*-01
Evolved gas analysis for an adhesive
in the curing process
The problem in curing process (e.g. contamination in apparatus, bubbles) can be attributed to the
evolved gases from an adhesive. Temperature Programmed Desorption - Mass Spectrometer (TPDMS) method is applied for the evolved gas analysis (EGA) from an adhesive in curing process.
10
m/z 98
m/z
8
Ｅ
3
40
m/z 72
m/z
6
H2O m/z 18
20
Splitter
12
4
MS
2
0
Adsorbent
tube B
Adsorbent
tube Ａ
0
0
TD-GC/MS
10
20
- Schematic diagram of TPD-MS connected with adsorbent tubes - Gas Sampling region Ａ
（using the tube Ａ）
The results of TD-GC/MS
H
C
3
Ｂ
m/z 91
m/z
H
C
OC
3
H
C
Ａ
m/z 58
m/z
30
Region B
(Simulating the heating process)
(Simulating the post cure process)
Ｃ
3
O
C H3C H 2C H 2C H 2C HC O H
Temperature range：88 ～100℃
C H 2C H3
H
C
2
H
C
OC
3
H
C
(Temperature was held at 100℃ after heating.)
m/z
m/z 72
Time（min）
Gas Sampling region B
（using the tube B）
Region Ａ
Temperature range：28 ～88℃
Ｅ
Rate of evolution（wtppm/sce）
O
C H 3 C C H=C C H 3
C H3
m/z
m/z 91
60
14
m/z 88
m/z
Ｄ
H
C
2
H
C
OC
3
H
C
Temperature（℃）
3
Ｂ
C H2C H3
H
C
Mass spectrometer
O
C H3C H2C H2C H2C HC OH
m/z 58
3
Temperature
温度
-controlled
コントローラfurnace
Conductive
adhesive
80
16
Ｃ
H
C
OC
3
H
C
He
Ａ
18
Temperature (measured)
昇温曲線
100
Rate of evolution (wtppm/sec)
120
The TPD-MS is used to determine the amount of gas
desorbed from the heated sample as a function of heating
time or temperature. Thermal Desorption (TD) - GC/MS
method allows to analyze organic gases in more detail.
Sample
【Temperature program simulating the curing process】
1)Heated from 28℃ to 100℃ under 10℃/min 20
2)Held at 100℃
The result of TPD-MS
EGA of a adhesive in curing process
m/z 88
m/z
3
Ｄ
m/z
m/z 98
O
C H3C C H=C C H3
C H3
0
5
10
15
20
25
30
35
0
5
10
15
Time（min）
【Temperature program】
Range：28～160℃
Heating rate：10℃/min
フッ素系フィルム
Fluorinated
resin film
Epoxy熱硬化性エポキシ
resin (Thermoset)
フッ素系フィルム
Fluorinated
resin film
MS
発生速度/wtppm･sec-1
Rate of evolution (wtppm/sec)
EGA using TPD-MS can simulate the process of
laminating the fluorinated resin films.
Oven
30
35
8 .5
EGA in the laminating process
Oven
25
In the region B, evolution of the constituent from a base resin
is observed.
In the region A, volatilization of solvents is observed mainly.
He
20
Time（min）
有
機 シ リコof
ーaンbase
（主 resin
剤由来）
constituent
7 .5
6 .5
5 .5
4 .5
Solvent
溶 剤 AA
3 .5
2 .5
1 .5
溶 剤BB
Solvent
0 .5
Constituent
ofィル
a fluorinated
フッ素フ
ム 由 来resin
-0.5
20
40
60
80
100
120
140
160
Temperature (℃)
温 度 /℃
- Sample assembly -
From ca. 30℃, volatillization of solvents is observed. At higher than ca.100℃, evolution
of constituent of a fluorinated resin as well as a base resin is observed simultaneously.
P01117材料物性第１研究室20131107
STC：開(20141121)

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