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What is a DSC?
What is DSC?
1
DSC working principle
Ice Air
Ts Tr
Hot Plate
2
DSC working principle
Temperature
Tr
Ts
Tf
Time
T =Ts-Tr
0
DSC raw signal
-0.5
Time
Tf or Tr
3
DSC working principle
T =Ts-Tr
-0.5
Time
Φ=T/Rth
or Tr
Rth, thermal
Heat flow (mW) resistence of the
system
H DSC signal, Φ
-10
Time Peak integral H
Tf or Tr
4
Baseline slope
Heat flow Φ
(mW) Φ = m ⋅ cp ⋅
Where,
0
Φ m is the sample mass
cp is the specific heat capacity
Initial deflection
of the sample
β is the heating rate
-10
Time
or Tr
5
ICTA and Anti-ICTA
ICTAC (International Confederation for Thermal Analysis and Calorimetry)
mW
0
-10
-20
!
&
,-
#"
$%
+ * *+
()
6
Endothermic and exothermic effects
Endothermic:
Exothermic:
7
Exothermic effect
Temperature
Tr
Ts
Time
T =Ts-Tr
Time
or Tr
8
Schematic DSC curve of a polymer
exo
6
1 2
Heat flow
3 4 5
endo
Temperature
crystalline amorphous
10
Melting and Crystallization with DSC
^exo prod 1 13. 03.2006 13:58:29
mW
10
Integral -193.95 mJ
normalized -28.52 Jg^-1
Onset 156.58 °C
-10
11
How to evaluate melting peaks
• Pure materials:
- onset (independent of heating rate)
- ∆Hf baseline: line, integral tangential
• Impure materials:
- peak temperature (depends on β)
- ∆Hf baseline: line, tangential right
- purity analysis for eutectic systems
(based on curve shape analysis)
• Polymers
- peak temperature (depends on β and m)
- ∆Hf baseline: line, spline, integral tangential
12
What is glass transition?
cp
1 dH
cp = ⋅
m dT
Temperature
exotherm Φ
Φ = m ⋅ cp ⋅ β
Temperature
14
Chemical reaction
15
Chemical reaction
16
Where to use DSC?
Polymers
Pharmaceuticals
Chemicals
Food
Cosmetics
Materials Processing
Additives Thermal treatment
Material
Plasticizers Mechanical stressing
Properties
Impurities Shaping
Fillers Storage and use
17
DSC
Multiple Thermocouples
increase sensitivity and
reduce noise
S R
Temperature gradients on the sensor lead to
baseline deviation from zero
∆TSR
S
T0
R A single sensor temperature (T0) is measured.
Inhomogeneous temperature distribution of
∆TS0 ∆TR0 the sensor is not considered.
19
Sensor technology
S R
TS
TS TR
TS0 TR0
20
Sensor technology
N TS ,i − TS 0 ,i
S R ΦS0 =
TS i =1 Ri
N TR ,i − TR 0 ,i
TS TR Φ R0 =
i =1 Ri
TS0 TR0 dq
= Φ S 0 − Φ R0
dt
5
100
uW
uW
60 65 70 75 80 °C
50 60 70 80 90 °C 18 20 22 24 min
22
Noise and sensitivity
23
Resolution
24
Signal time constant
25
Signal time constant
26
Cooling behavior
250
100
50
-50
-100
-150
0 5 10 15 20 25
Time [min]
27
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