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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
NASA NTRS1995

FTIR instrumentation to monitor vapors from Shuttle tile waterproofing materials

The Space Shuttle Thermal Protection System (TPS) tiles and blankets are waterproofed using DimethylEthoxySilane (DMEX) in the Orbiter Processing Facilities (OPF). DMES has a Threshold Limit Value (TLV) for exposure of personnel to vapor concentration in air of 0.5 ppm. The OPF high bay cannot be opened for normal work after a waterproofing operation until the DMES concentration is verified by measurement to be below the TLV. On several occasions the high bay has been kept closed for up to 8 hours following waterproofing operations due to high DMES measurements. In addition, the Miran 203 and Miran 1 BX infrared analyzers calibrated at different wavelengths gave different readings under the same conditions. There was reason to believe that some of the high DMES concentration readings were caused by interference form water and ethanol vapors. The Toxic Vapor Detection Laboratory (TVDL) was asked to test the existing DMES instruments and identify the best qualified instrument. In addition the TVDL was requested to develop instrumentation to ensure the OPF high bay could be opened safely as soon as possible after a waterproofing operation. A Fourier Transform Infrared (FTIR) spectrophotometer instrument developed for an earlier project was reprogrammed to measure DMES vapor along with ethanol, water, and several common solvent vapors. The FTIR was then used to perform a series of laboratory and field tests to evaluate the performance of the single wavelength IR instruments in use. The results demonstrated that the single wavelength IR instruments did respond to ethanol and water vapors, more or less depending on the analytical IR wavelength selected. The FTIR was able to separate the responses to DMES, water and ethanol, and give consistent readings for the DMES vapor concentration. The FTIR was then deployed to the OPF to monitor real waterproofing operations. The FTIR was also used to measure the time for DMES to evaporate from TPS tile under a range of humidity conditions in controlled laboratory tests. The combination of laboratory and field tests with the FTIR instrument demonstrated superior sensitivity, ability to reject interference from water and ethanol vapors, ruggedness to be transported from the lab to the OPF and set up without special procedures or degradation of performance. The multiple component vapor analysis algorithm was developed at KSC and incorporates automatic baseline correction and shape fitting of the spectra. The analysis for DMES, TetraMethylDiSiloxane (TMDS), ethanol, methanol, isopropanol, and baseline parameters uses 161 points per sample at 4 cm(exp -1) resolution, and processes an eight scan sample every ten seconds. The standard deviation of the measurements is 0.013 ppm and the upper linear limit is 125 ppm DMES. Based on successful demonstration of capabilities we produced three mobile instrument carts to be used in each OPF to support future waterproofing operations. The design and building of the 'DMES Carts' were accomplished in Fiscal year 1995.

Mattson, C. B.↗
NASA NTRS2008

Checking Contamination during Storage of Carbonaceous Chondrites for Micro FTIR Measurements

We examined organic contamination by Fourier transform infrared micro spectroscopic (micro FTIR) measurements of carbonaceous chondrite samples. Carbonaceous chondrites, Tagish Lake (C2), Murchison (CM2) and Moss (CO3), and some mineral powder samples pressed on aluminum plates were measured by micro FTIR before and after storage in several containers with silicone rubber mat. During storage, samples did not touch directly anything except the holding aluminum plates. The carbonaceous chondrites containing hydrous minerals (Tagish Lake and Murchison) pressed on aluminum plates and measured by transmission-reflection micro FTIR measurements were found to be contaminated during storage after only one day, as revealed by an increase of approximately 2965 /cm and approximately 1260 /cm peaks. The Moss meteorite which contains no hydrous minerals, did not show an increase of these peaks, indicating no organic contamination. This difference is probably related to the differing mineralogy and physical properties (including porosity and permeability) of these chondrites. Hydrous minerals such as antigorite, muscovite, montmorillonite and silica gel showed organic contamination by the same infrared measurements, while anhydrous materials such as SiO2 and KBr showed no contamination. These results indicate importance of surface OH groups for the organic contamination. Organic contamination was found on silica gel samples pressed on aluminum plates when they were stored within containers including silicone rubber, silicone grease or adhesive tape. Long path gas cell FTIR measurements for silicone rubber indicated methylsiloxane oligomers were released from the silicone rubber. In-situ heating infrared measurements on the contaminated antigorite and Tagish Lake showed decrease of the 1262 /cm (Si-CH3) and 2963 /cm (CH3) peaks from room temperature to 200-300 C indicating desorption of volatile contaminants. These results indicate that careful preparation and storage are essential for FTIR measurements on precious astromaterial samples such as meteorites, IDPs and samples returned from comets, asteroids and Mars. Every possible contamination source should be evaluated before anything is done to these samples.

Zolensky, Michael E.↗
NASA NTRS1990

Characterization of the surfaces of platinum/tin oxide based catalysts by Fourier Transform Infrared Spectroscopy (FTIR)

A Pt/SnO2 catalyst has been developed at NASA Langley that is effective for the oxidation of CO at room temperature (1). A mechanism has been proposed to explain the effectiveness of this catalyst (2), but most of the species involved in this mechanism have not been observed under actual catalytic conditions. A number of these species are potentially detectable by Fourier Transform Infrared Spectroscopy (FTIR), e.g., HOSnO sub x, HO sub y PtO sub z, Pt-CO, and SnHCO3. Therefore a preliminary investigation was conducted to determine what might be learned about this particular catalyst by transmission FTIR. The main advantage of FTIR for this work is that the catalyst can be examined under conditions similar to the actual catalytic conditions. This can be of critical importance since some surface species may exist only when the reaction gases are present. Another advantage of the infrared approach is that since vibrations are probed, subtle chemical details may be obtained. The main disadvantage of this approach is that FTIR is not nearly as sensitive as the Ultra High Vacuum (UHV) surface analytical techniques such as Auger, Electron Spectroscopy for Chemical Analysis (ESCA), Electron Energy Loss Spectroscopy (EELS), etc. Another problem is that the assignment of the observed infrared bands may be difficult.

Keiser, Joseph T.↗
NASA NTRS1999

FTIR Study of Vapor Offgassing from Orbiter Tile Re-Waterproofing Materials

The work presented in this paper was performed to identify and quantify the offgassing behavior of alternative re-waterproofmg materials under investigation for application to Shuttle Orbiter Thermal Protection System (TPS) tile and blanket materials. The purpose was to determine whether the new materials would cause a problem with the operational analysis of residual vapors using the current portable vapor analyzer, a Miran 203. The materials investigated were limited to dimethylethoxysilane (DMES) and proposed solvent selected as suitable for use in re-waterproofing Orbiter TPS. The solvent was selected in another phase of the overall project. Obiter TPS tiles were injected with the re-waterproofing materials under constant conditions of temperature, relative humidity and air flow. The vapor concentrations of offgassing materials were monitored using Fourier Transform Infrared (FTIR) multi-component analysis, and with the Miran 203 instruments. The procedure was to record the time dependent concentrations of offgassing materials as analyzed by the FTIR, and the time response of the Miran 203 to the materials under consideration. The FTIR was calibrated for vapor phase DMES, tetramethyldisiloxane (TMDS), ethanol and the hydrocarbon solvents to be used to dilute the DMES for application to the TPS tile. The Miran 203 was calibrated for the operational measurement of DMES airborne vapors. The FTIR data, shows for the first time that the principal product which offgases from the tile after the first hour is not DMES, but TMDS and ethanol. The Miran 203 response to TMDS is the primary reading after the re-waterproofing operation is completed. The operational use of the Miran 203 to measure DMES vapors after re-waterproofmg operations has been responding to TMDS. The results of this study suggest that the historical complaints that have contributed to the low threshold limit value (TLV) for DMES concentrations, as read with the Miran 203, are actually based on instrumental responses to TMDS, for which no other toxicology information is available at this time. While there is some interference, the use of the tested hydrocarbon solvents does not adversely affect the response of the Miran 203.

Mattson, C. B.↗
NASA NTRS1990

Novel laser gain and time-resolved FTIR studies of photochemistry

Several techniques are discussed which can be used to explore laboratory photochemical processes and kinetics relevant to planetary atmospheres; these include time-resolved laser gain-versus-absorption spectroscopy and time-resolved Fourier transform infrared (FTIR) emission studies. The laser gain-versus-absorption method employed tunable diode and F-center lasers to determine the yields of excited photofragments and their kinetics. The time-resolved FTIR technique synchronizes the sweep of a commercial FTIR with a pulsed source of light to obtain emission spectra of novel transient species in the infrared. These methods are presently being employed to investigate molecular photodissociation, the yields of excited states of fragments, their subsequent reaction kinetics, Doppler velocity distributions, and velocity-changing collisions of translationally fast atoms. Such techniques may be employed in future investigations of planetary atmospheres, for example to study polycyclic aromatic hydrocarbons related to cometary emissions, to analyze acetylene decomposition products and reactions, and to determine spectral features in the near infrared and infrared wavelength regions for planetary molecules and clusters.

Leone, Stephen R.↗
NASA NTRS2008

Rapid Contamination During Storage of Carbonaceous Chondrites Prepared for Micro FTIR Measurements

The carbonaceous chondrites Tagish Lake and Murchison, which contain abundant hydrous minerals, when pressed on aluminum plates and analyzed by micro FTIR, were found to have been contaminated during brief (24 hours) storage. This contamination occurred when the samples were stored within containers which included silicone rubber, silicone grease or adhesive tape. Long-path gas cell FTIR measurements for silicone rubber revealed the presence of contaminant volatile molecules having 2970 cm(sup -1) (CH3) and 1265 cm(sup -1) (Si-CH3) peaks. These organic contaminants are found to be desorbed by in-situ heating infrared measurements from room temperature to 200-300 C. Careful preparation and storage are therefore needed for precious astronomical samples such as meteorites, IDPs and mission returned samples from comets, asteroids and Mars, if useful for FTIR measurements are to be made.

Kebukawa, Yoko↗
NASA NTRS2017

Air Contamination Quantification by FTIR with Gas Cell

Air quality is of utmost importance in environmental studies and has many industrial applications such as aviators grade breathing oxygen (ABO) for pilots and breathing air for fire fighters. Contamination is a major concern for these industries as identified in MIL-PRF-27210, CGA G-4.3, CGA G-7.1, and NFPA 1989. Fourier Transform Infrared Spectroscopy (FTIR) is a powerful tool that when combined with a gas cell has tremendous potential for gas contamination analysis. Current procedures focus mostly on GC-MS for contamination quantification. Introduction of this topic will be done through a comparison of the currently used deterministic methods for gas contamination with those of FTIR gas analysis. Certification of the mentioned standards through the ISOIEC 17065 certifying body A2LA will be addressed followed by an evaluation of quality information such as the determinations of linearity and the limits of detection and quantitation. Major interferences and issues arising from the use of the FTIR for accredited work with ABO and breathing air will be covered.

Freischlag, Jason↗
NASA NTRS2018

Efficacy of FTIR Analysis in Determining CO2 Loading on Diglycolamine

In support of advanced air revitalization technologies to enable human spaceflight beyond low earth orbit, performance studies have been conducted using a liquid amine, Diglycolamine (DGA) between teams at NASA's Johnson Spaceflight Center (JSC) and Ames Research Center (ARC). Liquid amines have been used in regenerable earth-based systems to remove CO2 from industrial systems as well as for closed-environment air revitalization because they can be regenerated at lower temperatures than solid sorbent systems. As an additional advantage to solid sorbent-based systems, liquid sorbents can be cycled between an adsorbing contactor and degassing chamber, thereby reducing system complexity by operation in a continuous loop. In an effort to inform a regeneration system design for micro-gravity applications, ARC has performed a number of tests to characterize the degas mechanics of DGA. In order to accurately measure the amount of CO2 captured or released by the amine, methods such as gravimetric weighing and chemical desorption are reasonable, however the first iteration test setup for a scaled down degas system required analysis on small sample sizes. Fourier-transform infrared spectroscopy (FTIR) analysis was experimentally evaluated to analyze CO2 concentration because it can produce measurements with sample sizes on the order of 100's of μL. Calibration against chemical desorption showed relatively good correlation and test data showed reasonable adherence to expected trends, however more extensive testing should be conducted to fully validate the usage of FTIR to determine CO2 loading on DGA.

Diglycolamine↗
NASA NTRS2024

Solar FTIR Measurements of NOx Vertical Distributions – Part 2: Experiment-Based Scaling Factors Describing the Daytime Variation in Stratospheric NOx

Long-term experimental stratospheric NO2 and NO partial columns measured by means of solar Fourier-transform infrared (FTIR) spectrometry at Zugspitze (47.42° N, 10.98° E; 2964 m a.s.l.), Germany, were used to create a set of experiment-based monthly scaling factors (SFexp). The underlying data set is published in a companion paper (Nürnberg et al., 2024) and comprises over 25 years of measurements depicting the daytime variability of stratospheric NO2 and NO partial columns with respect to local solar time (LST). In accordance with simulation-based scaling factors recently published by Strode et al. (2022), we created SFexp normalized to SZA =72° for NO2 and NO for every month of the year as a function of solar zenith angle (SZA). Apart from a boundary value problem at minimum SZA values originating from averaging over different times of the month, the obtained scaling factors SFexp(NO2) and SFexp(NO) as a function of SZA represent the daytime behavior already shown in model simulations and experiments in the literature very well. This shows a well-pronounced increase in the NO2 and NO stratospheric partial column with the time of the day and a flattening of this increase after noon. In addition to the discussion of SFexp, we validate the simulation-based scaling factors SFsim(NO2) (Strode et al., 2022) and present simulation-based scaling factors for NO SFsim(NO). The simulation-based scaling factors show excellent agreement with the experiment-based ones; i.e., for NO2 and NO the mean value of the modulus between the experiment and simulation over all SZAs and months is only 0.02 %. We show that recently used model simulations can describe the real behavior of nitrogen oxide (NOx) variability in the stratosphere very well. Furthermore, we conclude that ground-based FTIR measurements can be used for validation of the output of photochemistry models and for creating experiment-based data sets describing the daytime stratospheric NOx variability as a function of SZA. This is a contribution to improved satellite validation and a better understanding of stratospheric photochemistry.

FTIR, nitrogen oxides, diurnal variability↗
NASA NTRS1986

FTIR characterization of advanced materials

This paper surveys the application of Fourier transform infrared spectroscopy to the characterization of advanced materials. FTIR sampling techniques including internal and external reflectance and photoacoustic spectroscopy are discussed. Representative examples from the literature of the analysis of resins, fibers, prepregs and composites are reviewed. A discussion of several promising specialized FTIR techniques is also presented.

Young, P. R.↗
NASA NTRS1989

Highly automated optical characterization with FTIR spectrometry

The procedure for evaluating the characteristics of II-VI semiconducting infrared sensor materials with a Fourier Transform Infrared (FTIR) spectrometer system will be discussed. While the method of mapping optical characteristics with a spectrometer has been employed previously, this system is highly automated compared to other systems where the optical transmission data are obtained using a FTIR system with a small stationary aperture in the optical path and moving the specimen behind the aperture. The hardware and software, including an algorithm developed for extracting cut-on wavelengths of spectra, as well as several example results, are described to illustrate the advanced level of the system. Additionally, data from transverse slices and longitudinal wafers of the aforementioned semiconductors will be used to show the accuracy of the system in predicting trends in materials such as shapes of growth interfaces and compositional uniformity.

Perry, G. L. E.↗
NASA NTRS1990

FTIR Monitoring Of Curing Of Composites

Infrared-sensing optical fiber system developed to monitor principal infrared absorption bands resulting from vibrations of atoms and molecules as chemical bonds form when resin cured. System monitors resin chemistry more directly. Used to obtain Fourier transform infrared (FTIR) spectrum from graphite fiber/polyimide matrix resin prepreg. Embedded fiber optic FTIR sensor used to indicate state of cure of thermosetting composite material. Developed primarily to improve quality of advanced composites, many additional potential applications exist because principal of operation applicable to all organic materials and most inorganic gases. Includes monitoring integrities of composite materials in service, remote sensing of hazardous materials, and examination of processes in industrial reactors and furnaces.

Druy, Mark A.↗
NASA NTRS1990

In situ analysis of CO during chemisorption and oxidation on graphite: Supported Pt by FTIR-microspectrometry

For chemisorption and oxidation on Pt/HOPG (highly-orientated pyrolytic) graphite, reflectance Fourier Transform Infrared (FTIR)-microspectrometry reveals a variable state and reactivity for CO. Even for model surface science systems, where surface heterogeneity is minimal, surface diffusion may be too slow relative to the reaction rate to avoid segregation of reactants into surface islands under steady-state conditions. Thus in CO oxidation on Pt (where the relevant surface diffusion coefficients are such that D sub O less than D sub CO) then reactant CO islands exists at the perimeters of which the surface reaction is thought to occur. Furthermore CO can chemisorb on metals in linear and bridge forms to extents which vary with precise faces predominantly exposed coverage, etc. Infrared has long been used to probe the nature of adsorbed CO on model film and heterogeneous surfaces, but it may now be that FTIR-microspectrometry will allow the state of this adsorbate and reactant to be investigated with a spatial resolution of 4.4 microns on model (and real) catalytic surfaces.

Self, Valerie A.↗
NASA NTRS1990

Calorimetry, activity, and micro-FTIR analysis of CO chemisorption, titration, and oxidation on supported Pt

The value of in situ analysis on CO chemisorption, titration and oxidation over supported Pt catalysts using calorimetry, catalytic and micro-FTIR methods is illustrated using silica- and titania-supported samples. Isothermal CO-O and O2-CO titrations have not been widely used on metal surfaces and may be complicated if some oxide supports are reduced by CO titrant. However, they can illuminate the kinetics of CO oxidation on metal/oxide catalysts since during such titrations all O and CO coverages are scanned as a function of time. There are clear advantages in following the rates of the catalyzed CO oxidation via calorimetry and gc-ms simultaneously. At lower temperatures the evidence they provide is complementary. CO oxidation and its catalysis of CO oxidation have been extensively studied with hysteresis and oscillations apparent, and the present results suggest the benefits of a combined approach. Silica support porosity may be important in defining activity-temperature hysteresis. FTIR microspectroscopy reveals the chemical heterogeneity of the catalytic surfaces used; it is interesting that the evidence with regard to the dominant CO surface species and their reactivities with regard to surface oxygen for present oxide-supported Pt are different from those seen on graphite-supported Pt.

Sermon, Paul A.↗
NASA NTRS1997

[Photodissociation of Acetylene and Acetone using Step-Scan Time-Resolved FTIR Emission Spectroscopy]

The photodissociation of acetylene and acetone was investigated as a function of added quenching gas pressures using step-scan time-resolved FTIR emission spectroscopy. Its main components consist of Bruker IFS88, step-scan Fourier Transform Infrared (FTIR) spectrometer coupled to a flow cell equipped with Welsh collection optics. Vibrationally excited C2H radicals were produced from the photodissociation of acetylene in the unfocused experiments. The infrared (IR) emission from these excited C2H radicals was investigated as a function of added argon pressure. Argon quenching rate constants for all C2H emission bands are of the order of 10(exp -13)cc/molecule.sec. Quenching of these radicals by acetylene is efficient, with a rate constant in the range of 10(exp -11) cc/molecule.sec. The relative intensity of the different C2H emission bands did not change with the increasing argon or acetylene pressure. However, the overall IR emission intensity decreased, for example, by more than 50% when the argon partial pressure was raised from 0.2 to 2 Torr at fixed precursor pressure of 160mTorr. These observations provide evidence for the formation of a metastable C2H2 species, which are collisionally quenched by argon or acetylene. Problems encountered in the course of the experimental work are also described.

McLaren, Ian A.↗
NASA NTRS1998

Oxygen Impurities and Defects in Epitaxial Layer SiC and SiC Wafer Characterized by Room and Low Temperatures FTIR

SiC as a highly promising semiconducting material has received increasing attention in the last decade. The impurities such as oxygen and hydrogen have a great effect in electronic properties of semiconducting materials. In this study, the FTIR spectra were measured at room temperature (25 C) and low temperature (-70 C) for an n-type SiC substrate, a p-type epitaxial layer SiC, and patterned Ta on a p-type epitaxial layer SiC sample. The oxygen related IR peaks were measured for all three samples at room and low temperatures. The peak at 1105 cm(exp -1) is the result of a substitutional carbon and a interstitial oxygen in SiC. The concentration of the impurity oxygen increases in the SiC epitaxial layer during the CVD and electron beam processes. For the n-type SiC substrate, this peak does not appear. The peak at 905 cm(exp -1) exists in the IR spectra only for two epitaxial layer on p-type SiC substrate samples. This peak is related to oxygen vacancy centers in SiC, which are introduced in the CVD epitaxial growth process. At low temperature, the peak at 1105 cm(exp -1) shifts down and the peak at 905 cm(exp -1) shifts up for the epitaxial layer SiC samples. It can be explained that, at low temperatures, the stress increases due to the distorted bonds. The study shows that FTIR is a very effective method to evaluate low concentration impurities in SiC.

Lu, W. J.↗
NASA NTRS2000

Deterrent Concentration Measurement with FTIR and Subsequent Ballistic Performance in Medium Caliber Propellant

To meet ballistic requirements, medium and small caliber propellants use deterrent coatings to obtain burn rate progressivity. The required amount and distribution of deterrent varies between gun systems, propellant types, and often between lots. Micro Fourier Transform Infrared (FTIR) spectroscopy was used to measure deterrent gradients in RP36 propellants coated with methyl centralite (MC) at different deterrent levels and different processing conditions. The aromatic C-C bonds at 1496 cm(exp -1) wavenumber were used to monitor the deterrent profiles through the grain. Deterrent gradients measured with FTIR spectroscopy were then used to estimate burn rate gradients in the deterred grains. Burn rates were calculated from literature models and from closed bomb data of RP36 containing uniform deterrent concentration. Finally, the burn rate gradients were input into an IBHFG2 model of a 200 cc-closed bomb. The early flame spreading portion of the closed bomb ballistic cycle (0 to 0.2 P/Pmax) was roughly modeled by dividing the charge up into five propellant decks and igniting them at different times in the ballistic cycle. Pressure traces and vivacity curves from closed bomb shots were compared to predictions. In addition to the burn rate gradient, the closed bomb pressure trace was heavily dependent on ignition and flame spread. These two phenomena were not readily distinguishable from one another in deterred grains. The same RP-36 propellant was shot in a 25 mm M793TP round which was again modeled with IBHVG2. Peak pressure and muzzle velocity were accurately modeled when erosive burning effects were empirically factored into the model.

Furrow, Keith W.↗
NASA NTRS2003

Correlating Flammability of Materials with FTIR Analysis Test Results

The purpose of this experiment was to correlate flammability data with FTIR test results. Kydex 100 is a blend of chlorinated polyvinyl chloride and polymethylmethacrylate, with some filler materials. Samples supplied were 0.125 in. thick. 10 samples were taken from a sheet of Kydex and analyzed for flammability and by FTIR spectroscopy. This material was utilized as a round robin sample for flammability testing. The flammability test results were found to vary across the same sheet.

Moore, Robin↗