abcit characterization of polyammides. abcit 3 methods p infrared spectroscopy p differential...
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Characterization of PolyammidesCharacterization of Polyammides
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3 methods3 methods
Infrared SpectroscopyInfrared Spectroscopy Differential Scanning CalorimetryDifferential Scanning Calorimetry Dynamic Mechanic AnalysisDynamic Mechanic Analysis
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Infrared SpectroscopyInfrared Spectroscopy
We send an infrared beam We send an infrared beam on the sampleon the sample
The radiation will be The radiation will be attenuated only at specific attenuated only at specific wavelenghtswavelenghts
The graph is called The graph is called Spectrum and is a Spectrum and is a “fingerprint” of every “fingerprint” of every moleculemolecule
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PA 6PA 6
4000.0 3000 2000 1500 1000 630.0
2.8
20
40
60
80
99.7
cm-1
%T
3296.45
3082.50
2933.19
2861.77
1637.50
1541.33
1460.951437.50
1370.83
1261.301200.94
1170.09
1118.56
1074.34
974.46
929.67
830.80
685.91
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PA 6,6PA 6,6
4000.0 3000 2000 1500 1000 630.0
3.110
20
30
40
50
60
70
80
90
101.8
cm-1
%T
3298.45
3071.87
2933.19
2861.04
1635.18
1538.06
1465.04
1418.371370.551274.35
1200.08
1065.05935.20
872.23
829.63
797.44
689.97
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Overlay of PA 6 and 6,6Overlay of PA 6 and 6,6
1786.7 1700 1600 1500 1400 1300 1200 1100 1000 912.6cm-1
%T
PA 6
PA 6 61635.18 1538.06
1465.04 1418.371370.55 1274.35
1200.08
1065.05935.20
1637.50 1541.33
1460.95
1437.501370.83
1261.30
1200.94
1170.09
1118.56
1074.34974.46
929.67
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Differential Scanning CalorimetryDifferential Scanning Calorimetry
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DSC of PA 6DSC of PA 6
DDSC of Nylon:Heat Flow and Storage Cp
Figure 2
Temperature (°C)
Heat Flo
w (m
W)
Specifi
c H
eat (J
/g°C
)
Storage Cp
Heat Flow
Onset 78.43°C
Peak 56.41°C
H 69.17 J/g
Tg 90.01°C
Cp 0.153 J/g°C
0.0 25.0 50.0 75.0 100.0 125.0 150.0
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1.0
1.6
1.8
2.0
2.2
2.4
2.6
2.8
Tue Apr 4 10:14:20 1995
Heat F
low
(m
W)
S2 std.pans Applications LabTemperature ( C)
Curve 1: DDSC in DDSC ModeFile info: nylon003 Mon Mar 20 11:09:31 1995Sample Weight: 6.171 mg
nylon floss, 1st heat
PERKIN-ELMER7 Series Thermal Analysis System
Temp 1:-30.0 C Time 1: 30.0 s Rate 1: 4.00 C/min Temp 2:-28.0 C
Segment: Iso-Scan Repeated 100 times
End:170.0 C Time: 100.0 min
nylon floss, 1st heat
Specific
Heat
(J/g
C)
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StepScan DSC of NylonStepScan DSC of Nylon
Nylon 6 polymers yield simultaneous moisture evolution peak Nylon 6 polymers yield simultaneous moisture evolution peak and plasticized Tgand plasticized Tg
Standard DSC has difficulty detecting plasticized Tg because Standard DSC has difficulty detecting plasticized Tg because of moisture peakof moisture peak
StepScan DSC can separate out the moisture evolution peak StepScan DSC can separate out the moisture evolution peak (‘slow’ process) from the Tg (‘fast’)(‘slow’ process) from the Tg (‘fast’)
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StepScan DSC of Ambient Humidity Nylon 6 FibersStepScan DSC of Ambient Humidity Nylon 6 Fibers
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StepScan DSC of Saturated Nylon 6 FibersStepScan DSC of Saturated Nylon 6 Fibers
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StepScan DSC of Dry Nylon 6 FibersStepScan DSC of Dry Nylon 6 Fibers
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Dynamic Mechanic AnalysisDynamic Mechanic Analysis
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A typical DMA curve...A typical DMA curve...
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PA 6PA 6
RH20%
RH0%
RH40%
RH60%
RH80%
T
RH80%
RH20%RH0%
RH40%RH60%
T
PA 12PA 12
Moisture effect on DMA of PA 6 and 12Moisture effect on DMA of PA 6 and 12
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Frequency effect on ModulusFrequency effect on Modulus
PMMA ( 0.01 ~ 100Hz )
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