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Differential Scanning
Calorimetry (DSC)
-0.2
Evaporation
-0.3
Other endothermic processes
-0.4
Endothermic
Exothermic
0.1
Heat Flow (W/g)
0.0
Heat flows out of the sample as a result of either
Heat capacity (cooling)
Crystallization
Curing
Oxidation
Other exothermic processes
-0.1
0 20 40 60 80 100 120 140 160
Exo Up Temperature (°C)
DSC Heat Flow
dH Cp Sample Heat Capacity
DSC heat flow signal
dt Sample Specific Heat x Sample Weight
dH dT
Cp f (T, t)
dt dt
dT
Heating Rate f (T, t) Heat flow that is function of time
dt at an absolute temperatu re (kinetic)
DSC - types
DSC is the most sophisticated and
advanced of the thermal methods.
Constantan disk
Alumel wire
Chromel disk
Chromel wire
S – glass transition
Ex – exothermic reaction
En – endothermic reaction
3/30/2019 Dr.Anand, MME, NITK 20
Enthalpy changes
The DSC curve may show an exothermic or
endothermic peak
The enthalpy changes associated with the events
occurring are given by the area under the peaks.
Peaks may be characterized by:
Position (i.e., start, end, extrapolated onset and peak
temperatures)
Size (related to the amount of material and energy of
the reaction)
Shape (which can be related to the kinetics of the
process)
dH dT
Cp f (T, t)
dt dt
dT
Heating Rate f (T, t) Heat flow that is function of time
dt at an absolute temperatu re (kinetic)
Measurement of ΔH of thermal
transitions
Exo
crystallization
7.96 Cal/g
Endo
melting
8.04 Cal/g
-5
Height
-15
-25
-30
140 145 150 155 160 165 170 175 180
Temperature (°C)
Melting of Indium
0
Extrapolated
Onset 156.60°C
28.50J/g
-5 Temperature
Indium
5.7mg
Heat Flow (mW)
-3 Extrapolated
Onset
Heat Flow (mW)
Temperature 236.15°C
-4 52.19J/g
-5 Heat of PET
Fusion 6.79mg
10°C/min
-6
249.70°C
Peak Temperature
-7
200 210 220 230 240 250 260 270
Exo Up Temperature (°C) Universal V4.0B TA Instruments
Effect of heating rate
Exo
Heat flow (mW)
Endo
Temperature (0 C)
-
0.
08F
i
rs
t 1
5
5.
93
°C
T
g
-
0.
12 R
e
s
id
ua
l
C u
r
e
1
0
2.
64
°C
-
0.
16S
e
co
n
d T
g2
HeatFlow(W/g)
0
.
38J
/g
-
0.
20
-
0.
24
0 5
0 1
0
01 5
02 0
025
030
0
Te
mp
e
ra
t
ur
e(
°C
)
Method Design Rules
Start Temperature
Generally, the baseline should have two (2) minutes to
completely stabilize prior to the transition of interest.
Therefore, at 10°C/min., start at least 20°C below the
transition onset temperature
End Temperature
Allow a two (2) minute baseline after the transition of
interest in order to correctly select integration or analysis
limits
Tg
Tc
Polystyrene
9.67mg
10°C/min
Step Change in Cp at the Glass Transition
PET
9.43mg
Polymer A
Polymer B
endo
Blend of A+B
Reference
R. F. Speyer, Thermal analysis of
materials, Marcel Dekker, 1994.