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1. ThermoGravimetric Analysis TGA
I.Process: weight changes of a specimen as a function of temperature
II.General instrumentation
Temperature Programmer
Furnace
S
Amplifier and data
collection
Display-Recorder
computer
Gas in Sensor
assembly
4
TGA instrumentation:
Calibration:
Temperature calibration: use of a reference with a known Curie point
Mass calibration: use of a reference with exact known mass
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How a typical microbalance works?
-A balance beam which is connected to the sample cup and a magnetic coil through
its two extremes Principles of Insturmental Analysis 6th ed.,
Skoog, Holler and Crouch
-There is a lamp and two photodiodes
-A permanent magnet surrounding the coil
T1 T1<T2 T2
MetalA
Types:
e
K: chromel-alumel
E: chromel-Constantan
HEAT V
J: iron-constantan
N: nicrosil-nisil MetalB
e
Pt types
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Applications of thermogravimetry
i.Analysis of mixtures
Each part of a mixture behaves differently with temperature change
ii.Oxidation studies
Study of the oxidation of metals at a constant temperature
iii.Reduction studies
Study of the reduction of a solution/suspension of metal(s)
iv.Exact chemical identification
Different TGA behaviours of identical samples with different history
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Undergraduate Instrumental Analysis 6th Ed.,
Robinson, Frame and Frame
CaC2O4.H2O CaC2O4 + H2O T ~ 100 C
CaC2O4 CaCO3 + CO T ~ 500 C
CaCO3 CaO + CO2 T ~ 800 C 9
Analysis of mixtures
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Polymer Degradation and Stability
91 (2006) 3312
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Principles of Insturmental Analysis 6th ed., Skoog, Holler and Crouch 12
N2
O2
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2. Differential Scanning Calorimetry DSC
1.Power-compensated DSC
1. Separate heating of sample and reference
2. Identical temperature difference
3. Measurement of electrical power
2.Heat flux DSC
1. In-concert heating of sample and reference
2. Measurement of temperature change
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DSC (Power Compensated )
Furnace
S R
Display-Recorder
computer
Sensor
Gas assembly
in
Amplifier and data
collection
Programmer
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DSC (and DTA) instrumentation:
Calorimetry
Measuring the heat of physical/chemical interactions
Heat capacity
The amount of heat needed to increase temperature of a substance
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Calibration:
1.Baseline: correction for the baseline slope of a blank run (no pan)
2.Heat flux and temperature: melting a reference (Indium) of known heat flux
3.Heat capacity: use of a reference of known heat capacity (i.e. sapphire)
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Hyphenated techniques
I. TGA-DSC
II. TGA-DTA
III. TGA (or DTA, DSC)-MS
IV. TGA (or DTA, DSC)-GC
V. TGA (or DTA, DSC)-GCMS
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Thermal analysis
Advantages
Accurate
Low detection limit (up to 10-7 g)
Reliable data
Easy to use
Rather cheap
Minimal sample preparation
Disadvantages
Destructive
Limited range of samples
Time consuming
Usually not qualitative
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TO-KNOW LIST
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