about omics group
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About OMICS Group. - PowerPoint PPT PresentationTRANSCRIPT
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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.
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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.
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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 LaboratoryHouston, Texas
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Controlling Heat in Aerospace
Picture of Space Shuttle During Atmospheric Re-entry taken from ISS
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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, TGA-MS, TGA-IR
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Optical Vs. Thermal Techniques
Material CuringThermal Transition-TgMelting Point/ Boiling PointResidual SolventIdentification of additivesMaterial DecompositionElimination of labile functional groupsIdentification of Material ComponentsIdentification of Inorganic Components
LightReflectance EmittanceAbsorbance/TransmissionFluorescenceUV-Vis AbsorbanceFT-IR AnalysisRaman Analysis
Heat
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Controlling Heat Exposure
Sample at 25oC Sample at 1000oC
Slow: minutes to hours
Fast: microseconds to seconds
TGAFurnace
PyrolysisFilament
Thermal Analysis
Thermochemical Analysis
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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
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The Influence of Temperature Ramp Rates
Faster RampSlower Ramp
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Pyrolysis for GC-MS of Solids
• Sample size is relatively small:
50 to 200 mg is sufficient for solids50 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.
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Pyrolyzers: Filament Versus Furnace
CDS Platinum Filament• Heating Rate: ~20,000oC per sec• Max Temperature: 1400oC • Cooling Rate: > 1000oC per sec
• Fast Heating, Fast Cooling
Microfurnace • Heating Rate: ~50oC per min• Max Temperature: 800oC• Cooling Rate: 25oC per min
• Slow to Heat, Slow to Cool
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Chromatogram Plots
5.0 7.5 10.0 12.5 15.0minutes
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TIC; PE std 750 3min.xms; Filtered
TIC; PTFE 750 3min.xms; Filtered
TIC; PVC test SP2 750.xms; Filtered
TIC; PDMS std.XMS; Filtered
Flash Pyrolysis of Polymers
Side Group Elimination
Random Scission
Unzipping
PVC: -CH2-CH-CH2-CH-CH2-CH-CH2-CH-CH2-CH-
Mechanism of Pyrolytic Degradation
PTFE : -CF2-CF2-CF2-CF2-CF2-CF2-CF2-CF2-CF2-
Polyethylene: -CH2-CH2-CH2-CH2-CH2-CH2-CH2-CH2-CH2-
Silicone ScissionSilicones : -O-Si(CH3)2-O-Si(CH3)2-O-Si(CH3)2-O-Si(CH3)2-
Cl Cl Cl Cl Cl
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Thermal Analysis of Composite
Thermal AnalysisThermal Desorption
Pyrolysis
Tg
Curing Temperature
Onset of Decomposition
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Flash Pyrolysis-GC-MS of Ultem 1000
Chromatogram Plots
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RIC Merged ultem_1_750.xms 1200 CENTROID RAW (+) EI Q1MS 10.0 - 800.0 >
RIC Merged ultem_2_750.xms 1200 CENTROID RAW (+) EI Q1MS 10.0 - 800.0 >
RIC Merged ultem_3_750.xms 1200 CENTROID RAW (+) EI Q1MS 10.0 - 800.0 >
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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.
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Thermal Analysis of Ultem 1000
218.60°C(I)
436.86°C99.37%
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Ultem 1000 DSCUltem 1000 TGA
Exo Up Universal V4.3A TA Instruments
Key thermal values can be measured or obtained from product specification information.
Ultem 1000 Tg: 218oC
Onset of Decomposition: 437oC
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Thermal Extraction of Ultem 1000
MS Data Review Active Chromatogram and Spectrum Plots - 7/18/2014 2:51 PMFile: c:\brukerws\data\082013\ult 300.xmsSample: ult 300 Operator: RDevivarScan Range: 1 - 1327 Time Range: 1.20 - 12.43 min. Date: 7/18/2014 2:36 PM
4 5 6 7 8 9 10 11minutes
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TIC; ult 300.xms; Filtered1A
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74.1 9.101e+6
75.1 1.771e+7
111.0 3.216e+7
145.9 7.904e+7
147.9 5.092e+7
149.9 8.196e+6
6.558 min, Scan: 634, MergedSpectrum 1A
Thermal extraction temperature: 400oC
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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.
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TGA Comparison of Gaskets
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16435 New.002––––––– 16435 old.002– – – –
Universal V4.7A TA Instruments
Area of difference
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.
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Thermal Extraction of SamplesChromatogram Plots
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16435 New 400C.xms 10.0:800.0>10.0:800.0>
16435 Old 400C.xms 10.0:800.0>10.0:800.0>
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In Service Sample1,4-Dioxane
Carbon Dioxide
Carbon Dioxide
Glycerin
HOO
OHHO
OO
OOH
HOO
OOH
BHT
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).
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FT-IR Analysis of Silicone Materials
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.
1. Silicone O-ring2. RTV 5603. Red, Tacky RTV4. PDMS
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Thermal Analysis of Silicone Materials
350.65°C96.30%
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RTV 560––––––– Silicone O-ring– – – – Tacky RTV––––– · PDMS––– – –
Universal V4.7A TA Instruments
The Silicone samples that were nearly identical by FT-IR displayed very different properties by thermal analysis.
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PDMS––––––– Red Tacky RTV– – – – RTV 560––––– · Silicone O-ring––– – –
Exo Up Universal V4.3A TA Instruments
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TGA Analysis of Silicone Oil
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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–––––––
Universal V4.7A TA Instruments
The thermal profile of silicone oil at different ramp rates indicates the complexity of thermal analysis
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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.
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Pyrolytic Analysis of Silicone Oil at Different Heating Rates
Chromatogram Plots
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TIC; Silicone oil 5Cps.xms; Filtered
TIC; Silicone oil 10C pe.xms; Filtered
TIC; Siliconeoil 750Cpy.xms; Filtered
Heating Rate: 30oC per min
Heating Rate: 60oC per min
Heating Rate: 120oC per min
Heating Rate: 300oC per min
Heating Rate: 600oC per min
Flash Pyrolysis
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
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Chromatogram Plots
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TIC; PTFE 3mindly 750.xms; Filtered
FEP Vs. PTFE Teflon
497.48°C89.29%
562.04°C57.61%
521.69°C81.55%
995.85°C42.90%
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Sample: FEP Teflon N2Size: 7.2350 mgMethod: Ramp
DSC-TGAFile: D:...\rdevivar\Desktop\FEP Teflon.001Operator: RDevivarRun Date: 28-Jun-2013 16:05Instrument: SDT Q600 V20.9 Build 20
Universal V4.7A TA Instruments
563.05°C46.16%
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Sample: PTFE Teflon N2Size: 5.8520 mgMethod: Ramp
DSC-TGAFile: D:...\rdevivar\Desktop\PTFE Teflon.001Operator: RDevivarRun Date: 01-Jul-2013 07:42Instrument: SDT Q600 V20.9 Build 20
Universal V4.7A TA Instruments
PTFEFEP Teflon
Overlaid Chromatogram Plots
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FEP Teflon Heated at Different Rates
Chromatogram Plots
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Heating Rate: 12oC per minGC Method run time: 100 min
Heating Rate: 120oC per minGC Method run time: 60 min
Heating Rate: >1000oC per secGC Method run time: 30 min
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.
497.48°C89.29%
562.04°C57.61%
521.69°C81.55%
995.85°C42.90%
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DSC-TGAFile: D:...\rdevivar\Desktop\FEP Teflon.001Operator: RDevivarRun Date: 28-Jun-2013 16:05Instrument: SDT Q600 V20.9 Build 20
Universal V4.7A TA Instruments
TGA
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Thermal Analysis of HDPE and LDPE
Chromatogram Plots
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RIC 1 MAR 14612 lot 2.xms 1200 CENTROID RAW (+) EI Q1MS 10.0 - 800.0 >
RIC 1 MAR 14612 lot 1.xms 1200 CENTROID RAW (+) EI Q1MS 10.0 - 800.0 >
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LDPE––––––– HDPE– – – –
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TGA
Pyrolysis-GC-MS
Polyethylene: -CH2-CH2-CH2-CH2-CH2-CH2-CH2-CH2-CH2-
C15C14C13C12C11C10
C9C8C7C6
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Chromatogram Plots
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TIC; PE 25CPM.xms; Filtered
TIC; PE test 052913.xms; Filtered
Temperature Ramp Pyrolysis
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TGAHeating Rate: 5oC per min
Heating PE in Pyrolysis chamber from 25oC to 750oC at different rates
Heating Rate: 30oC per min
Heating Rate: 60oC per min
Heating Rate: 120oC per min
Heating Rate: 180oC per min
Heating Rate: 300oC per min
Heating Rate: 600oC per min
Heating Rate: 1200oC per min
Heating Rate: >1000oC per sec
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Correlating TGA and Pyrolysis Techniques
Chromatogram Plots
5.0 7.5 10.0 12.5 15.0 17.5minutes
0.0
1.0
2.0
GCps
0.0
1.0
2.0
GCps
0.0
1.0
2.0
GCps
0.0
1.0
2.0
GCps
0.0
1.0
2.0
GCps
0.0
1.0
2.0
GCps
0.00.51.01.52.02.5
GCps
0.00.51.01.52.0
GCps
0
1
2
3
GCps
TIC; PE 440 3min.xms; Filtered
TIC; PE 450 3min.xms; Filtered
TIC; PE 460 3min.xms; Filtered
TIC; PE 470 3min.xms; Filtered
TIC; PE 480 3min.xms; Filtered
TIC; PE 490 3min.xms; Filtered
TIC; PE 500 3min.xms; Filtered
TIC; PE 510 3min.xms; Filtered
TIC; PE SP2 750 3 min.xms; Filtered
Py 750oC
Py 440oC
Py 450oC
Py 460oC
Py 470oC
Py 480oC
Py 490oC
Py 500oC
Py 510oC
Pyrolysis at specified temperatures for 20 seconds
Irganox 1076
Irganox 1010
440oC450oC
460oC
470oC
480oC490oC
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Thermal Analysis of PE
450.15°C84.25%
460.14°C66.63%
470.13°C34.72%
480.11°C4.767%
440.16°C92.37%
-1
0
1
2
3
4
Der
iv. W
eigh
t (%
/°C
)
-50
0
50
100
150
Wei
ght (
%)
300 350 400 450 500 550 600 650
Temperature (°C)
Sample: PE 5C per minSize: 2.8770 mg DSC-TGA
File: D:...\Desktop\PE 5 Cpermin Nitrogen.001Operator: RDevivarRun Date: 24-Oct-2013 15:41Instrument: SDT Q600 V20.9 Build 20
Universal V4.7A TA Instruments
Chromatogram Plots
5.0 7.5 10.0 12.5 15.0 17.5minutes
0.0
0.5
1.0
1.5
2.0
2.5
3.0
GCps
0
1
2
3
4
GCps
0.0
0.5
1.0
1.5
2.0
2.5
GCps
0.0
0.5
1.0
1.5
2.0
2.5
GCps
TIC; PE 450 3min.xms; Filtered
TIC; PE 450 40sec.xms; Filtered
TIC; PE 450 60sec.xms; Filtered
TIC; PE 450 80sec.xms; Filtered
Pyrolysis at 450oC For Specified Duration
20 seconds
40 seconds
60 seconds
80 seconds
Irganox 1010Irganox 1076
Modification of the thermal parameters at the onset of TGA degradation for PE can provide valuable information about the additives or contaminants.
Silicone
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TGA Analysis of Fluorinated Materials
-20
0
20
40
60
80
100
120
Wei
ght (
%)
0 100 200 300 400 500 600
Temperature (°C)
––––––– Krytox 143AZ oil in N2 to 1000C.001– – – – Krytox 143AZ oil in air to 1000C.001
Universal V3.9A TA Instruments
-20
0
20
40
60
80
100
120
Wei
ght (
%)
0 100 200 300 400 500 600 700
Temperature (°C)
––––––– Brayco 815Z oil in N2 to 1000C.001– – – – Brayco 815Z oil in air to 1000C.001
Universal V3.9A TA Instruments
Brayco 815ZKrytox 143 AZ
0
20
40
60
80
100
Wei
ght (
%)
0 200 400 600 800 1000
Temperature (°C)
––––––– Krytox 143AZ oil in N2 to 1000C.001– – – – Brayco 815Z oil in N2 to 1000C.001
Universal V3.9A TA Instruments
Krytox 143 AZBrayco 815Z
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Thermal Response of Travertine in Different Atmospheres
599.46°C97.25%
800.75°C55.58%
732.56°C65.50%
745.03°C66.43%
599.46°C97.97%
800.75°C56.79%
60
70
80
90
100
Wei
ght (
%)
0 200 400 600 800 1000 1200
Temperature (°C)
Travertine N2––––––– Travertine air– – – –
Universal V4.5A TA Instruments
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CaCO3 CaC2 or Calcium Kaolinite
Travertine
Travertine TGA ashes (Helium or Nitrogen)
Travertine TGA ashes (Air)
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599.46°C97.25%
800.75°C55.58%
732.56°C65.50%
745.03°C66.43%
599.46°C97.97%
800.75°C56.79%
60
70
80
90
100
Wei
ght (
%)
0 200 400 600 800 1000 1200
Temperature (°C)
Travertine N2––––––– Travertine air– – – –
Universal V4.5A TA Instruments
Calcium Carbonate
Calcium Carbide
Calcium Kaolinite
The Role of Gaseous Atmosphere During Thermal Decomposition of Travertine
TGA of Travertine in Air
TGA of Travertine in Nitrogen
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TGA Analysis of Geothite in Helium
At 120oC, Mass losses include: m/z 14 (CH2), 16 (O), 32 (O2)
At 308oC, Mass losses include: m/z 18 (H2O), 32 (O2)
At 1290oC, Mass losses include: m/z 16 (O), 18 (H2O), 32 (O2)
Goethitea-FeO(OH)
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Goethite Analysis by Py-GC-MS at 1400oC
Chromatogram PlotsFile: c:\brukerws\data\goeth 1400.xmsSample: Goeth 1400 Operator: RDevivarScan Range: 1 - 3404 Time Range: 1.20 - 30.00 min. Date: 1/27/2014 4:49 PM
2.5 5.0 7.5 10.0 12.5minutes
0.0
0.5
1.0
1.5
2.0
2.5
GCps
0
5
10
15
20
25
30
MCp
s
TIC; Goeth 1400.xms; Filtered
18.0 (TIC); Goeth 1400.xms; Filtered
Total Ion Count
m/z = 18 amu
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.
Oxygen
Water
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Applying Thermal Energy to Extract Chemical Information
Using Thermal Energy:
• How much Thermal Energy do we add
• How fast do we add the Thermal Energy
• How long do we maintain the Thermal Energy
• What atmosphere do we use
• How much sample do we use
Chemical Information
• Trapped solvent
• Organic additives
• Contaminants
• Labile Functional Groups
• Monomer identification
• Off-gassing information
• Inorganic additives
TGA DSC Pyrolysis-GC-MS TGA-MS-IR
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Questions?
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