About OMICS Group
OMICS Group International is an amalgamation of Open Access
publications and worldwide international science conferences and
events. Established in the year 2007 with the sole aim of making the
information on Sciences and technology ‘Open Access’, OMICS
Group publishes 400 online open access scholarly journals in all
aspects of Science, Engineering, Management and Technology
journals. OMICS Group has been instrumental in taking the
knowledge on Science & technology to the doorsteps of ordinary
men and women. Research Scholars, Students, Libraries,
Educational Institutions, Research centers and the industry are main
stakeholders that benefitted greatly from this knowledge
dissemination. OMICS Group also organizes 300 International
conferences annually across the globe, where knowledge transfer
takes place through debates, round table discussions, poster
presentations, workshops, symposia and exhibitions.
About OMICS Group Conferences
OMICS Group International is a pioneer and leading science
event organizer, which publishes around 400 open access
journals and conducts over 300 Medical, Clinical, Engineering,
Life Sciences, Phrama scientific conferences all over the globe
annually with the support of more than 1000 scientific
associations and 30,000 editorial board members and 3.5 million
followers
to
its
credit.
OMICS Group has organized 500 conferences, workshops and
national symposiums across the major cities including San
Francisco, Las Vegas, San Antonio, Omaha, Orlando, Raleigh,
Santa Clara, Chicago, Philadelphia, Baltimore, United Kingdom,
Valencia, Dubai, Beijing, Hyderabad, Bengaluru and Mumbai.
Precise Heat Control.
Essential Materials Characterization
Techniques Everyone Needs to Solve
Real Problems
Rodrigo Devivar, Ph.D.
Jacobs Technology / NASA-Johnson Space Center
ES4 Materials Analysis Laboratory
Houston, Texas
Controlling Heat in Aerospace
Picture of Space Shuttle During Atmospheric Re-entry
taken from ISS
Analytical Chemistry Laboratory Equipment
Key Laboratory Equipment
–
–
–
Optical Instrumentation
• UV-Vis, Fluorimeter, Solar Reflectance,
Infrared Emittance, Raman
Thermal Analysis Instrumentation
• DSC, DMA, TGA, TMA, LFA, Rheometer
Chemical Analysis Instrumentation
• FT-IR, Ion trap GC-MS, Py-GC-MS, TGAMS, TGA-IR
Optical Vs. Thermal Techniques
Light
Heat
Reflectance
Emittance
Absorbance/Transmission
Fluorescence
UV-Vis Absorbance
FT-IR Analysis
Raman Analysis
Material Curing
Thermal Transition-Tg
Melting Point/ Boiling Point
Residual Solvent
Identification of additives
Material Decomposition
Elimination of labile functional groups
Identification of Material Components
Identification of Inorganic Components
Controlling Heat Exposure
Thermal Analysis
Slow: minutes to hours
TGA
Furnace
Sample at 1000oC
Sample at 25oC
Pyrolysis
Filament
Fast: microseconds to seconds
Thermochemical Analysis
Thermogravimetric Analysis (TGA)
• A TGA instrument consists of an analytical balance and a furnace.
• A small sample of material is heated and its change in mass is
measured as a function of temperature.
• Experiments can be conducted under inert or oxidizing atmospheres.
• Information gained from TGA includes:
– Thermal stability for conducting additional thermal analysis
– Identification of the number of components in the sample if the
decomposition temperatures are different
– Residual mass for assessing the extent of inorganic additives
The Influence of Temperature Ramp Rates
Slower Ramp
Faster Ramp
Pyrolysis for GC-MS of Solids
•
Sample size is relatively small:
50 to 200 mg is sufficient for solids
50 to 200 nL is sufficient for liquids
•
Sample preparation is easy:
Place sample inside 1.5 inch
quartz tube containing filler tube
and plug with glass wool.
•
Samples can be solids, gels,
viscous liquids, greases,
crystalline, emulsions, foams,
fabrics
•
Pyrolysis temperatures are
almost instantaneous
•
Sample components can be
quantified with the use of
software
Pyrolysis is the thermal degradation of any substance through the fast application of heat.
Pyrolyzers: Filament Versus Furnace
CDS Platinum Filament
Microfurnace
•
•
•
Heating Rate:
~20,000oC per sec
Max Temperature: 1400oC
Cooling Rate:
> 1000oC per sec
•
•
•
Heating Rate:
~50oC per min
Max Temperature: 800oC
Cooling Rate:
25oC per min
•
Fast Heating, Fast Cooling
•
Slow to Heat, Slow to Cool
Flash Pyrolysis of Polymers
Chromatogram Plots
G C ps
Mechanism of
Pyrolytic Degradation
Random Scission
Polyethylene:
TIC; PE std 750 3min.xms; Filtered
-CH2-CH2-CH2-CH2-CH2-CH2-CH2-CH
2-CH2-
5
4
3
2
1
0
TIC; PTFE 750 3min.xms; Filtered
Unzipping
G Cps
12.5
PTFE :
-CF2-CF2-CF2-CF2-CF2-CF2-CF2-CF2-CF2-
10.0
7.5
5.0
2.5
0.0
TIC; PVC test SP2 750.xms; Filtered
PVC:
4
G C ps
Side Group Elimination
-CH2-CH-CH2-CH-CH2-CH-CH2-CH-CH2-CH-
3
Cl
Cl
Cl
Cl
Cl
2
1
0
TIC; PDMS std.XMS; Filtered
Silicones :
5
G C ps
Silicone Scission
-O-Si(CH3)2-O-Si(CH3)2-O-Si(CH3)2-O-Si(CH3)2-
4
3
2
1
0
5.0
7.5
10.0
12.5
15.0
minutes
Thermal Analysis of Composite
Thermal Analysis
Thermal Desorption
Pyrolysis
Onset of
Decomposition
Curing
Temperature
Tg
Flash Pyrolysis-GC-MS of Ultem 1000
Relay sensor boxes along the shuttle’s wing
leading edge were composed of Ultem 1000.
One lot used to make these relay sensor
boxes had failed
Various manufacture lots of sensor boxes
were analyzed by Py-GC-MS and an extra
peak was noted in one of those lots. The
extra peak was due to dichlorobenzene, a
solvent used during manufacture of Ultem
1000.
Chromatogram Plots
RIC Merged ultem_1_750.xms 1200 CENTROID RAW
+ 10.235 min
10.570 min
9.988 min
9.448 min
9.102 min
9.193 min
8.730 min
7.756 min
8.002 min
8.181 min
6.277 min
5.414 min
4.077 min
100
4.380 min
200
4.805 min
300
7.414 min
+ 5.696 min
400
6.584 min
6.767 min
+ 6.023 min
500
7.140 min
5.237 min
600
9.879 min
6.665 min
700
8.514 min
7.839 min
MCounts
800 (+) EI Q1MS 10.0 - 800.0 >
0
9.824 min
9.939 min
+ 9.578 min
9.516 min
+ 9.134 min
8.874 min
8.407 min
+ 8.061 min
7.074 min
7.425 min
5.904 min
+ 4.760 min
0
MCounts
300
+ 5.163 min
4.440 min
200
+ 5.679 min
+ 5.349 min
300
100
7.549 min
6.811 min
4.895 min
6.338 min
(+) EI Q1MS 10.0 - 800.0 >
400
RIC Merged ultem_2_750.xms 1200 CENTROID RAW
8.197 min
MCounts
RIC Merged ultem_3_750.xms 1200 CENTROID RAW
(+) EI Q1MS 10.0 - 800.0 >
5
6
7
9
9.890 min
9.471 min
+ 9.089 min
8.829 min
+ 8.027 min
8
+ 8.363 min
+ 9.529 min
+ 7.472 min
7.431 min
7.636 min
50
4.402 min
100
5.307 min
5.118 min
150
6.773 min
6.293 min
200
9.777 min
8.148 min
250
10
11
minutes
Thermal Analysis of Ultem 1000
Key thermal values can be
measured or obtained from
product specification information.
Ultem 1000 Tg: 218oC
Onset of Decomposition: 437oC
-0.2
120
Ultem 1000 DSC
Ultem 1000 TGA
436.86°C
99.37%
-0.4
100
-0.6
80
-1.0
Weight (%)
Heat Flow (W/g)
218.60°C(I)
-0.8
-1.2
60
-1.4
-1.6
0
Exo Up
200
400
600
Temperature (°C)
800
40
1000
Universal V4.3A TA Instruments
Thermal Extraction of Ultem 1000
Thermal extraction
temperature:
400oC
MS Data Review Active Chromatogram and Spectrum Plots - 7/18/2014 2:51 PM
File: c:\brukerws\data\082013\ult 300.xms
Sample: ult 300
Scan Range: 1 - 1327 Time Range: 1.20 - 12.43 min.
Operator: RDevivar
Date: 7/18/2014 2:36 PM
TIC; ult 300.xms; Filtered
1A
500
M C ps
400
300
200
100
4
5
6
7
8
9
10
Spectrum 1A
11
minutes
6.558 min, Scan: 634, Merged
145.9
7.904e+7
100%
75%
147.9
5.092e+7
50%
111.0
3.216e+7
75.1
1.771e+7
25%
74.1
149.9
9.101e+6 8.196e+6
0%
0
250
500
750
1000
m/z
Neutral Buoyancy Training Facility
The NBL tank is 202 feet (62 m) long, 102 feet (31 m) wide, and 40 feet 6 inches (12.34 m)
deep, and contains 6.2 million gallons (23.5 million litres) of water.
The facility is essential for astronaut EVA training prior to a mission.
On one occasion, a Viton gasket from the Canadarm hydraulics swelled and failed. We
implemented a few thermal techniques to reveal the cause of the failure.
TGA Comparison of Gaskets
120
––––––– 16435 New.002
––––
16435 old.002
1.5
80
1.0
Weight (%)
Area of
difference
60
0.5
40
0.0
20
0
200
400
600
Temperature (°C)
800
Deriv. Weight (%/°C)
100
2.0
-0.5
1000
Universal V4.7A TA Instruments
Under conditions of increasing temperature, the only difference between the two Viton
Gaskets was found below 400oC, where the old sample lost a larger percentage of its mass
compared to the new sample.
Thermal Extraction of Samples
Chromatogram Plots
75
New Sample
Carbon
Dioxide
+ 1 .1 9 9 m in
100
16435 New 400C.xms 10.0:800.0>
10.0:800.0>
1 .3 5 3 m in
MCounts
125
50
25
MCounts
Carbon
Dioxide
1,4-Dioxane
16435 Old 400C.xms 10.0:800.0>
10.0:800.0>
O
OH
O
O
OH
7 .1 8 6 m in
HO
Glycerin
50
In Service Sample
BHT
1 .5 9 3 m in
HO
8 .4 8 5 m in
75
+ 1 .3 6 5 m in
100
O
O
HO
O
OH
25
2.5
5.0
7.5
10.0
12.5
15.0
minutes
Thermal extraction of the two samples was performed to account for the difference observed in the TGA
experiments at temperatures below 400oC. Such an experiment indicated the Old sample contained various
fragments that are attributed to polyethylene oxide. Other substances found included Glycerin and Butylated
hydroxy toluene (BHT).
FT-IR Analysis of Silicone Materials
1. Silicone O-ring
2. RTV 560
3. Red, Tacky RTV
4. PDMS
FT-IR is a non-destructive technique
that is very diagnostic. However, if
infrared light cannot penetrate the
sample, any signal obtained through
reflectance is only valid for the external
surface of a sample.
Thermal Analysis of Silicone Materials
100
350.65°C
96.30%
80
0.0
–––––––
––––
––––– ·
––– – –
PDMS
Red Tacky RTV
RTV 560
Silicone O-ring
-0.4
60
Heat Flow (W/g)
Weight (%)
-0.2
-0.6
-0.8
40
-1.0
-1.2
-100
-80
-60
-40
-20
0
Temperature (°C)
Exo Up
20
–––––––
––––
––––– ·
––– – –
20
40
Universal V4.3A TA Instruments
RTV 560
Silicone O-ring
Tacky RTV
PDMS
0
0
100
200
300
400
500
Temperature (°C)
600
700
800
900
Universal V4.7A TA Instr
The Silicone samples that were nearly identical by FT-IR displayed very different
properties by thermal analysis.
TGA Analysis of Silicone Oil
120
–––––––
––––
––––– ·
––– – –
––– –––
––––– –
–– –– –
–––––––
100
Ramp at 2C/min
Ramp at 5C/min
Ramp at 10C/min
Ramp at 50C/min
Ramp at 75C/min
Ramp at 100C/min
Ramp at 125C/min
Ramp at 200C/min
Weight (%)
80
60
40
20
0
0
200
400
600
Temperature (°C)
800
1000
Universal V4.7A TA Instruments
The thermal profile of silicone oil at different ramp rates indicates the complexity of thermal analysis
High Temperature Ramp Rates
Increase Molecular Fragmentation
At high temperature ramp rates, silicone oil undergoes two types of processes
detected by TGA analysis, evaporation through boiling and molecular fragmentation.
Pyrolytic Analysis of Silicone Oil at Different Heating Rates
Chromatogram Plots
TIC;
Silicone oil 0_5CPS.xms;
GCps
3
Filtered
Heating Rate: 30oC per min
2
1
0
TIC;
Silicone oil 1Cps.xms;
Filtered
3.0
GCps
2.5
Heating Rate: 60oC per min
2.0
1.5
1.0
0.5
0.0
GCps
TIC;
Silicone oil 2CPS001.xms;
6
5
4
3
2
1
0
Filtered
Heating Rate: 120oC per min
TIC;
Silicone oil 5Cps.xms;
Filtered
GCps
4
Heating Rate:
3
300oC
per min
2
1
0
TIC;
Silicone oil 10C pe.xms;
Filtered
GCps
10.0
Heating Rate: 600oC per min
7.5
5.0
2.5
0.0
TIC;
GCps
7.5
Siliconeoil 750Cpy.xms;
Filtered
Flash Pyrolysis
5.0
2.5
0.0
5
10
15
20
25
minutes
Pyrolysis provides insight into the TGA data. Pyrolysis indicates that silicone oil stays
intact and simply boils off at heating rates of 30oC/min. The oil starts to display
substantial fragmentation at 120oC
FEP Vs. PTFE Teflon
Sample: FEP Teflon N2
Size: 7.2350 mg
Method: Ramp
Sample: PTFE Teflon N2
Size: 5.8520 mg
Method: Ramp
File: D:...\rdevivar\Desktop\FEP Teflon.001
Operator: RDevivar
Run Date: 28-Jun-2013 16:05
Instrument: SDT Q600 V20.9 Build 20
DSC-TGA
120
File: D:...\rdevivar\Desktop\PTFE Teflon.001
Operator: RDevivar
Run Date: 01-Jul-2013 07:42
Instrument: SDT Q600 V20.9 Build 20
DSC-TGA
120
1.0
FEP Teflon
2.0
PTFE
100
0.8
1.5
100
80
0.4
562.04°C
57.61%
Deriv. Weight (%/°C)
Weight (%)
Weight (%)
497.48°C
89.29%
1.0
60
563.05°C
46.16%
40
0.5
Deriv. Weight (%/°C)
80
0.6
521.69°C
81.55%
0.2
20
60
995.85°C
42.90%
0.0
0.0
40
0
200
400
600
800
Temperature (°C)
0
-20
-0.2
1000
0
200
400
600
-0.5
1000
800
Temperature (°C)
Universal V4.7A TA Instruments
Universal V4.7A TA Instruments
Chromatogram Plots
TIC;
FEP 3mindly 750.xms;
Filtered
20
Overlaid Chromatogram Plots
TIC; FEP 3mindly 750.xms; Filtered
TIC; PTFE 3mindly 750.xms; Filtered
15
GCps
20
10
15
5
TIC;
PTFE 3mindly 750.xms;
Filtered
GCps
0
10
15
GCps
5
10
5
0
4.00
0
5
10
15
20
25
minutes
4.25
4.50
4.75
5.00
5.25
minutes
FEP Teflon Heated at Different Rates
Chromatogram Plots
TIC;
FEP 3mindly 750.xms;
Filtered
TIC;
Filtered
20
>1000oC
GCps
15
Heating Rate:
per sec
GC Method run time: 30 min
10
5
0
8
7
6
FEP 2CPM.xms;
120oC
Heating Rate:
per min
GC Method run time: 60 min
GCps
5
4
3
TGA
Sample: FEP Teflon N2
Size: 7.2350 mg
Method: Ramp
2
DSC-TGA
File: D:...\rdevivar\Desktop\FEP Teflon.001
Operator: RDevivar
Run Date: 28-Jun-2013 16:05
Instrument: SDT Q600 V20.9 Build 20
120
1
1.0
0
TIC;
GCps
5
100
Heating Rate:
per min
GC Method run time: 100 min
0.6
521.69°C
81.55%
497.48°C
89.29%
80
0.4
562.04°C
57.61%
4
0.2
60
3
Deriv. Weight (%/°C)
6
0.8
Filtered
Weight (%)
7
FEP 0_2CPM.xms;
12oC
995.85°C
42.90%
0.0
2
1
40
0
200
400
600
Temperature (°C)
0
10
20
30
40
50
60
70
80
-0.2
1000
800
Universal V4.7A TA Instruments
minutes
During pyrolysis, materials undergo thermal degradation via chemical pathways dictated by
the thermal stability of the components. When pyrolysis is slowed to simulate TGA conditions,
a thermal response pattern similar to what was observed with TGA first derivative plot is
observed.
Thermal Analysis of HDPE and LDPE
-CH2-CH2-CH2-CH2-CH2-CH2-CH2-CH2-CH2-
150
–––––––
––––
4
LDPE
HDPE
TGA
3
2
Weight (%)
2
1
50
1
Heat Flow
100
DSC of HDPE vs LDPE
Deriv. Weight (%/°C)
Polyethylene:
0
-1
0
50
100
150
200
250
300
-2
-3
0
0
-4
Temperature
-50
0
200
400
600
-1
1000
800
Temperature (°C)
Universal V4.7A TA Instruments
Chromatogram Plots
MCounts
RIC 1 MAR 14612 lot 2.xms
1200 CENTROID RAW
RIC 1 MAR 14612 lot 1.xms
1200 CENTROID RAW
(+) EI Q1MS 10.0 - 800.0 >
Pyrolysis-GC-MS
50
9.546 min
8.893 min
7.457 min
30
6.655 min
5.779 min
40
20
8.879 min
10
MCounts
10.153 min
9.533 min
+ 9.570 min
+ 8.919 min
8.226 min
8.184 min
C14 C15
C12 C13
7.441 min
6.641 min
C9
C11
7.491 min
C8
3.772 min
C7
2.874 min
2.286 min
1.876 min
30
4.789 min
C6
40
5.764 min
C10
6.694 min
(+) EI Q1MS 10.0 - 800.0 >
50
20
10
2.5
5.0
7.5
10.0
12.5
15.0
minutes
Temperature Ramp Pyrolysis
Heating PE in Pyrolysis chamber from 25oC to 750oC at different rates
Chromatogram Plots
TIC; PE 0_5CPM.xms; Filtered
Heating Rate: 30oC per min
G Cps
6
4
2
0
150
Heating Rate:
6
G C ps
TGA
Heating Rate: 5oC per min
–––––––
––––
TIC; PE 2CPM.xms; Filtered
120oC
per min
4
4
LDPE
HDPE
3
100
2
0
G Cps
0
Heating Rate:
5
4
3
2
1
0
TIC; PE 5CPM.xms; Filtered
300oC
G Cps
0
per min
-50
0
200
400
600
Temperature (°C)
Heating Rate: 600oC per min
5
4
3
2
1
0
TIC; PE 25CPM.xms; Filtered
G Cps
50
1
TIC; PE 10CPM.xms; Filtered
Heating Rate: 1200oC per min
6
4
2
0
TIC; PE test 052913.xms; Filtered
G C ps
2
Weight (%)
G Cps
TIC; PE 3CPM.xms; Filtered
Heating Rate: 180oC per min
5
4
3
2
1
0
Deriv. Weight (%/°C)
G C ps
TIC; PE 1CPM.xms; Filtered
Heating Rate: 60oC per min
5
4
3
2
1
0
Heating Rate: >1000oC per sec
1.5
1.0
0.5
0.0
5
10
15
20
25
minutes
800
-1
1000
Universal V4.7A TA Instruments
Correlating TGA and Pyrolysis Techniques
Chromatogram Plots
Irganox 1076
GCps
TIC; PE 440 3min.xms; Filtered
Py 440oC
2.0
1.0
0.0
GCps
TIC; PE 450 3min.xms; Filtered
Py 450oC
2.0
1.0
0.0
GCps
TIC; PE 460 3min.xms; Filtered
Py 460oC
2.0
1.0
0.0
GCps
TIC; PE 470 3min.xms; Filtered
Py 470oC
2.0
Irganox 1010
1.0
0.0
GCps
TIC; PE 480 3min.xms; Filtered
Py 480oC
2.0
1.0
0.0
440oC
450oC
GCps
TIC; PE 490 3min.xms; Filtered
Py 490oC
2.0
1.0
460oC
470oC
0.0
GCps
TIC; PE 500 3min.xms; Filtered
2.5
2.0
1.5
1.0
0.5
0.0
Py 500oC
GCps
TIC; PE 510 3min.xms; Filtered
2.0
1.5
1.0
0.5
0.0
Py 510oC
TIC; PE SP2 750 3 min.xms; Filtered
Py 750oC
GCps
3
2
1
0
5.0
7.5
10.0
12.5
15.0
17.5
minutes
Pyrolysis at specified temperatures for 20 seconds
480oC
490oC
Thermal Analysis of PE
Pyrolysis at 450oC For Specified Duration
Chromatogram Plots
TIC; PE 450 3min.xms; Filtered
3.0
GCps
2.5
2.0
20 seconds
1.5
Irganox 1076
Sample: PE 5C per min
Size: 2.8770 mg
Irganox 1010
1.0
DSC-TGA
File: D:...\Desktop\PE 5 Cpermin Nitrogen.001
Operator: RDevivar
Run Date: 24-Oct-2013 15:41
Instrument: SDT Q600 V20.9 Build 20
150
4
0.5
440.16°C
92.37%
TIC; PE 450 40sec.xms; Filtered
450.15°C
84.25%
4
40 seconds
2
1
0
TIC; PE 450 60sec.xms; Filtered
2.5
2.0
GCps
3
460.14°C
66.63%
100
Weight (%)
GCps
3
2
470.13°C
34.72%
50
1
60 seconds
480.11°C
4.767%
Deriv. Weight (%/°C)
0.0
1.5
0
1.0
0
0.5
0.0
TIC; PE 450 80sec.xms; Filtered
2.5
GCps
2.0
80 seconds
-50
300
1.0
0.5
0.0
5.0
7.5
400
450
500
Temperature (°C)
Silicone
1.5
350
10.0
12.5
15.0
17.5
minutes
550
-1
650
600
Universal V4.7A TA Instruments
Modification of the thermal parameters at the
onset of TGA degradation for PE can provide
valuable information about the additives or
contaminants.
TGA Analysis of Fluorinated Materials
Krytox 143 AZ
Brayco 815Z
120
––––––– Brayco 815Z oil in N2 to 1000C.001
––––
Brayco 815Z oil in air to 1000C.001
100
Weight (%)
80
60
40
20
0
-20
0
100
200
300
400
Temperature (°C)
100
––––––– Krytox 143AZ oil in N2 to 1000C.001
––––
Brayco 815Z oil in N2 to 1000C.001
80
Weight (%)
60
Krytox 143 AZ
Brayco 815Z
40
20
0
0
200
400
600
Temperature (°C)
800
1000
Universal V3.9A TA Instruments
500
600
700
Universal V3.9A TA Instruments
Thermal Response of Travertine
in Different Atmospheres
100
599.46°C
97.97%
599.46°C
97.25%
Weight (%)
90
80
745.03°C
66.43%
732.56°C
65.50%
70
800.75°C
56.79%
800.75°C
55.58%
60
––––––– Travertine N2
––––
Travertine air
0
200
400
600
Temperature (°C)
800
1000
1200
Universal V4.5A TA Instruments
CaCO3
CaC2 or Calcium Kaolinite
Travertine
Travertine TGA ashes (Helium or Nitrogen)
Travertine TGA ashes (Air)
The Role of Gaseous Atmosphere
During Thermal Decomposition of Travertine
Calcium Carbonate
100
599.46°C
97.97%
599.46°C
97.25%
TGA of Travertine in
Air
Weight (%)
90
80
TGA of Travertine in
Nitrogen
745.03°C
66.43%
732.56°C
65.50%
70
Calcium Kaolinite
800.75°C
56.79%
800.75°C
55.58%
60
––––––– Travertine N2
––––
Travertine air
0
200
400
600
Temperature (°C)
800
1000
1200
Universal V4.5A TA Instruments
Calcium Carbide
TGA Analysis of Geothite in Helium
At 120oC, Mass losses
include: m/z 14 (CH2),
16 (O), 32 (O2)
Goethite
a-FeO(OH)
At 308oC, Mass losses
include: m/z 18 (H2O),
32 (O2)
At 1290oC, Mass losses
include: m/z 16 (O), 18
(H2O), 32 (O2)
Goethite Analysis by Py-GC-MS at 1400oC
Chromatogram Plots
File: c:\brukerws\data\goeth 1400.xms
Sample: Goeth 1400
Scan Range: 1 - 3404 Time Range: 1.20 - 30.00 min.
Operator: RDevivar
Date: 1/27/2014 4:49 PM
TIC;
Goeth 1400.xms;
Filtered
2.5
GCps
Total Ion Count
Oxygen
2.0
1.5
Water
1.0
0.5
0.0
18.0 (TIC);
Goeth 1400.xms;
Filtered
m/z = 18 amu
30
25
MCps
20
15
10
5
0
2.5
5.0
7.5
10.0
12.5
minutes
A sample of Goethite was first pyrolyzed at 750oC to remove all but the pertinent high
temperature species. The same sample was then pyrolyzed at 1400oC to reveal two key
molecules, Oxygen and Water. Since ample quantities of Goethite have been detected on
the surface of Mars by Spirit, the NASA rover, we essentially have a source of water and
oxygen waiting on Mars; we just have to heat the Goethite under the proper conditions to
release these vital substances.
Applying Thermal Energy
to Extract Chemical Information
Using Thermal Energy:
Chemical Information
•How much Thermal Energy do we
add
•Trapped solvent
•Organic additives
•How fast do we add the Thermal
Energy
•Contaminants
•How long do we maintain the
Thermal Energy
•Labile Functional Groups
•Monomer identification
•What atmosphere do we use
•Off-gassing information
•How much sample do we use
•Inorganic additives
TGA
DSC
Pyrolysis-GC-MS
TGA-MS-IR
Questions?
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