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At least 19 records

Fourier transform infrared (FTIR) fiber optic monitoring of composites during cure in an autoclave

Real-time in situ monitoring of the chemical states of epoxy resins was investigated during cure in an autoclave using infrared evanescent spectroscopy. Fiber evanescent sensors were developed which may be sandwiched between the plies of the prepreg sample. A short length of sapphire fiber was used as the sensor cell portion of the fiber probe. Heavy metal fluoride glass optical fiber cables were designed for connecting the FTIR spectrometer to the sensor fiber within the autoclave. The sapphire fibers have outstanding mechanical thermal properties which should permit their use as an embedded link in all thermoset composites. The system is capable of operation at a temperature of 250 C for periods up to 8 hours without major changes to the fiber transmission. A discussion of the selection of suitable sensor fibers, the construction of a fiber-optic interface, and the interpretation of in situ infrared spectra of the curing process is presented.

Druy, Mark A.↗

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.↗

Surface inspection using FTIR spectroscopy

The use of reflectance Fourier transform infrared (FTIR) spectroscopy as a tool for surface inspection is described. Laboratory instruments and portable instruments can support remote sensing probes that can map chemical contaminants on surfaces with detection limits under the best of conditions in the sub-nanometer range, i.e.. near absolute cleanliness, excellent performance in the sub-micrometer range, and useful performance for films tens of microns thick. Examples of discovering and quantifying contamination such as mineral oils and greases, vegetable oils, and silicone oils on aluminum foil, galvanized sheet steel, smooth aluminum tubing, and sandblasted 7075 aluminum alloy and D6AC steel. The ability to map in time and space the distribution of oil stains on metals is demonstrated. Techniques associated with quantitatively applying oils to metals, subsequently verifying the application, and non-linear relationships between reflectance and the quantity oil are described.

Powell, G. L.↗

FTIR Spectroscopic Characterization Of II-VI Semiconductors

Combination of commercial Fourier-transform infrared (FTIR) spectrometer with computer and special-purpose software constitutes highly automated facility for acquisition and processing of infrared transmission or reflection spectral image data. Intended principally to acquire transmission spectra of some compounds of elements in groups II and VI of periodic table. System used to characterize specimens of II/VI alloy semiconductors grown by directional solidification and quenching. Transmission-edge maps helpful in studies of flows, gradients of temperature, and coefficients of diffusion in solidifying melts. Data acquired by system include optical characteristics, and they both verify and complement data obtained by such other techniques as measurements of density and x-ray-dispersion analysis.

Perry, G. L. E.↗

FTIR Spectroscopy of HNO3 and NO2 Relevant to Stratospheric Wake Analysis

The Fourier Transform Infrared (FTIR) technique has been employed to measure absolute concentrations of nitric acid (HNO3) and nitrogen dioxide (NO2) with 1/cm resolution and an absorption pathlength of 4 m under quasi-static and flow conditions at atmospheric pressure and room temperature. Water features seen under quasi-static conditions diminished in intensity under flowing conditions. Nitric acid was observed in the 1660-1760/cm range, while nitrogen dioxide was detected both in the 1536-1660 and 1213-1400/cm ranges. Concentrations of nitrogen dioxide and nitric acid were determined to be 11.9 and 4.35 parts per million (ppm), respectively, with an uncertainty of 0.2 ppm. Experiments are underway with a 10 m cell to measure the absorption of nitric acid, water, sulfur dioxide, hydrochloric acid and ammonia on various materials such as glass, teflon, stainless steel and aluminum used for implementation of the flow system. Such materials will be used for the measurements of stratospheric trace gases by the Quartz Crystal Microbalance (QCM) and Surface Acoustic Wave (SAW) devices.

Abina, Rafiu A.↗

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.↗

[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.↗

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.↗

Spaceborne Hybrid-FPGA System for Processing FTIR Data

Progress has been made in a continuing effort to develop a spaceborne computer system for processing readout data from a Fourier-transform infrared (FTIR) spectrometer to reduce the volume of data transmitted to Earth. The approach followed in this effort, oriented toward reducing design time and reducing the size and weight of the spectrometer electronics, has been to exploit the versatility of recently developed hybrid field-programmable gate arrays (FPGAs) to run diverse software on embedded processors while also taking advantage of the reconfigurable hardware resources of the FPGAs.

Bekker, Dmitriy↗

Absolute band intensities in the nu19/nu23 (530 cm(-1)) and nu7 (777 cm(-1)) bands of acetone ((CH3)2CO) from 232 to 295 K

Absolute band intensities of acetone ((CH3)2CO) in the nu19/nu23 and nu7 band systems near 530 and 777 cm(-1), respectively, were measured at temperatures of 232, 262 and 295 K, using a Fourier transform infrared (FTIR) spectrometer. No evident temperature dependence for the band intensities was observed. The dipole moments and the fundamental band intensities were derived in the harmonic oscillator approximation. The results are useful for the spectroscopic retrieval of acetone concentrations in the upper atmosphere.

Acetone/chemistry↗

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↗

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.↗

FTIR-spectrometer-determined absorption coefficients of seven hydrazine fuel gases - Implications for laser remote sensing

The absorption spectra of three hydrazines and four of their air-oxidation products were measured in the 9-12-micron spectral region with a Fourier transform infrared (FTIR) spectrometer with a 0.05-kayser resolution to determine absorption coefficients at CO2 and tunable diode laser wavelengths. The measurements agreed well with published CO2 laser determinations for many of the absorption coefficients, except where the published values are thought to be in error. The coefficients were then used to estimate the sensitivity for remote detection of these gases using CO2 and tunable diode lasers in long-path differential absorption measurements.

Molina, L. T.↗

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.↗

FTIR studies of low temperature sulfuric acid aerosols

Sub-micrometer sized sulfuric acid H2SO4 particles were generated using a constant output atomizer source. The particles were then exposed to water vapor before being injected into a low temperature cell. Multipass transmission Fourier Transformation Infrared (FTIR) spectroscopy was used to determine the phase and composition of the aerosols as a function of time for periods of up to five hours. Binary H2SO4H2O aerosols with compositions from 35 to 95 wt % H2SO4 remained liquid for over 3 hours at room temperatures ranging from 189-240 K. These results suggest that it is very difficut to freeze SSAs via homogeneous nucleation. Attempts to form aerosols more dilute than 35 wt % H2SO4 resulted in ice formation.

Anthony, S. E.↗

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.↗

Water Content of the Oceanic Lithosphere at Hawaii from FTIR Analysis of Peridotite Xenoliths

Although water in the mantle is mostly present as trace H dissolved in minerals, it has a large influence on its melting and rheological properties. The water content of the mantle lithosphere beneath continents is better constrained by abundant mantle xenolith data than beneath oceans where it is mainly inferred from MORB glass analysis. Using Fourier transform infrared (FTIR) spectrometry, we determined the water content of olivine (Ol), clinopyroxene (Cpx) and orthopyroxene (Opx) in spinel peridotite xenoliths from Salt Lake Crater, Oahu, Hawaii, which are thought to represent fragments of the Pacific oceanic lithosphere that was refertilized by alkalic Hawaiian melts. Only Ol exhibits H diffusion profiles, evidence of limited H loss during xenolith transport to the surface. Water concentrations (Ol: 9-28 ppm H2O, Cpx: 246-566 ppm H2O, Opx: 116-224 ppm H2O) are within the range of those from continental settings but higher than those from Gakkel ridge abyssal peridotites. The Opx H2O contents are similar to those of abyssal peridotites from Atlantic ridge Leg 153 (170-230 ppm) but higher than those from Leg 209 (10- 14 ppm). The calculated bulk peridotite water contents (94 to 144 ppm H2O) are in agreement with MORB mantle source water estimates and lower than estimates for the source of Hawaiian rejuvenated volcanism (approx 540 ppm H2O) . The water content of Cpx and most Opx correlates negatively with spinel Cr#, and positively with pyroxene Al and HREE contents. This is qualitatively consistent with the partitioning of H into the melt during partial melting, but the water contents are too high for the degree of melting these peridotites experienced. Melts in equilibrium with xenolith minerals have H2O/Ce ratios similar to those of OIB

Peslier, Anne H.↗