Differential Scanning
Calorimetry (MDSC®)
Question:
Is the Structure of a Slow Cooled
Frozen Solution Stable?
NO !
10% Sucrose-water Solution in Open DSC Hermetic Lid
(Permits Sublimation of Water)
YES !
Use of MDSC to Study Sublimation (Drying) Rate
Quenched
Slow‐cooled
Drying Temperature
Liquid (Mobile)
Phase
Glassy (Rigid) Phase
Heat Capacity of Solution Decreases During Drying
Due to Both Structure Change and Mass Loss
Tg
Heat Capacity of Solution Decreases During Drying
Due to Both Structure Change and Mass Loss
Tg
Heat Capacity of Solution Decreases During Drying
Due to Both Structure Change and Mass Loss
Tg
Heat Capacity of Dilute Solution Decreases During
Drying Due Only to Mass Loss
MDSC Relative Drying Rates of
Sucrose/Water Solutions at -40°C
Steven Aubuchon
Product Manager, Thermal Analysis
saubuchon@tainstruments.com
+1 302.427.4073