热重分析 TGA 完整版
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losses associated with volatilization or small amounts of residue.
• Run clean, empty, tared pan, over temperature
range of interest, at desired heating rate.
80
60
40
20
0
0
100
200
300
400
Temperature (°C)
Polystyrene 17.6 mg Polystyrene 10.2 mg Polystyrene 5.4 mg Polystyrene 2.7 mg
500
600
Universal V4.2D TA Instruments 16
800
1000
Temperature (°C)
Universal V3.4A TA Instruments
Weight (%) Deriv. Weight (%/min)
TGA: The Technique
Thermo gravimetric Analysis (TGA) measures the amount and rate of change in the weight of a material as a function of temperature or time in a controlled atmosphere.
pin-hole lid
13
TGA: Sample Pan Selection
• Platinum (useful for most materials)
Easy to Clean Nonporous Alloys with most metals
• Alumina (Ceramic)
Corrosives/Inorganics Large samples
18
Pan Shape Effect – Amorphous PMMA
120
100
365.01癈 369.13癈
80
Weight (%)
60
4.6mg; spread evenly
40
4.6mg; in tall S.S. pan (150 mg)
20
0
-20 0
100
200
300
400
500
Temperature (癈 )
which they occur).
4
TG曲线 积分型曲线
DTG曲线 微分型曲线
5
初始热分解 温度(B、G)
最大失重 速率温度
反应终了温 度(C、H)
6
影响热重测定的因素: Purge Gas
• TGA: Always purge through balance housing with dry inert gas • TGA: Only introduce reactive/corrosive gases through sample
• Plot weight in µg vs. temperature.
11
TGA: Accurate Residuals
120
Polyolefin
4
100
2 80
60
0
Expanded Scale
0.28%
Weight (%)
40 -2
20
Baseline
0
-20 0
200
400源自文库
600
800
1000
热稳定性
• Oxidative Stability of Materials
氧化稳定性
• Composition of Multi-component Systems 组成
• Estimated Lifetime of a Product
产品寿命
• Decomposition Kinetics of Materials
40
20
0
0
100
200
300
400
500
600
Temperature (癈 )
Universal V3.8A TA Instruments
20
Shift in Onset with Ramp Rate
120
100
524.26°C 563.82°C
80
60
Weight (%)
40
20
0
-20
400
80
60
Weight (%)
40
20
0
-20
20
40
60
80
100
120
140
160
180
Time (min)
Universal V3.7A TA Instruments
22
Q5000 IR – High-Heating Rate TGA Analysis
23
Typical Applications
Weight (%)
Effect of Heating Rate
100
80
60
40
20
0
0
100
200
300
400
Temperature (°C)
Polystyrene 20°C/min Polystyrene 10°C/min Polystyrene 5°C/min Polystyrene 1°C/min
in the oxidative stability (versus thermal stability) of components. 气氛不同反应机理的不同。
7
TGA: Purge Gas Flow
40ml/min
10ml/min
90ml/min
Standard Furnace
60ml/min
350
400
450
500
550
600
Temperature (°C)
10
TGA: Baseline Considerations
• Good way to quantify how the TGA/SDT is working. • Especially important for measuring small weight
650.00°C 55.59%
PEEK
650.00°C 14.32%
Weight (%)
0 50
650.00°C 5.928%
250
450
650
850
1050
0
40 0
-1
100
200
300
400
500
600
Temperature (°C)
9
Effect of Oxygen on Copper Oxalate Decomposition
46
45
Weight (%)
44
High Oxygen
43
Medium Oxygen
42
Low Oxygen
41
300
•Thermal Stability •Compositional Analysis •Oxidative Stability
24
Thermal Stability of Polymers
100
PVC
80
PMMA
60
PET
40
LDPE
20
Method Log: 1:Select gas: 1 - N2 2: Ramp 20.00 °C/min to 650.00 °C 3: Select gas: 2 - Air 4: Ramp 20.00 °C/min to 1000.00 °C
分解动力学
• The Effect of Reactive or Corrosive Atmospheres
on Materials
反应或腐蚀气氛对材料的影响
• Moisture and Volatiles Content of Materials
材料水分和挥发份含量
3
Mechanisms of Weight Change in TGA
100 µL
100 µL
Platinum and Aluminum pans have attached wire bail.
250 µL
500 µL
Ceramic pans have removable wire bail.
15
Weight (%)
Effect of Sample Size
100
450
500
550
600
Temperature (°C)
2.5°C/min 5°C/min 10°C/min 20°C/min
650
700
Universal V3.7A TA Instruments
21
Time to Complete Degradation
120
100
2.5°C/min 5°C/min 10°C/min 20°C/minj
Temperature (°C)
Universal V3.9A TA Instrume1n2ts
TGA: Sample Preparation (cont.)
• Use brass tweezers to eliminate static effects • Tare a clean sample pan before every run • Distribute sample evenly over bottom of pan • Liquid samples - use hermetic pan with a
Desorption. Weight Gain:
Oxidation: Interaction of the sample with an oxidizing atmosphere. Absorption.
All of these are kinetic processes (i.e. there is a rate at
热重分析(TGA)
Theory & Applications
120 100
80 60 40 20
0
12.57% Water (0.8753mg)
6
19.47% Carbon Monoxide (1.355mg)
4
30.07% Carbon Dioxide (2.093mg)
2
0
-2
200
400
600
Universal V3.8A TA Instruments
19
Sample Morphology Effects – PET
120
419.58癈 424.58癈
100
80
Weight (%)
60
2.9 2m.9gm; ga;mamoorrpphhoouussPEPTET
2.8 mg2.;8smegm; cir-ycsrtaylslintaelPlinETe PET
•样品在热环境中发生化学变化、分解、成分改变时可能伴随着重量的 变化。 •热重分析就是在不同的热条件（以恒定速度升温或等温条件下延长时 间）下对样品的质量变化加以测量的动态技术。
热重分析的结果用热重曲线或微分热重曲线表示。
2
What TGA Can Tell You
• Thermal Stability of Materials
Weight Loss:
Decomposition: The breaking apart of chemical bonds. Evaporation: The loss of volatiles with elevated temperature. Reduction: Interaction of sample to a reducing atmosphere (hydrogen, ammonia, etc).
• Aluminum (TGA) (designed for one-time use)
Lower cost Lower temperature limit (<=600°C)
14
TGA: Sample Pans - Types/Sizes
Platinum Aluminum
Ceramic
50 µL
500
600
17
Mass Effect – Semi-crystalline PE
120
436.28癈 457.57癈
100
80
Weight (%)
60
0.492mg
40
48.422mg
20
0
-20 0
100
200
300
400
500
600
Temperature (癈 )
Universal V3.8A TA Instruments
area/furnace housing • Nitrogen most common. • Helium often provides best baseline but will make furnace
work hard at high temperature. • Air can sometimes improve resolution because of differences
EGA Furnace
8
Test for Oxygen Contamination of N2 Purge Gas
120
3
Copper Oxalate
320.79°C
+
100
2
Weight (%) [------------] Deriv. Weight (%/°C)
80
1
60 10 minute N2 pre-purge
• Run clean, empty, tared pan, over temperature
range of interest, at desired heating rate.
80
60
40
20
0
0
100
200
300
400
Temperature (°C)
Polystyrene 17.6 mg Polystyrene 10.2 mg Polystyrene 5.4 mg Polystyrene 2.7 mg
500
600
Universal V4.2D TA Instruments 16
800
1000
Temperature (°C)
Universal V3.4A TA Instruments
Weight (%) Deriv. Weight (%/min)
TGA: The Technique
Thermo gravimetric Analysis (TGA) measures the amount and rate of change in the weight of a material as a function of temperature or time in a controlled atmosphere.
pin-hole lid
13
TGA: Sample Pan Selection
• Platinum (useful for most materials)
Easy to Clean Nonporous Alloys with most metals
• Alumina (Ceramic)
Corrosives/Inorganics Large samples
18
Pan Shape Effect – Amorphous PMMA
120
100
365.01癈 369.13癈
80
Weight (%)
60
4.6mg; spread evenly
40
4.6mg; in tall S.S. pan (150 mg)
20
0
-20 0
100
200
300
400
500
Temperature (癈 )
which they occur).
4
TG曲线 积分型曲线
DTG曲线 微分型曲线
5
初始热分解 温度(B、G)
最大失重 速率温度
反应终了温 度(C、H)
6
影响热重测定的因素: Purge Gas
• TGA: Always purge through balance housing with dry inert gas • TGA: Only introduce reactive/corrosive gases through sample
• Plot weight in µg vs. temperature.
11
TGA: Accurate Residuals
120
Polyolefin
4
100
2 80
60
0
Expanded Scale
0.28%
Weight (%)
40 -2
20
Baseline
0
-20 0
200
400源自文库
600
800
1000
热稳定性
• Oxidative Stability of Materials
氧化稳定性
• Composition of Multi-component Systems 组成
• Estimated Lifetime of a Product
产品寿命
• Decomposition Kinetics of Materials
40
20
0
0
100
200
300
400
500
600
Temperature (癈 )
Universal V3.8A TA Instruments
20
Shift in Onset with Ramp Rate
120
100
524.26°C 563.82°C
80
60
Weight (%)
40
20
0
-20
400
80
60
Weight (%)
40
20
0
-20
20
40
60
80
100
120
140
160
180
Time (min)
Universal V3.7A TA Instruments
22
Q5000 IR – High-Heating Rate TGA Analysis
23
Typical Applications
Weight (%)
Effect of Heating Rate
100
80
60
40
20
0
0
100
200
300
400
Temperature (°C)
Polystyrene 20°C/min Polystyrene 10°C/min Polystyrene 5°C/min Polystyrene 1°C/min
in the oxidative stability (versus thermal stability) of components. 气氛不同反应机理的不同。
7
TGA: Purge Gas Flow
40ml/min
10ml/min
90ml/min
Standard Furnace
60ml/min
350
400
450
500
550
600
Temperature (°C)
10
TGA: Baseline Considerations
• Good way to quantify how the TGA/SDT is working. • Especially important for measuring small weight
650.00°C 55.59%
PEEK
650.00°C 14.32%
Weight (%)
0 50
650.00°C 5.928%
250
450
650
850
1050
0
40 0
-1
100
200
300
400
500
600
Temperature (°C)
9
Effect of Oxygen on Copper Oxalate Decomposition
46
45
Weight (%)
44
High Oxygen
43
Medium Oxygen
42
Low Oxygen
41
300
•Thermal Stability •Compositional Analysis •Oxidative Stability
24
Thermal Stability of Polymers
100
PVC
80
PMMA
60
PET
40
LDPE
20
Method Log: 1:Select gas: 1 - N2 2: Ramp 20.00 °C/min to 650.00 °C 3: Select gas: 2 - Air 4: Ramp 20.00 °C/min to 1000.00 °C
分解动力学
• The Effect of Reactive or Corrosive Atmospheres
on Materials
反应或腐蚀气氛对材料的影响
• Moisture and Volatiles Content of Materials
材料水分和挥发份含量
3
Mechanisms of Weight Change in TGA
100 µL
100 µL
Platinum and Aluminum pans have attached wire bail.
250 µL
500 µL
Ceramic pans have removable wire bail.
15
Weight (%)
Effect of Sample Size
100
450
500
550
600
Temperature (°C)
2.5°C/min 5°C/min 10°C/min 20°C/min
650
700
Universal V3.7A TA Instruments
21
Time to Complete Degradation
120
100
2.5°C/min 5°C/min 10°C/min 20°C/minj
Temperature (°C)
Universal V3.9A TA Instrume1n2ts
TGA: Sample Preparation (cont.)
• Use brass tweezers to eliminate static effects • Tare a clean sample pan before every run • Distribute sample evenly over bottom of pan • Liquid samples - use hermetic pan with a
Desorption. Weight Gain:
Oxidation: Interaction of the sample with an oxidizing atmosphere. Absorption.
All of these are kinetic processes (i.e. there is a rate at
热重分析(TGA)
Theory & Applications
120 100
80 60 40 20
0
12.57% Water (0.8753mg)
6
19.47% Carbon Monoxide (1.355mg)
4
30.07% Carbon Dioxide (2.093mg)
2
0
-2
200
400
600
Universal V3.8A TA Instruments
19
Sample Morphology Effects – PET
120
419.58癈 424.58癈
100
80
Weight (%)
60
2.9 2m.9gm; ga;mamoorrpphhoouussPEPTET
2.8 mg2.;8smegm; cir-ycsrtaylslintaelPlinETe PET
•样品在热环境中发生化学变化、分解、成分改变时可能伴随着重量的 变化。 •热重分析就是在不同的热条件（以恒定速度升温或等温条件下延长时 间）下对样品的质量变化加以测量的动态技术。
热重分析的结果用热重曲线或微分热重曲线表示。
2
What TGA Can Tell You
• Thermal Stability of Materials
Weight Loss:
Decomposition: The breaking apart of chemical bonds. Evaporation: The loss of volatiles with elevated temperature. Reduction: Interaction of sample to a reducing atmosphere (hydrogen, ammonia, etc).
• Aluminum (TGA) (designed for one-time use)
Lower cost Lower temperature limit (<=600°C)
14
TGA: Sample Pans - Types/Sizes
Platinum Aluminum
Ceramic
50 µL
500
600
17
Mass Effect – Semi-crystalline PE
120
436.28癈 457.57癈
100
80
Weight (%)
60
0.492mg
40
48.422mg
20
0
-20 0
100
200
300
400
500
600
Temperature (癈 )
Universal V3.8A TA Instruments
area/furnace housing • Nitrogen most common. • Helium often provides best baseline but will make furnace
work hard at high temperature. • Air can sometimes improve resolution because of differences
EGA Furnace
8
Test for Oxygen Contamination of N2 Purge Gas
120
3
Copper Oxalate
320.79°C
+
100
2
Weight (%) [------------] Deriv. Weight (%/°C)
80
1
60 10 minute N2 pre-purge