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Stephen Collins
Definitions
A calorimeter measures the heat into or out of a sample. A differential calorimeter measures the heat of a sample relative to a reference. A differential scanning calorimeter does all of the above and heats the sample with a linear temperature ramp. Endothermic heat flows into the sample. Exothermic heat flows out of the sample.
Conventional DSC
Sample
Metal 1 Metal Metal 2 1
Empty
Metal 2
Sample Temperature
Reference Temperature
DSC Thermogram
Crystallisation
Cross-Linking (Cure)
Oxidation
Glass Transition
Melting
Temperature
6
DSC
File: C:...\DSC\Melt Mixed1\PET80PC20_MM1.001 Operator SAC : Run Date 05-Apr-2006 15:34 : Instrument DSC Q1000 V9.4 Build 287 :
Tm
245.24C
1.0
Tg
Heat Flow(W/g)
0.5
79.70C(I) 75.41C 81.80C
Tc
137.58C 20.30J/g 228.80C 22.48J/g
Cycle 1
0.0
144.72C
-0.5
Exo Down
50
100
150
200
250
300
Universal V .2E TA Instruments 4
TemperatureC) (
-2
706
162
164
166
156
158
166
168
170
Sample mass
Processing errors
99
Good for:
Poor for: Accuracy: transitions can be shifted by as much as 40oC Repeatabiliy: Very sensitive to thermal lag.
Technical Group Talk
60
60
58
58
Modulation:
Period: 60 second Amplitude: +/-10C
56
56
54
54
Time (min)
Modulated DSC
Benefits Increased Sensitivity for Detecting Weak (Glass) Transitions Eliminates baseline curvature and drift Increased Resolution Without Loss of Sensitivity Two heating rates (average and instantaneous) Ability to Separate Complex Thermal Events and Transitions Into Their Heat Capacity and Kinetic Components Ability to Measure Heat Capacity (Structure) Changes During Reactions and Under Isothermal Conditions Downside Slow data collection
Example MDSC
0.00 0.00
-0.02
-0.02
-0.02
-0.04
-0.04
-0.04
-0.06
-0.06
-0.06
-0.08
-0.08
-0.08
-0.10
-0.10
-0.10
-0.12
-0.12
-0.12
-0.14 -50
Exo Up
50
100
150
200
-0.14 250
Universal V4.2E TA Instruments
Temperature (C)
Modulated DSC
Reversible Transitions Glass Transition Melting
Evaporation
Technical Group Talk