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Introduction To DSC
Introduction To DSC
What is a DSC?
What is DSC?
Differential: measurement of the difference in heat flow from sample and reference side Scanning: the common operation mode is to run temperature or time scans
Air Tr
Heat the hot plate from -20 C to 30 C, What will happen to the ice? How do Ts and Tr react? How do the Ts and Tr relate to each other?
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Tr Ts
Tf
T =Ts-Tr 0
Time
Tf
Time or Tr
=T/Rth
Rth, thermal resistence of the system
Baseline slope
Heat flow (mW)
= m cp
Where,
0
Initial deflection
-10 Time or Tr
m is the sample mass cp is the specific heat capacity of the sample is the heating rate
mW 0
-10
-20
120
130
140
150
160
170
C
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Exothermic:
When the sample releases energy, the process is said to be exothermic. Processes such as crystallization and oxidation are exothermic.
Exothermic effect
Temperature
Tr Ts
T =Ts-Tr
0 Time or Tr
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exo 6 3 endo 4 5
Heat flow
Temperature
crystalline
amorphous
prod 1
20
10
-10
140
145
150
155
160
165
MSG2006: Marco
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TA Re SW 9. 01 S TAR
1 dH cp = m dT
Temperature
= m cp
exotherm
Temperature
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Chemical reaction
A chemical reaction is a process that one or more substances (reactants) are converted to one or more new chemical substances (products) with different properties. e.g. oxidation, decomposition, polymerization etc.
Chemical reactions always involve a change in energy. Depending on whether the energy is absorbed or released during the process, they can be endothermic or exothermic.
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Chemical reaction
Homogeneous decomposition of dibenzoyl peroxide; peak temperature and peak shape depend on heating rate; peak area is independent of heating rate.
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Material Properties
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DSC
Resolution and Sensitivity Multiple Thermocouples increase sensitivity and reduce noise For Best Resolution: Low signal time constant e.g 1.7 s (20- L Al crucible, N2 gas) High baseline stability using chemically resistant ceramic substrate and relatively inert silver furnace
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Sensor technology
TSR
T0
A single sensor temperature (T0) is measured. Inhomogeneous temperature distribution of the sensor is not considered.
TS0 TR0
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Sensor technology
TS S R
TS TS0
TR TR0
Inner ring of thermocouples measure TR and TS Outer ring measures sensor temperatures at reference and samples sides, TS0 and TR0 Thermocouples act as thermal resistence, R.
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Sensor technology
TS S R
S0 =
R0 =
N i =1
N i =1
TS ,i TS 0 ,i Ri
TR ,i TR 0 ,i Ri
TS TS0
TR TR0
dq = S 0 R0 dt
Heat flow on the sample and reference sides are separately measured N is the number of thermocouples (TC) per ring.
FRS5 sensor (56 TC): N = 14
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Step 0.69 uW
0.1 % Lysozyme
60 50 60 70 80 90 C 18
65 20
70 22
75 24
80
C min
22
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Resolution
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Signal = RthCs,
FRS5 sensor (Rth 0.04 K/mW) & Al40 l (50 mg) Cpan Csample (10 mg, 1.5 J/gK) Csensor 50 mJ/K 15 mJ/K 10 mJ/K => Signal 3 s
FRS5 sensor (Rth 0.04 K/mW) & Al20 l (20 mg) Cpan 20 mJ/K
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Cs can be reduced by using smaller sample size Signal can be further decreased by using He as purge gas.
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Cooling behavior
250 200 150
Temperature [ C]
Time [min]
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