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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 NTRS1998

Fourier Transform Infrared (FT-IR) Spectroscopy of Atmospheric Trace Gases HCl, NO and SO2

Fourier Transform Infrared (FT-IR) spectral data have been recorded in the spectral region 400-4000/cm of hydrogen chloride and sulfur dioxide with I/cm resolution and of nitric oxide with 0.25 cm-i resolution, under quasi-static conditions, when the sample gas was passed through tubings of aluminum, copper, stainless steel and teflon. The absorbance was measured for the rotational lines of the fundamental bands of (1)H(35)Cl and (1)H(37)Cl for pressures in the range 100-1000 Torr and for the (14)N(16)O molecule in the range 100-300 Torr. The absorbance was also measured for individual rotational lines corresponding to the three modes of vibrations (upsilon(sub 1) - symmetric stretch, upsilon(sub 2) - symmetric bend, upsilon(sub 3) - anti-symmetric stretch) of the SO2 molecule in the pressure range 25-150 Torr. A graph of absorbance versus pressure was plotted for the observed rotational transitions of the three atmospherically significant molecules, and it was found that the absorbance was linearly proportional to the pressure range chosen, thereby validating Beer's law. The absorption cross-sections were determined from the graphical slopes for each rotational transition recorded for the HCl, NO and SO2 species. Qualitative and quantitative spectral changes in the FT-IR data will be discussed to identify and characterize various tubing materials with respect to their absorption features.

Haridass, C.↗
NASA NTRS1990

FT-IR spectroscopic studies of polycyclic aromatic hydrocarbons

Proper assessment of the hypothesis which correlates polycyclic aromatic hydrocarbons (PAHs) with the unidentified infrared emission bands requires additional experimental laboratory data. In order to address this need, thermal infrared emission studies were performed on a subset of PAHs suggested to be of astrophysical importance. It was proposed that infrared emission from interstellar PAHs occurs following absorption of an ultraviolet photon. Since energy transfer to the ground electronic state can be rapid for a species in which intersystem crossing is negligible, the emission spectrum may be viewed as resulting from an equilibrium vibrational temperature (Leger and d'Hendecourt, 1987). This has been the basis for using infrared absorption spectra to calculate the corresponding emission spectra at various temperatures. These calculations were made using room temperature infrared absorption coefficients instead of those at the temperature of interest because of the latter's unavailability. The present studies are designed to address the differences between the calculated and experimental thermal emission spectra and to provide information which will be useful in future ultraviolet induced infrared fluorescence studies. The emission spectra have been obtained for temperatures up to 825K using an emission cell designed to mount against an external port of an FT-IR spectrometer. These spectra provide information concerning relative band intensities and peak positions which is unavailable from previous calculations.

Salisbury, D. W.↗
NASA NTRS1992

FT-IR microscopic mappings of early mineralization in chick limb bud mesenchymal cell cultures

Chick limb bud mesenchymal cells differentiate into chondrocytes and form a cartilaginous matrix in culture. In this study, the mineral formed in different areas within cultures supplemented with 4 mM inorganic phosphate, or 2.5, 5.0, and 10 mM beta-glycerophosphate (beta GP), was characterized by Fourier-transform infrared (FT-IR) microscopy. The relative mineral-to-matrix ratios, and distribution of crystal sizes at specific locations throughout the matrix were measured from day 14 to day 30. The only mineral phase detected was a poorly crystalline apatite. Cultures receiving 4 mM inorganic phosphate had smaller crystals which were less randomly distributed around the cartilage nodules than those in the beta GP-treated cultures. beta GP-induced mineral consisted of larger, more perfect apatite crystals. In cultures receiving 5 or 10 mM beta GP, the relative mineral-to-matrix ratios (calculated from the integrated intensities of the phosphate and amide I bands, respectively) were higher than in the cultures with 4 mM inorganic phosphate or in the in vivo calcified chick cartilage.

NASA Discipline Musculoskeletal↗
NASA NTRS1985

Fourier transform-infrared spectroscopic methods for microbial ecology: analysis of bacteria, bacteria-polymer mixtures and biofilms

Fourier transform-infrared (FT-IR) spectroscopy has been used to rapidly and nondestructively analyze bacteria, bacteria-polymer mixtures, digester samples and microbial biofilms. Diffuse reflectance FT-IR (DRIFT) analysis of freeze-dried, powdered samples offered a means of obtaining structural information. The bacteria examined were divided into two groups. The first group was characterized by a dominant amide I band and the second group of organisms displayed an additional strong carbonyl stretch at approximately 1740 cm-1. The differences illustrated by the subtraction spectra obtained for microbes of the two groups suggest that FT-IR spectroscopy can be utilized to recognize differences in microbial community structure. Calculation of specific band ratios has enabled the composition of bacteria and extracellular or intracellular storage product polymer mixtures to be determined for bacteria-gum arabic (amide I/carbohydrate C-O approximately 1150 cm-1) and bacteria-poly-beta-hydroxybutyrate (amide I/carbonyl approximately 1740 cm-1). The key band ratios correlate with the compositions of the material and provide useful information for the application of FT-IR spectroscopy to environmental biofilm samples and for distinguishing bacteria grown under differing nutrient conditions. DRIFT spectra have been obtained for biofilms produced by Vibrio natriegens on stainless steel disks. Between 48 and 144 h, an increase in bands at approximately 1440 and 1090 cm-1 was seen in FT-IR spectra of the V. natriegens biofilm. DRIFT spectra of mixed culture effluents of anaerobic digesters show differences induced by shifts in input feedstocks. The use of flow-through attenuated total reflectance has permitted in situ real-time changes in biofilm formation to be monitored and provides a powerful tool for understanding the interactions within adherent microbial consortia.

NASA Discipline Number 61-10↗
NASA NTRS1987

Synthesis and solution imidization studies of soluble poly(imide siloxane) segmented copolymers

Soluble metalinked poly(imide siloxane) segmented copolymers were synthesized utilizing a THF/NMP cosolvent system. The presence of dual solvent makes it possibled to reach high molecular weight in the amid acid stage. Incorporation of siloxanes at about 10 weight percent or higher enables the materials to be fully soluble in a range of polar solvents even after imidization. Imidization may be achieved either by conventional thermal methods on cast amic acid films or in appropriate solvent/azeotroping-agent systems employing moderate temperatures. The imidization procedure has been followed by FT-IR and NMR studies. FT-IR studies show the solution imidization follows first order kinetics and proceeds to about 96 percent completion. NMR studies of the isolated products show residual amic acid may be present after solution imidization, but only at very low levels. Properties of the solution imidized materials compared well with those obtained from samples imidized as thin films.

Summers, J. D.↗
NASA NTRS1995

Standardization of surface contamination analysis systems

Corrosion products, oils and greases can potentially degrade material bonding properties. The Marshall Space Flight Center (MSFC) Surface Contamination Analysis Team (SCAT) utilizes a variety of analytical equipment to detect identify and quantify contamination on metallic and non-metallic substrates. Analysis techniques include FT-IR Microscopy (FT-IR), Near Infrared Optical Fiber Spectrometry (NIR), Optically Stimulated Electron Emission (OSEE), Ultraviolet Fluorescence (UVF) and Ellipsometry. To insure that consistent qualitative and quantitative information are obtained, standards are required to develop analysis techniques, to establish instrument sensitivity to potential contaminants, and to develop calibration curves. This paper describes techniques for preparing and preserving contamination standards. Calibration of surface contamination analysis systems is discussed, and methods are presented for evaluating the effects of potential contaminants on bonding properties.

Boothe, Richard E.↗
NASA NTRS1981

Flammability and Photo-Stability of Selected Polymer Systems

A systematic approach to the improvement of the flammability of epoxy resins, bisphenol-A polycarbonate poly(butylene terephthalate), and Nylon 6.6 by introducing halogens and loop functionality into the flame retardants is described. The phthalides (the loop functionality containing molecules) include 3,3-bis(4-bromophenyl)-phthalide, 3,3-bis(4-chlorophenyl)phthalide, and phenolphthalein. The phthalide containing epoxy resins are synthesized and characterized in comparison with the bisphenol-A epoxy resins in terms of flammability in the copolymer systems. The resins include diglycidyl ethers of phenolphthalein, bisphenol-A. tetrabromobisphenol-A, and tetraoromophenolphthalein. The vaporization of the phthalide additive in the polymers is observed in Thermal Gravimetric Analysis. The flame retardancy is primarily due to the presence of halogens. In the poly(butylene terephthalate) system, the cleavage of the C(sub aromatic) -B bond of the flame retardant additive enhances the crosslinking react ions between the aromatic rings resulting in an increase of char formation. In the epoxy resin systems, loop functionality contributes to char formation to a larger extent. The interaction between the epoxy resin and poly-(butylene terephthalate) follows the mechanism of insertion of the oxirane ring into the ester bond. This mechanism is studied by FT-IR. The investigation of the thermal properties of the char-forming phenol-formaldehyde resins is conducted to provide information for the systematic design of high temperature flame-resistant phenolics. NMR and FT-IR are used to characterize the oligomeric resins and the cured resins. The curing agents used in the study include formaldehyde, s-trioxane and terephthaloyl chloride. The brominated phenolic resins are found to have higher oxygen indices with lower char yields.

Lo, Jeelin↗
NASA NTRS1998

Fluoropolymer Films Deposited by Argon Ion-Beam Sputtering of Polytetrafluoroethylene

The FT-IR, XPS and UV spectra of fluoropolymer films (SPTFE-I) deposited by argon ion-beam sputtering of polytetrafluoroethylene (PTFE) were obtained and compared with prior corresponding spectra of fluoropolymer films (SPTFE-P) deposited by argon rf plasma sputtering of PTFE. Although the F/C ratios for SPTFE-I and -P (1.63 and 1.51) were similar, their structures were quite different in that there was a much higher concentration of CF2 groups in SPTFE-I than in SPTFE-P, ca. 61 and 33% of the total carbon contents, respectively. The FT-IR spectra reflect that difference, that for SPTFE-I showing a distinct doublet at 1210 and 1150 per centimeter while that for SPTFE-P presents a broad, featureless band at ca. 1250 per centimeter. The absorbance of the 1210-per centimeter band in SPTFE-I was proportional to the thickness of the film, in the range of 50-400 nanometers. The SPTFE-I was more transparent in the UV than SPTFE-P at comparable thickness. The mechanism for SPTFE-I formation likely involves "chopping off" of oligomeric segments of PTFE as an accompaniment to "plasma" polymerization of TFE monomer or other fluorocarbon fragments generated in situ from PTFE on impact with energetic Ar ions. Data are presented for SPTFE-I deposits and the associated Ar(+) bombarded PTFE targets where a fresh target was used for each run or a single target was used for a sequence of runs.

Golub, Morton A.↗
NASA NTRS1997

XPS Study of Plasma- and Argon Ion-Sputtered Polytetrafluoroethylene

The similarity of plasma-polymerized tetrafluoroethylene (PPTFE) and the fluoropolymer film deposited by rf (radio frequency) plasma sputtering (SPTFE) of polytetrafluoroethylene (PTFE), noted earlier in the literature, has been reconfirmed. FT-IR (Fourier Transform Infrared), XPS (X ray Photoelectron Spectroscopy) and UV (ultraviolet) spectroscopy has been employed in apparently the first study to involve preparation of PPTFE and SPTFE in the same reactor and under comparable low-power plasma conditions. Most of the work concerned the use of He or Ar as sputtering gas, but some runs were also carried out with the other rare gases Ne, Kr and Xe. The C1s XPS spectra of SPTFE films displayed a relatively higher content of CF2 groups, and yielded higher F/C (fluorine / carbon) ratios, than PPTFE films, while the SPTFE films were somewhat more transparent in the UV than PPTFE. The F/C ratios for SPTFE were essentially independent of the rare gas used for sputtering. Increasing rf power from 10 to 50 W for Xe plasma-sputtering of PTFE resulted in successively lower F/C ratios (1.55 to 1.21), accompanied by sputtering of the glass reactor occurring at 40 W and above. Some limited XPS, FT-IR and UV data are presented on Ar ion-sputtered PTFE.

Golub, Morton A.↗
NASA NTRS1977

High resolution infrared absorptivities for gaseous chlorine nitrate

High resolution infrared absorptivities of chlorine nitrate (ClONO2) are required in order to quantitatively evaluate, by examination of infrared spectra obtained recently from balloon-borne spectrometers, the possible occurrence of this compound in the stratosphere. In the present study, infrared absorptivities for four absorption bands of gaseous ClONO2 have been measured at 0.0625 per cm spectral resolution with a Fourier transform infrared (FT-IR) system. Spectra were obtained at two pressures (0.05 and 1.05 torr) of pure ClONO2 and with 125 torr of N2 added to a 0.50 torr sample. Absorptivities for a range of spectral resolutions (0.0625, 0.125, 0.25 and 0.50 per cm) have been calculated from the data.

Graham, R. A.↗
NASA NTRS1983

Mechanism and kinetics of the curing process in a resin system

The present investigation is concerned with the development of a cure reactivity model for a resin system consisting of tetraglycidyl diaminodiphenyl methane (TGDDM) and diaminodiphenyl sulfone (DDS), taking into account the temperature range from 153 to 177 C. Differential scanning calorimetry and FT-IR spectroscopy have been used to investigate the cure kinetics of the resin with the objective to obtain a correlation between the total conversion and the rates of formation and disappearance of specific functionalities. It was found that the overall process can be satisfactorily described in terms of two first order processes.

Moacanin, J.↗
NASA NTRS1986

Kinetic study of polymerization/curing of filament-wound composite epoxy resin systems with aromatic diamines

The kinetics of polymerization/curing of a filament-wound composite epoxy resin consisting of an 80/20 DGEBA/DGEBD blend and an MDA/m-PDA blend (Tonox 60/40) was studied at various temperatures and at amine epoxy ratios between 1.1 and 4.4 by means of Fourier-transform (FT) IR and bulk viscosity measurements. The activation energy for the polymerization/curing reaction using an amine/epoxy ratio of 1.1 was 11.9 kcal/mole, in agreement with a previous value. The FT-IR conversion-time plots were fitted to a kinetic expression containing two rate constants with activation energies of 13.7 and 10.0 kcal/mole. The bulk viscosity followed the Williams et al. (1955) equation, with a Di Benedetto (1965) expression for the glass transition temperature.

Golub, M. A.↗
NASA NTRS1988

The V3, V4 and V6 bands of formaldehyde: A spectral catalog from 900 cm(-1) to 1580 cm(-1)

The results of a complete high resolution study of the three vibration-rotation bands v sub 3, v sub 4, and V sub 6 using both TDLs and FT-IR spectroscopy are presented. The reults are given in terms of a table of over 8000 predicted transition frequencies and strengths. A plot of the predicted and calculated spectra is shown. Over 3000 transitions were assigned and used in the simultaneous analysis of the three bands. The simultaneous fit permitted a rigorous study of Coriolis and other type iterations among bands yielding improved molecular constants. Line intensities of 28 transitions measured by a TDL and 20 transitions from FTS data were used, along with the eigenvectors from the frequency fitting, in a least squares analysis to evaluate the band strengths.

Nadler, Shachar↗
NASA NTRS1991

High performance addition-type thermoplastics (ATTs) - Evidence for the formation of a Diels-Alder adduct in the reaction of an acetylene-terminated material and a bismaleimide

Recently, the concept and demonstration of a new versatile synthetic reaction for making a large number of high-performance addition-type thermoplastics (ATTs) were reported. The synthesis shows promise for providing polymers having an attractive combination of easy processability, good toughness, respectable high temperature mechanical performance, and excellent thermo-oxidative stability. The new chemistry involves the reaction of an acetylene-terminated material with a bismaleimide or benzoquinone. In order to clarify the reaction mechanism, model compound studies were undertaken in solutions as well as in the solid state. The reaction products were purified by flash chromatography and characterized by conventional analytical techniques including NMR, FT-IR, UV-visible, mass spectroscopy, and high pressure liquid chromatography. The results are presented of the model compound studies which strongly support the formation of a Diels-Alder adduct in the reaction of an acetylene-terminated compound and a bismaleimide or benzoquinone.

Pater, R. H.↗
NASA NTRS1992

Modification of primordial ices by cosmic rays as simulated by cyclotron irradiation

Frozen CH4 and CH4/Ar mixtures closed into metal cuvettes and open to the vacuum were irradiated at 15 and 77 K with 10 - 20 MeV p and He-3(2+) ions in order to simulate the effect of cosmic rays on solid organic matter in space. Ices exposed to vacuum represent surfaces of icy systems whereas closed systems stand for bulk ices. The products were analyzed by MS, SEM, RBS, ERDA, H-1-NMR, HPLC, GC-MS, NEXAFS, and FT-IR. Volatile products consisted of a mixture of low molecular species, e.g., C2H2, C2H4, C2H6, and long linear aliphatic and olefinic compounds. The formation of polycyclic aromatic hydrocarbons (PAH's) and related species in solid CH4 is due to a multi-center reaction within one collision cascade and is governed by energy density effects with critical linear energy transfer values L(sub T) between 2 and 10 keV/micron. Open ices exhibit preferential hydrogen release resulting in an increased carbonization as compared to more hydrogen rich molecules protected inside large icy bodies.

Kaiser, R. I.↗
NASA NTRS1998

In Situ Infrared Spectroscopy of the Gaseous Species Present in a Diamond Chemical Vapor Deposition System

We interfaced a Hot-Filament Chemical Vapor Deposition (HFCVD) system to the emission port of an FT-IR spectrometer, in order to study the gas phase species present during the deposition of diamond thin films. The implementation of the infrared (IR) emission technique in situ allowed the study of various carbon-containing species believed to be crucial in diamond film growth. The two IR-active vibrational fundamentals of methane, v(3)(f2) and v(4)(f2), were observed at three different filament temperatures: 1000, 1500 and 2000 C. However, the net signal of v(3) was emission, while that of v(4) was absorption. These results indicate that the v(4) fundamental is excited beyond equilibrium, while the v(3) fundamental remains mostly in the ground state. This is due to the small concentration of methane, the low energy of v(4) compared to v(3) or to the Hz vibrational mode, and symmetry considerations that forbid interaction among the four fundamentals of methane. Thus, the excitation of v(3) is more likely than its decay under HFCVD conditions, producing a non-equilibrium population. At a filament temperature of 2000 C, the v(3) (sigma(+)(3)) fundamental of acetylene and a band at 1328 cm-l also ascribed to acetylene (v5 (pi(U)) + v4) appear in net absorption. This correlates well with the onset of molecular hydrogen breaking by the filament, which occurs at temperatures around 2000 C and above. The hydrogen atoms produced in this heterogeneous reaction give rise to a chain of reactions that lead to acetylene, among other carbonaceous species.

Morell, G.↗
NASA NTRS1998

Fluoropolymer Films Deposited by RF Plasma Sputtering of Polytetrafluoroethylene Using Inert Gases

The FT-IR (Fourier Transform Infrared), UV (Ultraviolet) and XPS (X Ray Photoelectron Spectroscopy) spectra of fluoropolymer films (SPTFE) deposited by rf (radio frequency) plasma sputtering of polytetrafluoroethylene (PTFE), using Ne, Kr and Xe as sputtering gases, were obtained and compared with prior spectra for SPTFE formed using He and Ar. The F/C (fluorine / carbon) ratios for SPTFE films (1.44-1.55), obtained at a rf power of 10 W, were essentially the same for all five rare gases, there being no trend of decreasing fluorine content in the SPTFE product with increasing atomic weight of the sputtering gas - contrary to the momentum transfer notion advanced by M. E. Ryan, et al. Increasing rf power from 10 to 50 W resulted in successively lower F/C ratios for SPTFE (e.g., from 1.55 to 1.21 in the case of Xe plasma-sputtered PTFE), accompanied by sputtering of the glass reactor and deposition of fragments of sodium aluminum silicate occurring at 40 W and above. In order to achieve a "Teflon-like" SPTFE structure (i.e., products with as high a F/C ratio as possible) in a given plasma reactor, an optimum rf power must be found, which in the present case was approximately 10 W.

Golub, Morton A.↗