Transcript MDSC - University Blog Service

Modulated Differential Scanning
Calorimetry ®
(MDSC®)
MDSC® Training Course Topics
• What is actually measured by MDSC
•
•
•
•
•
•
– MDSC does not measure the reversibility of
transitions
Understanding heat flow from DSC and MDSC
experiments
Calculation of MDSC signals
Heat capacity calculation
Optimization of MDSC experimental conditions
Characterization of transitions involving a change in
heat capacity (glass transition etc.)
Measurement of polymer melting and crystallinity
– When not to use MDSC
What Does MDSC® Measure?
• As will be shown, MDSC separates the Total heat flow of
•
•
•
DSC into two parts based on the heat flow that does and does
not respond to a changing heating rate
MDSC applies a changing heating rate on top of a linear
heating rate in order measure the heat flow that responds to
the changing heating rate
In general, only heat capacity and melting respond to the
changing heating rate.
The Reversing and Nonreversing signals of MDSC should
never be interpreted as the measurement of reversible and
nonreversible properties
MDSC® Separates the Total Heat Flow Signal of DSC into Two
Parts
dH
 DSC heat flow signal
dt
Cp  Sample Heat Capacity
 SampleSpecific Heat xSample Weight
dH
dT
 Cp
 f (T, t)
dt
dt
dT
 Heating Rate
dt
f (T ,t)  Heat flow thatis functionof time
at an absolute temperatu
re (kinetic)
Understanding Heat Capacity and the Benefits of Being Able
to Measure It
Understanding Heat Capacity
• Heat Capacity or Specific Heat is the amount of heat required to
change the temperature of a specific mass of material (no transition in
structure):
Heat Capacity = Specific Cp (J/g°C) x Sample Weight (g)
• Heat capacity is a measure of molecular motion. Heat capacity
increases as molecular motion increases.
Vibration – occurs below and above Tg
Rotation – polymer backbone and sidechains (in and above
Tg)
Translation – entire polymer molecule (above Tg)
• Transitions in the structure of a material are important because they
result in changes in heat capacity (molecular mobility) and other
important physical, and sometimes chemical, properties
•
Thermodynamic property of material (vs. heat flow). Heat flow is
relative; whereas, the heat capacity is absolute
Changes in Heat Capacity Indicate Significant Changes in
Physical Properties
Sample: Polystyrene
Size: 14.0200 mg
Method: Anneal80
Comment: MDSC.3/40@2; After Anneal @ 80øC various times
DSC
File: C:\TA\Data\Len\FictiveTg\PSanneal80.002
-0.3
Translation
2.0
-0.4
Rotation
Vibration
1.5
Glass Transition is Detectable by DSC
Because of a Step-Change in Heat Capacity
Heat Capacity
Heat Flow
-0.7
Temperature Below Tg
- lower Cp
- lower Volume
- lower CTE
- higher stiffness
- higher viscosity
- more brittle
- lower enthalpy
1.0
-0.6
[ ––––– · ] Heat Flow (mW)
Heat Capacity (J/g/°C)
-0.5
-0.8
-0.9
0.5
-1.0
70
Exo Up
90
110
Temperature (°C)
Universal V3.8A TA Instruments
Understanding Heat Capacity and the Benefits of Being
Able to Measure It (cont.)
Understanding the Benefits
• Knowledge of the baseline due to heat capacity is important
for almost all DSC and MDSC measurements because all
transitions must be analyzed between two points on the heat
capacity baseline for accurate temperatures and heats of
transition.
– It is often impossible to identify the heat capacity baseline
in DSC data
– The MDSC Reversing signals (Cp and Heat Flow)
provide the heat capacity baseline
– Although melting is primarily seen in the Reversing
signal, it is a latent heat (no change in sample
temperature) and is not a heat capacity component
Without Knowledge of the Baseline Due to
Capacity,
File:Heat
C:\TA\Data\Len\Epoxy\MDSCiso100.001
DSC
Analysis of This Epoxy is Not Possible
Sample: Epoxy
Size: 10.8500 mg
Method: MDSCiso.5/40@100
Comment: MDSC iso@100
0.2
0.4
Heating
Experiment at
at 3°C/min
Heating
Experiment
3 C/min
after 160min Isothermal Cure @ 100°C
After 160 min Isothermal Cure at
100 C
Note Inability to
Measure Tg or Integrate
Note Inability to
Peak
Due to Cure
Measure Tg
Nonreversing
-0.6
Total
-1.0
Reversing
110.75°C
117.14°C
31.08J/g
0.0
0.0
-0.4
-0.4
-0.8
All Signals at
Same Sensitivity
119.12°C(H)
0.2810J/g/°C
-1.4
-1.2
52
Exo Up
0.4
[ ––––– · ] Rev Heat Flow (mW)
Sample: Epoxy
Size: 10.85 mg
[ –– –– – ] Nonrev Heat Flow (mW)
Heat Flow (mW)
-0.2
Note Onset
of Decomposition
Note Onset
of Decomosition
Before before
Complete
Cure
Complete
Cure
102
152
Temperature (°C)
202
252
Universal V3.8A TA Instruments
Understanding the Heat Flow Signal from DSC and
MDSC® Experiments
• For a given sample, the rate of heat flow (mW = J/sec) due to
heat capacity is linearly proportional to heating rate.
• At a heating rate of zero, the heat flow due to heat capacity is
also zero.
dH
dT
 Cp
 f (T, t)
dt
dt
• Any heat flow detected at a zero heating rate must be due to
kinetic processes ƒ(T,t) in the sample.
• The purpose of MDSC is to separate the total heat flow into the
part that responds to heating rate and the part that responds to
absolute temperature.
Heat flow due to heat capacity responds linearly to
heating rate
Comparison of DSC and MDSC Heat Flow and
Heat Capacity Signals
dH
dT
 Cp
 f (T, t)
dt
dt
DSC
MDSC®
COMMENTS
Total Heat
Flow
Modulated
Heat Flow
Signals contain all thermal
events occurring in the
sample
Total Heat
Flow
Quantitatively the same in
both techniques at the same
average heating rate
Reversing
Heat Flow
Heat capacity component of
total heat flow
Nonreversing
Heat Flow
Kinetic component of total
heat flow
Heat Capacity All calculated heat flow
signals are also available in
heat capacity units
Selecting MDSC® Mode and Type of Experiment
Storing MDSC® Signals
Signal Selection Button
Selecting MDSC® Signals for Plotting in Universal
Analysis
Average & Modulated Temperature
62
62
Modulate +/- 0.42 °C every 40 seconds (Heat-Iso)
Ramp 4.00 °C/min to 290.00 °C
Temperature (°C)
Temperature (°C)
56.5
Amplitude
60
56.5
56.0
56.0
55.5
55.5
55.0
55.0
Modulated Temperature (°C)
60
Modulated Temperature
57.0
58
58
54.5
13.70
13.75
13.80
13.85
13.90
13.95
14.00
54.5
14.05
Time (min)
56
56
Average Temperature
54
54
Note that temperature is not decreasing during
Modulation i.e. no cooling
52
13.0
13.5
14.0
Time (min)
14.5
52
15.0
Modulated Temperature (°C)
57.0
Average & Modulated Heating Rate; MDSC® Does Not
Require Cooling During Modulation
10
10
Period
Note That Heating Rate is
Never Negative (no cooling)
8
6
6
Average
Heating Rate
4
4
2
2
Modulated
Heating Rate
0
13.0
13.5
14.0
Time (min)
14.5
0
15.0
Deriv. Modulated Temperature (°C/min)
Deriv. Temperature (°C/min)
8
Signal Calculations (cont.)
Reversing Heat Flow
• Calculated from Reversing Heat Capacity signal
Heat Flow Amp
Rev Cp 
x KCp Rev
HeatingRate Amp
Rev Heat Flow  Rev Cp x Avg Heat Rate
Calculation of MDSC® Reversing Heat Flow and Heat
Capacity Signals
Signal Calculations (cont.)
Nonreversing Heat Flow
• Calculated by subtracting the Reversing Heat Flow
signal from the Total Heat Flow signal
dH
dT
 Cp
 f (T, t)
dt
dt
Total = Reversing + Nonreversing
Nonreversing = Total – Reversing
Calculated MDSC® Heat Flow Signals
Separation of Transitions into Modulated DSC®
Signals
MDSC® Data Signals
dH
dt

dT
Cp
dt
Total
=
Reversing +
Transitions:

f (T, t)
Nonreversing
Heat Capacity
Enthalpic Recovery
Glass Transition Evaporation
Most Melting
Crystallization
Thermoset Cure
Protein Denaturation
Starch Gelatinization
Decomposition
Some Melting
Calibration
• Cp Calibration is independent of heating rate
•
•
– 0-5°C/min
Cp Calibration is independent of amplitude
– 0-1°C
Cp Calibration is dependent on period and purge gas
– Calibrate with period that you intend to use for
subsequent runs
– Use purge gas that you plan to use for subsequent
runs
Set Mode & Test as
shown above
1.2
1.2
1.1
1.1
1.0
1.0
0.9
0.9
Plot Heat Capacity and Rev Cp
vs. temperature
0.8
0.7
0
50
100
150
Temperature (°C)
200
250
0.8
0.7
300
[ ––––– · ] Rev Cp (J/g/°C)
Heat Capacity (J/g/°C)
Sapphire Cp data
Sapphire Cp data
1.2
1.2
Total
1.1
276.85°C
1.076J/g/°C
Theoretical Values
1.1
176.85°C
0.9975J/g/°C
1.0
1.0
126.85°C
0.9423J/g/°C
Reversing
76.85°C
0.8713J/g/°C
0.9
0.9
26.85°C
0.7788J/g/°C
Theoretical values of
Sapphire indicated
0.8
0.7
0
50
100
150
Temperature (°C)
200
250
0.8
0.7
300
[ ––––– · ] Rev Cp (J/g/°C)
Heat Capacity (J/g/°C)
226.85°C
1.041J/g/°C
View spreadsheet of data
Cp Data Table
Temperature Heat Capacity
°C
J/g/°C
26.85
0.7675
36.85
0.7887
46.85
0.8086
56.85
0.8275
66.85
0.8454
76.85
0.8614
86.85
0.8765
96.85
0.8914
106.85
0.9069
116.85
0.9217
126.85
0.9339
136.85
0.9467
146.85
0.9573
156.85
0.9674
Rev Cp
J/g/°C
0.7816
0.8026
0.8223
0.8405
0.8578
0.873
0.8869
0.9008
0.9133
0.9256
0.9378
0.9479
0.9582
0.9676
Temperature Heat Capacity
166.85
0.9778
176.85
0.9874
186.85
0.9974
196.85
1.005
206.85
1.012
216.85
1.021
226.85
1.03
236.85
1.037
246.85
1.048
256.85
1.056
266.85
1.066
276.85
1.074
286.85
1.082
Rev Cp
0.9761
0.9826
0.9903
0.9978
1.004
1.01
1.016
1.022
1.027
1.032
1.036
1.041
1.044
Determining K
Temperature Heat Capacity
°C
J/g/°C
26.85
0.7675
36.85
0.7887
46.85
0.8086
56.85
0.8275
66.85
0.8454
76.85
0.8614
86.85
0.8765
96.85
0.8914
106.85
0.9069
116.85
0.9217
126.85
0.9339
136.85
0.9467
146.85
0.9573
156.85
0.9674
166.85
0.9778
176.85
0.9874
186.85
0.9974
196.85
1.005
206.85
1.012
216.85
1.021
226.85
1.03
236.85
1.037
246.85
1.048
256.85
1.056
266.85
1.066
276.85
1.074
286.85
1.082
Rev Cp
J/g/°C
0.7816
0.8026
0.8223
0.8405
0.8578
0.873
0.8869
0.9008
0.9133
0.9256
0.9378
0.9479
0.9582
0.9676
0.9761
0.9826
0.9903
0.9978
1.004
1.01
1.016
1.022
1.027
1.032
1.036
1.041
1.044
Theo.
Cp
K  Meas.
Cp
The heat capacity calibration
constant, K, is calculated as the
ratio of the theoretical heat
capacity of a standard material,
to the measured heat capacity of
the material.
Sapphire Cp Values
Aluminum Oxide Specific Heat Capacity*
°C
J/g°C
°C
J/g°C
°C
J/g°C
-143.15
-133.15
-123.15
-113.15
-103.15
-93.15
-83.15
-73.15
-63.15
-53.15
-43.15
-33.15
-23.15
-13.15
-3.15
6.85
16.85
26.85
36.85
46.85
56.85
0.2349
0.2739
0.3133
0.3525
0.3912
0.4290
0.4659
0.5014
0.5356
0.5684
0.5996
0.6294
0.6577
0.6846
0.7102
0.7344
0.7574
0.7792
0.7999
0.8194
0.8380
66.85
76.85
86.85
96.85
106.85
116.85
126.85
136.85
146.85
156.85
166.85
176.85
186.85
196.85
206.85
216.85
226.85
236.85
246.85
256.85
276.85
0.8556
0.8721
0.8878
0.9027
0.9168
0.9302
0.9429
0.9550
0.9666
0.9775
0.9879
0.9975
1.0074
1.0164
1.0250
1.0332
1.0411
1.0486
1.0559
1.0628
1.0758
286.85
296.85
306.85
316.85
326.85
336.85
346.85
356.85
366.85
376.85
386.85
396.85
406.85
416.85
426.85
446.85
466.85
486.85
506.85
526.85
546.85
1.0819
1.0877
1.0934
1.0988
1.1040
1.1090
1.1138
1.1184
1.1228
1.1272
1.1313
1.1353
1.1393
1.1431
1.1467
1.1538
1.1605
1.1667
1.1727
1.1784
1.1839
*Taken from ASTM E1269, Standard Test Method for Determining Specific Heat Capacity by
Differential Scanning Calorimetry, which references Archer, D.G.,J. Phys. Chem. Ref. Data,
Vol.22, No. 6, pp. 1441-1453.
Determining K @ 1 temperature
Temperature Heat Capacity
°C
J/g/°C
26.85
0.7675
36.85
0.7887
46.85
0.8086
56.85
0.8275
66.85
0.8454
76.85
0.8614
86.85
0.8765
96.85
0.8914
106.85
0.9069
116.85
0.9217
126.85
0.9339
136.85
0.9467
146.85
0.9573
156.85
0.9674
166.85
0.9778
176.85
0.9874
186.85
0.9974
196.85
1.005
206.85
1.012
216.85
1.021
226.85
1.03
236.85
1.037
246.85
1.048
256.85
1.056
266.85
1.066
276.85
1.074
286.85
1.082
Rev Cp Lit value
J/g/°C
0.7816
0.8026
0.8223
0.8405
0.8578
0.873
0.8869
0.9008
0.9133 0.9168
0.9256
0.9378
0.9479
0.9582
0.9676
0.9761
0.9826
0.9903
0.9978
1.004
1.01
1.016
1.022
1.027
1.032
1.036
1.041
1.044
KCp
K RevCp
1.0109
1.0038
Theo.
Cp
K  Meas.
Cp
Determining K(multiple temperatures)
Temperature Heat Capacity
°C
J/g/°C
26.85
0.7675
36.85
0.7887
46.85
0.8086
56.85
0.8275
66.85
0.8454
76.85
0.8614
86.85
0.8765
96.85
0.8914
106.85
0.9069
116.85
0.9217
126.85
0.9339
136.85
0.9467
146.85
0.9573
156.85
0.9674
166.85
0.9778
176.85
0.9874
186.85
0.9974
196.85
1.005
206.85
1.012
216.85
1.021
226.85
1.03
236.85
1.037
246.85
1.048
256.85
1.056
266.85
1.066
276.85
1.074
286.85
1.082
Rev Cp Lit value
J/g/°C
0.7816
0.8026
0.8223
0.8405 0.8380
0.8578
0.873
0.8869
0.9008
0.9133 0.9168
0.9256
0.9378
0.9479
0.9582
0.9676 0.9775
0.9761
0.9826
0.9903
0.9978
1.004
1.0250
1.01
1.016
1.022
1.027
1.032
1.0628
1.036
1.041
1.044
Theo.
Cp
K  Meas.
Cp
Determining K(multiple temperatures)
Temperature Heat Capacity
°C
J/g/°C
26.85
0.7675
36.85
0.7887
46.85
0.8086
56.85
0.8275
66.85
0.8454
76.85
0.8614
86.85
0.8765
96.85
0.8914
106.85
0.9069
116.85
0.9217
126.85
0.9339
136.85
0.9467
146.85
0.9573
156.85
0.9674
166.85
0.9778
176.85
0.9874
186.85
0.9974
196.85
1.005
206.85
1.012
216.85
1.021
226.85
1.03
236.85
1.037
246.85
1.048
256.85
1.056
266.85
1.066
276.85
1.074
286.85
1.082
Rev Cp Lit value
J/g/°C
0.7816
0.8026
0.8223
0.8405 0.8380
0.8578
0.873
0.8869
0.9008
0.9133 0.9168
0.9256
0.9378
0.9479
0.9582
0.9676 0.9775
0.9761
0.9826
0.9903
0.9978
1.004
1.0250
1.01
1.016
1.022
1.027
1.032
1.0628
1.036
1.041
1.044
Avg
KCp
K RevCp
1.0127
0.9970
1.0109
1.0038
1.0104
1.0102
1.0128
1.0209
1.0064
1.0298
1.0107
1.0124
Theo.
Cp
K  Meas.
Cp
Type K values into
Cell Calibration table
Optimization of MDSC® Experimental Conditions
MDSC® controls the Heating Rate(s) applied to the
sample through three experimental parameters:
1. Average Heating Rate (°C/min)
–
Typically less than 5°C/minute in order to
get a minimum of 4-5 temperature
modulations during a transition
2. Temperature Modulation Amplitude (± °C)
–
Typically ± 0.1 to 2°C
3. Temperature Modulation Period (Seconds)
–
Typically 40 – 100 seconds
Optimization (cont.)
Proper selection of the three experimental parameters
is important in order to maximize the quality of the
results.
• Specific recommendations for different types of
transitions will be provided in later sections.
• In general, temperature is controlled to either
provide or not provide cooling during the
temperature modulation.
• The combination of temperature modulation
amplitude and period control the range in
heating rate while its average is defined by the
specified heating rate.
MDSC® Heat-Iso Amplitudes (no cooling/measure
crystallinity)
Period (sec)
H
e
a
t
i
n
g
40
50
60
70
80
90
100
0.1
0.011
0.013
0.016
0.019
0.021
0.024
0.027
0.2
0.021
0.027
0.032
0.037
0.042
0.048
0.053
0.5
0.053
0.066
0.080
0.093
0.106
0.119
0.133
1.0
0.106
0.133
0.159
0.186
0.212
0.239
0.265
R
2.0
0.212 0.265 0.318 0.371 0.424 0.477 0.531
a
t
5.0
0.531 0.663 0.796 0.928 1.061 1.194 1.326
e
This table is additive, i.e. the heat only amplitude for a period of 40 sec & a
heating rate of 2.5°C/min is the sum of the values for 2.0°C/min & 0.5°C/min
Amplitude (40s,2.5°C/min)=0.212+0.053=0.265°C
MDSC® Heat-Iso Temperature Modulation
No Cooling
Heating Rate never goes below 0°C/min
MDSC® Heat-Cool Temperature Modulation
Heating &
Cooling
Heating Rate goes below 0°C/min
Optimization of MDSC® Conditions for Glass
Transitions w/ a Q Series MDSC (heat-cool)
MDSC® Analysis of the Glass Transition
The following measurements will be illustrated
• Measurement of Tg in Complex Samples
• Quantitative Measurement of Amorphous Structure in
Materials
• Quantitative Measurement of Enthalpic Recovery
(Relaxation) in Aged Samples
– Glass transition is frequency dependent
– MDSC applies a frequency (Period) during the
measurement and this affects the measured temperature of
the Reversing signal
– It is necessary to do a “Frequency Correction” in order to
measure absolute values of enthalpic recovery
Measuring Tg in Complex Samples with MDSC®
• Complex samples are ones that have overlapping
•
•
transitions which make it difficult to detect or
measure Tg
MDSC experimental conditions which provide some
cooling during temperature modulation are
recommended
Use an underlying heating rate that is slow enough
to provide 4 or more modulation cycles over the
transition of interest in order to improve separation
of overlapping events (resolution)
Figure 25 - MDSC® of Frozen Sucrose Solution
Sample: Epoxy
Size: 10.8500 mg
Method: MDSCiso.5/40@100
Comment: MDSC iso@100
File: C:\TA\Data\Len\Epoxy\MDSCiso100.001
Advantage of MDSC® for Post Cure Scan
DSC
0.2
0.4
Heating
Experiment
3 C/min
Heating
Experiment atat
3°C/min
160min
Isothermal Cure
@ 100°C
Afterafter
160
min Isothermal
Cure
at
100 C
Nonreversing
-0.6
Note Inability to
Measure Tg
Total
-1.0
Reversing
110.75°C
117.14°C
31.08J/g
0.0
0.0
-0.4
-0.4
-0.8
All Signals at
Same Sensitivity
119.12°C(H)
0.2810J/g/°C
-1.4
-1.2
52
Exo Up
0.4
[ ––––– · ] Rev Heat Flow (mW)
Sample: Epoxy
Size: 10.85 mg
[ –– –– – ] Nonrev Heat Flow (mW)
Heat Flow (mW)
-0.2
Note Onset of Decomosition
before Complete Cure
102
152
Temperature (°C)
202
252
Universal V3.8A TA Instruments
DSC of Complex Polymer Blend
MDSC® of Complex Polymer Blend
Optimization of MDSC® Experimental Conditions
for Analysis of Melting and Crystallinity
• Sample Size; 10-15mg
• Period
– 40 sec. Q Series for crimped pans
– 60 sec. Q Series for hermetic pans
• Heating Rate
– Slow enough to get a minimum of 4-5 cycles at halfheight of the melting peaks
• Amplitude
– Use “Heat-Iso” amplitude which provides no cooling
during temperature modulation (see Table)
– Crystallization will not be caused by a lowering of
the temperature
Optimization of MDSC® Conditions for Melting (cont.)
Issues with Use of MDSC in Melting Region
Before discussing how MDSC® can be used to analyze melting and
crystallinity, it is necessary to discuss some technical issues with the
measurement.
• Issue 1: MDSC® cannot provide a meaningful measurement
on samples that have a narrow melting range (pure metals and
chemicals). The reason is that the temperature of the sample
cannot be modulated during melting (Figures 43-44).
• Issue 2: Because there are two simultaneous endothermic
processes occurring during melting (heat capacity and latent
heat of fusion), and because those processes respond
differently to temperature modulation, the separation of the
Total signal into the Reversing and Nonreversing components
changes when experimental conditions are changed (Fig 4553).
MDSC® Should Not Be Used on Sharp Melting
Transitions
MDSC® of Water Melting/Boiling
MDSC® Raw Data Signals on Polymer Blend
MDSC® of 57/43 % PET/PC Blend
Sample: Quenched PET and PC
Size: 13.6000 mg
DSC
Method: MDSC .318/40@3
Comment: MDSC 0.318/40@3; PET13.60/PC 10.40/Al film 0.96mg
File: C:\TA\Data\Len\Crystallinity\qPET-PC.002
3
57% PET; 43% PC
MDSC Signals
2
Heat Flow (mW)
270.00°C
-1
-3
155.00°C
270.00°C
1
0
-1
-2
[ ––––– · ] Rev Heat Flow (mW)
95.13J/g
110.00°C
[ –– –– – ] Nonrev Heat Flow (mW)
1
-3
93.60J/g
-5
-4
Initial Crystallinity = 93.6 + (-95.1) = -1.5 J/g
-5
50
Exo Up
100
150
Temperature (°C)
200
250
300
Universal V3.8A TA Instruments
DSC Analysis of Cycoloy C2950: Standard DSC Ramp
Sample: Cycoloy C2950
Size: 5.5740 mg
0.0
Method Log:
1: Equilibrate at 0.00°C
2: Ramp 5.00°C/min to 300.00°C
3: End of method
Using standard DSC a single glass transition is observed.
Heat Flow (W/g)
-0.1
107.05°C
113.87°C(I)
119.62°C
-0.2
-0.3
0
Exo Up
50
100
150
Temperature (°C)
200
250
300
Universal V4.3A TA Instruments
DSC Analysis of Cycoloy C2950: MDSC Heat Cool Heat
Method/ First Heat
Sample: Cycoloy
Size: 6.3900 mg
0.00
First Heat Cycle
-0.02
-0.04
106.65°C
110.99°C(I)
159.55°C
115.08°C
Rev Heat Flow (W/g)
Using MDSC two glass transitions are observed in the
MDSC Reversing heat flow signal.
165.47°C(I)
-0.06
168.89°C
0
Exo Up
50
100
150
Temperature (°C)
200
-0.08
250
Universal V4.3A TA Instruments
Using the TMA Q400 to Observe the Glass Transitions in
Cycoloy C2950
Sample: Cycoloy C2950
Size: 1.8208 mm
500
Glass Transition
108.90°C
0
113.39°C(I)
185.1µm
Dimension Change (µm)
115.28°C
-500
Glass Transition
136.34°C
144.27°C(I)
1742µm
-1000
Method Log:
1: Force 0.200 N
2: Ramp 5.00°C/min to 200.00°C
3: End of method
-1500
152.25°C
-2000
20
40
60
80
100
120
Temperature (°C)
140
160
180
200
Universal V4.3A TA Instruments
Summary
• MDSC® is a slow technique. Always start the
analysis of a new material with standard DSC
and only use MDSC if you need.
–
–
–
–
Improved sensitivity
Better resolution
Separation of overlapping transitions
Most accurate measurement of polymer crystallinity
• Don’t forget that MDSC can be used while
•
•
cooling
Optimum results require the selection of
optimum experimental conditions
When in doubt, ask TA Instruments for help?
What if I need help?
• On-site training & e-Training courses - see Website
• Call the TA Instruments Hotline
•
•
– 302-427-4070 M-F 8-4:30 Eastern Time
– [email protected]
Call the TA Instruments Service Hotline
– 302-427-4050 M-F 8-4:30 Eastern Time
Check out our Website
– www.tainstruments.com