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Thermogravimetric Analysis (TGA)
Thermogravimetric Analysis (TGA)
Sample % Furnace Magnet Attraction of Sample to Magnet Results in Initial Weight Gain Offset temp
200
350
400
TGA
-5
-10
Weight (g)
-15
-20
Weight (g)
-10
600.00C -20.10g
-20
600.00C -25.04g
-30 0 200 400 600 800 1000
Temperature (C)
-5
Weight (g)
20C/min
-10
-15
50C/min
-20
-25
Most TGA instruments have baseline drift of +/-0.025mg which is 0.25% of a 10mg sample
PI
60 40 20 0 0
wt. : 10 mg prog.: 5C atm.,: N
2
100
200
700
800
Weight (%)
50
size: prog: atm: 8 mg 6C/min 300 Pa vacuum
P - MS
PS
100
400
500
10 8
19.2% CO
6 4
30.0% CO2
2 0
-2 1000
100
23%
WEIGHT PERCENT
390
50
Vinyl acetate (VA) %= wt loss of acetic acid x mol wt of VA / mol weight of acetic acid
VA(%) = 23% x
0 200
86.1 = 33 60.1
600
700
80 Weight (%)
Switch to Air
60
1.0
40
0.5
20
24.96% Carbon Black + Ash (5.656mg)
0.0
-0.5
WEIGHT CHANGE
50 25
0 10
20
30
40 50 60 TIME (Min.)
70
80
90
Means of Enhancing Resolution Slower Heating Rate Reduced Sample Size Change Purge Gas Pin-hole Hermetic Pans
Heating stops (isothermal) once a certain operator defined weight loss rate is exceeded then restarts after this rate falls below a second operator defined value.
100
90
88
80 [
78 [
70 300
350
400
450
500
68 550
Exit.TH Ent. TH
1/ 20 1/10 1/5 1/2 1/1.7
P
30
Entrance Threshold: Entrance Threshold: 1/10 (P) 1/10 (P) Exit Threshold: Exit Threshold: <1/10 (Ent. TH) <1/10 (Ent. TH)
20 10 0
120 100 80 Weight (%) 60 40 20 0 -20 0 100 200 300 400 500 Temperature (C) 600 700
Weight (%)
200
300
500
600
Conversion
95
size: 60mg atm.: N 2
90
10%
85
80
Overview of Mass Spectrometry Vacuum Requirements Ion Creation Ion Filtering Ion detection
Mass Spectroscopy
A gas phase compound is ionized, accelerated, then filtered according to its mass to charge ratio and detected The ionization process typically breaks the compound into fragments, each with its own mass to charge (m/e) ratio The largest m/e detected is called the parent ion and corresponds to the molecular weight of the compound. The pattern of fragments detected is the mass spectrum of the compound and can be used for qualitative identification
Vacuum Requirements
e-
Filament Longevity
H H
C = 12 A.M.U.
= Electron ~ 0 AMU = Neutron ~ 1 AMU = Proton ~ 1AMU
Isotope Patterns
Isotope Patterns
Isotope Patterns
Ionization
Atom
12
Ion
12
C + 1e-
C+ + 2e-
Ionization
Double Ionization
1 e- +
12C
m/e=6
12C++
+ 3e-
Fragmentation - Ionization
m/e=17 1 e- +
18H2O
1 e- +
17OH
1 e- +
17OH
17OH+
+2 e-
Key fragments
C++ C++ C++ C+ C+ C+ N+ N+ CH2+ CO++ O+ O+ CH4+ NH2+ OH+ NH3+ H2O+
16
17 18
Natural Abundance's
18O
= 0.2% = 1.1%
13C
Filaments
Ions Out
Gas In
10-05
10-04
10-03
10
Pressure (mBar)
Mass Filter
+ -
Cylindrical Rods. Stainless Steel or Molybdenum. Opposite Rods are Connected Electrically. Alignment is Critical not adjustable.
Mass Filter
y z x
+
+ + + + +
e-
SEM
Ii
Selected m/e ion - reaches detector Higher m/e ion - deflected in z-axis Lower m/e ion - deflected in y-axis
Ii
e-
I i ~ 10-14....10-9 A
= Selected ion - positive charge
Indestructible Detector but gain = unity. Cannot detect small ion currents <10-14 Amps. (Limit depends on electrometer only)
e-
Ii
eCan be destroyed by high currents >10-5 Amps , or by operation at high pressure.
I i ~ 10-14....10-5 A
ThermoStar
Pressure Conditions in the Gas Inlet
Gas In
Transport vacuum
5 x 10-6
10-4
CONNECTOR
TGA FURNACE
1 mm GAP
TEFLON SEAL
Silica Capillary
Mass-Spec Benefits
Additional information for the interpretation of the reactions in the TGA results Sensitive method for the analysis of gaseous reaction products Exact control of the furnace atmosphere before starting and during the experiment Location of air leaks around the furnace
TGA
10
8 100
80
4 60 2
40 0
Weight (%)
200
400
600
800
Temperature (C)
TGA-MS
Sample: 583-35-E Size: 19.6330 mg
TGA
4
98
3 96
Weight (%)
2 94 1
92 0
TGA-MS
MS Intensity
Mass 56 (Hydrocarbon)
100 80 60
PVC Benzene (78 amu)
MS Intensity
40 20 0
PVC + MoO 3
100
500
100
500