About OMICS Group

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.

http://www.omicsonline.org/open-access-publication.php

http://www.omicsonline.org/scholarly-journals.php

http://www.omicsonline.org/international-scientific-conferences/

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 LaboratoryHouston, 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, TGA-MS, TGA-IR

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

Controlling Heat Exposure

Sample at 25oC Sample at 1000oC

Slow: minutes to hours

Fast: microseconds to seconds

TGAFurnace

PyrolysisFilament

Thermal Analysis

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

Faster RampSlower Ramp

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.

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

Chromatogram Plots

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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

Thermal Analysis of Composite

Thermal AnalysisThermal Desorption

Pyrolysis

Tg

Curing Temperature

Onset of Decomposition

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 >



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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.

Thermal Analysis of Ultem 1000

218.60°C(I)

436.86°C99.37%

40

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Temperature (°C)

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

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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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

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

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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.

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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New Sample

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).

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

Thermal Analysis of Silicone Materials

350.65°C96.30%

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Temperature (°C)

RTV 560––––––– Silicone O-ring– – – – Tacky RTV––––– · PDMS––– – –


The Silicone samples that were nearly identical by FT-IR displayed very different properties by thermal analysis.

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Temperature (°C)

PDMS––––––– Red Tacky RTV– – – – RTV 560––––– · Silicone O-ring––– – –

Exo Up Universal V4.3A TA Instruments

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–––––––


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

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TIC; Silicone oil 0_5CPS.xms; Filtered

TIC; Silicone oil 1Cps.xms; Filtered

TIC; Silicone oil 2CPS001.xms; Filtered

TIC; Silicone oil 5Cps.xms; Filtered

TIC; Silicone oil 10C pe.xms; Filtered

TIC; Siliconeoil 750Cpy.xms; Filtered

Heating Rate: 30oC 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

Chromatogram Plots

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TIC; FEP 3mindly 750.xms; Filtered

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


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


PTFEFEP Teflon

Overlaid Chromatogram Plots

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FEP Teflon Heated at Different Rates

Chromatogram Plots

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TIC; FEP 2CPM.xms; Filtered

TIC; FEP 0_2CPM.xms; Filtered

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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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


TGA

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 >

5.7

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DSC of HDPE vs LDPE

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LDPE––––––– HDPE– – – –


TGA

Pyrolysis-GC-MS

Polyethylene: -CH2-CH2-CH2-CH2-CH2-CH2-CH2-CH2-CH2-

C15C14C13C12C11C10

C9C8C7C6

Chromatogram Plots

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TIC; PE 1CPM.xms; Filtered






TIC; PE test 052913.xms; Filtered

Temperature Ramp Pyrolysis

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LDPE––––––– HDPE– – – –


TGAHeating Rate: 5oC per min

Heating PE in Pyrolysis chamber from 25oC to 750oC at different rates








Heating Rate: >1000oC per sec

Correlating TGA and Pyrolysis Techniques

Chromatogram Plots

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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

Thermal Analysis of PE

450.15°C84.25%

460.14°C66.63%

470.13°C34.72%

480.11°C4.767%

440.16°C92.37%

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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


Chromatogram Plots

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Pyrolysis at 450oC For Specified Duration

20 seconds

40 seconds

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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

TGA Analysis of Fluorinated Materials

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––––––– Krytox 143AZ oil in N2 to 1000C.001– – – – Krytox 143AZ oil in air to 1000C.001


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––––––– Brayco 815Z oil in N2 to 1000C.001– – – – Brayco 815Z oil in air to 1000C.001


Brayco 815ZKrytox 143 AZ

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––––––– Krytox 143AZ oil in N2 to 1000C.001– – – – Brayco 815Z oil in N2 to 1000C.001


Krytox 143 AZBrayco 815Z

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%

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Travertine N2––––––– Travertine air– – – –


CaCO3 CaC2 or Calcium Kaolinite

Travertine

Travertine TGA ashes (Helium or Nitrogen)

Travertine TGA ashes (Air)

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

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Travertine N2––––––– Travertine air– – – –


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

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)

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

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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

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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