Gas-phase acidities of alcohols
Gas phase acidities of aliphatic alcohols by ion cyclotron resonance spectroscopy
Blair, L. K.↗
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Adherence of sputtered titanium carbides
Sputtered coatings of the refractory metal carbides are of great interest for applications where hard wear-resistant materials are desired. The usefulness of sputtered refractory carbides is often limited, in practice, by spalling or interfacial separation. In this work improvements in the adherence of refractory carbides on iron, nickel and titanium based alloys were obtained by using oxidation, reactive sputtering or sputtered interlayers to alter the coating-substrate interfacial region. X-ray photoelectron spectroscopy and argon ion etching were used to characterize the interfacial regions, and an attempt was made to correlate adherence as measured in wear tests with the chemical nature of the interface.
Brainard, W. A.↗
Metal-dielectric interactions
Metal direlectric surface interactions and dielectric films on metal substrates were investigated. Since interfacial interaction depends so heavily on the nature of the surfaces, analytical surface tools such as Auger emission spectroscopy, X-ray photoelectron spectroscopy and field ion microscopy were used to assist in surface and interfacial characterization. The results indicate that with metals contacting certain glasses in the clean state interfacial, bonding produces fractures in the glasses while when a film such as water is present, fractures occur in the metal near the interface. Friction forces were used to measure the interfacial bond strengths. Studies with metals contacting polymers using field ion microscopy revealed that strong bonding forces could develop being between a metal and polymer surface with polymer transferring to the metal surface in various ways depending upon the forces applied to the surface in contact. With the deposition of refractory carbides, silicides and borides onto metal and alloy substrates the presence of oxides at the interface or active gases in the deposition plasma were shown to alter interfacial properties and chemistry. Auger ion depth profile analysis indicated the chemical composition at the interface and this could be related to the mechanical, friction, and wear behavior of the coating.
Buckley, D. H.↗
Improved adhesion of sputtered refractory carbides to metal substrates
Sputtered coatings of the refractory metal carbides are of great interest for applications where hard wear-resistant materials are desired. The usefulness of sputtered refractory carbides is often limited in practice by spalling or interfacial separation. In this work improvements in the adherence of refractory carbides on iron, nickel and titanium base alloys were obtained by using oxidation, reactive sputtering or sputtered interlayers to alter the coating-substrate interfacial region. X-ray photoelectron spectroscopy and argon ion etching were used to characterize the interfacial regions, and an attempt was made to correlate adherence as measured in wear tests with the chemical nature of the interface.
Wheeler, D. R.↗
Electron impact spectroscopy
The concepts of electron impact spectroscopy are discussed, comparing the electron spectroscopy techniques with those of the optical spectroscopy. The main advantage of the electron spectroscopy is to be found in the elimination of optical selection rules in excitation processes and the ability to scan the spectrum from the infrared to the X-ray region. The range of the method is indicated through a review of several examples, including electron impact excitation of Ba and rotational excitation of H2. The sensitivity of the method is demonstrated by vibrational excitation spectrum of N2. It is shown that the application of the method to the inner-shell excitation allows to obtain information about molecular species which are not commonly available, while spectroscopy of negative ions yields information about their energy and symmetry properties. However, the techniques are still under development and more data are expected to become available in the coming years.
Trajmar, S.↗
Gas chromatography: Possible application of advanced instrumentation developed for solar system exploration to space station cabin atmospheres
Gas chromatography (GC) technology was developed for flight experiments in solar system exploration. The GC is a powerful analytical technique with simple devices separating individual components from complex mixtures to make very sensitive quantitative and qualitative measurements. It monitors samples containing mixtures of fixed gases and volatile organic molecules. The GC was used on the Viking mission in support of life detection experiments and on the Pioneer Venus Large Probe to determine the composition of the venusian atmosphere. A flight GC is under development to study the progress and extent of STS astronaut denitrogenation prior to extravehicular activity. Advanced flight GC concepts and systems for future solar system exploration are also studied. Studies include miniature ionization detectors and associated control systems capable of detecting from ppb up to 100% concentration levels. Further miniaturization is investigated using photolithography and controlled chemical etching in silicon wafers. Novel concepts such as ion mobility drift spectroscopy and multiplex gas chromatography are also developed for future flight experiments. These powerful analytical concepts and associated hardware are ideal for the monitoring of cabin atmospheres containing potentially dangerous volatile compounds.
Carle, G. C.↗
Theoretical study of the spectroscopy of Al2(+)
The electronic states of Al2(+) below about 40,000/cm are studied using a CASSCF/MRCI approach in a large Gaussian basis set. The computed spectroscopic constants, excitation energies, Einstein coefficients, and radiative lifetimes should give insight into the spectroscopy of this ion.
Rosi, Marzio↗
Hot ion plasma heating experiments in SUMMA
Initial results are presented for the hot-ion plasma heating experiments conducted in the new SUMMA (superconducting magnetic mirror apparatus) at NASA Lewis Research Center. A discharge is formed by applying a radially inward dc electric field between cylindrical anodes and hallow cathodes located at the peak of the mirrors. Data were obtained at midplane magnetic field strengths from 1.0 to 3.5 tesla. Charge-exchange neutral particle energy analyzer data were reduced to ion temperatures using a plasma model that included a Maxwellian energy distribution superimposed on an azimuthal drift, finite ion orbits, and radial variations in density and electric field. The best ion temperatures in a helium plasma were 5 keV and in hydrogen the H2(+) and H(+) ions were 1.2 keV and 1 keV respectively. Optical spectroscopy line broadening measurements yielded ion temperatures about 50 percent higher than the charge-exchange neutral particle analyzer results. Spectroscopically obtained electron temperature ranged from 3 to 30 eV. Ion temperature was found to scale roughly linearly with the ratio of power input-to-magnetic field strength, P/B.
Reinmann, J. J.↗
Laser Optogalvanic Spectroscopy pf Neon and Argon in a Discharge Plasma and its Significance for Microgravity Combustion
A detailed study of combustion mechanisms in flames, employing laser-based diagnostics, has provided good knowledge and understanding of the physical phenomena, and led to better characterization of the dynamical and chemical combustion processes, both under low-gravity (in space) and normal gravity (in ground based facilities, e.g. drop towers). Laser induced fluorescence (LIF), laser-induced incandescence (LII) and LIF thermometry have been widely used to perform nonintrusive measurements and to better understand combustion phenomena. Laser optogalvanic (LOG) spectroscopy has well-established applications in ion mobility measurements, atomic and molecular spectroscopy, ionization rates, recombination rates, velocity measurements and as a combustion probe for trace element detection. Absorption spectra of atomic and molecular species in flames can be obtained via LOG spectroscopy by measuring the voltage and current changes induced by laser irradiation. There are different kinds of processes that contribute to a discharge current, namely: (1) electron impact ionization, (2) collisions among the excited atoms of the discharge species and (3) Penning ionization. In general, at higher discharge currents, the mechanism of electron impact ionization dominates over Penning ionization, whereby the latter is hardly noticeable. In a plasma, whenever the wavelength of a laser coincides with the absorption of an atomic or molecular species, the rate of ionization of the species momentarily increases or decreases due to laser-assisted acceleration of collisional ionization. Such a rate of change in the ionization is monitored as a variation in the transient current by inserting a high voltage electrode into the plasma. Optogalvanic spectroscopy in discharges has been useful for characterizing laser line-widths and for providing convenient calibration lines for tunable dye lasers in the ultraviolet, visible and infrared wavelength regions. Different kinds of quantitative information, such as the electron collisional ionization rate, can be extracted from the complex processes occurring within the discharge. In the optogalvanic effect (OGE), there is no problem of overlap from background emissions, and hence even weak signals can be detected with a high signal-to-noise ratio, which makes the optogalvanic effect sensitive enough to resolve vibrational changes in molecular bonds and differences in energy levels brought about by different electron spins. For calibration purposes, neon and argon gaseous discharges have been employed most extensively, because these gases are commonly used as buffer gases within hollow-cathode lamps and provide an acceptable density of calibration lines. In the present work, our main aim has been to understand the dominant physical processes responsible for the production of the OGE signal, based on the extensive time resolved optogalvanic waveforms recorded, and also to extract quantitative information on the rates of excited state collisional processes.
Misra, Prabhakar↗
Soluble Organic Matter (SOM) analysis of the Hayabusa2 samples: The first results
The Hayabusa2 spacecraft successfully collected the surface and possible sub-surface materials of the asteroid 162173 Ryugu. Ryugu is a C-type asteroid characterized by a low-albedo surface probably consisting of hydrous minerals and carbonaceous materials. [1] The direct optical and spectral analysis of the returned samples indicates that Ryugu material is dominated by hydrous carbonaceous chondrite-like matter (similar to CI chondrites) [2]. Since carbonaceous chondrites have generally yielded various types of organic matter, the collected Ryugu grains are expected to contain diverse types of organic compounds including bio-related molecules. The occurrence of organic compounds in the Ryugu surface will provide clues to the evolution of prebiotic molecules and their preservations associated with aqueous alteration of the primitive asteroid. The initial analysis of soluble organic matter (SOM) of the Hayabusa2-returned samples has been performed by an international team consisting of 32 members. Because the sample amount available for comprehensive SOM analyses is limited, and because the SOM is expected to be present as a complex mixture of various types of organic compounds with very small concentrations of each compound, high-sensitivity and high-resolution analytical techniques have been developed using carbonaceous meteorites [e.g. 3]. Two aggregate samples of the Ryugu grains (A106 and C107) were allocated for the solvent extractions and bulk carbon (C), hydrogen (H), nitrogen (N), sulfur (S) and oxygen (O) measurements. The A106 sample was collected during the 1st sampling in February 2019 and the C107 sample was collected during the 2nd sampling in July 2019 after the Small Carry Impactor (SCI) operation. They consist mainly of particles smaller than 1 mm in diameter, and each sample mass was 38-39 mg. They were firstly investigated spectroscopically in the near infrared wavelength range by the Stone Team prior to the solvent extractions. Other small grains (A0080 and C0057) were also allocated for this study to investigate the spatial distribution of organic compounds on the sample surface. The extraction and analytical measurements implemented by the SOM Team are summarized in Figure 1. Each powder sample was extracted sequentially with non-polar to polar solvents, i.e., hexane, dichloromethane (DCM), methanol (MeOH) and H2O, for non-targeted analysis to reveal the compound composition. Each solvent extract was analyzed by solution state nuclear magnetic resonance (NMR) spectroscopy [4], Fourier transform- ion cyclotron resonance/mass spectrometry (FT-ICR/MS) with ESI and APPI ionization [5] and by high-resolution mass spectroscopy using Orbitrap MS coupled with nano-liquid chromatography (nanoLC/Orbitrap MS) [6], and using two dimensional gas chromatography/mass spectrometry (GC×GC/MS). The extracted residues were passed to the Chemistry Team for further inorganic element analysis. The other powder sample was subjected to the hot water extraction for amino acid analyses including chiral isomer separation, which was performed by three-dimensional (3D) high-performance liquid chromatography (HPLC) with high-sensitivity fluorescence detection (FD) [7] and by HPLC/FD coupled with quadrupole-time of flight/mass spectrometry (QToF/MS) [8]. After the hot water extraction, the residue was split into two halves. One half was further extracted with hydrochloric acid (HCl) to analyze for amino acids in bound-form. The other half was sequentially extracted with DCM/MeOH (1/1) to analyze semi-polar compounds such as polycyclic aromatic hydrocarbons (PAHs) by GC/MS, followed by further extraction with formic acid to analyze polar heterocyclic compounds, and subsequent extraction with HCl to detect bound-form polar compounds. The extracted residues were passed to the IOM Team for the analysis of insoluble organic matter (IOM). Compound-specific stable isotope analyses will be performed using GC/combustion/isotope ratio mass spectrometry (GC/C/IRMS) if the compound concentration is high enough to enable such an isotopic measurement. All extraction procedures were performed on an ISO 6 (Class 100) clean bench inside an ISO 5 (Class 1000) clean room. Baked serpentine powder was also analyzed as a procedural blank. In situ organic compound analysis with the molecular imaging was performed using desorption electrospray ionization (DESI) equipped with Orbitrap MS [9, 10], followed by spatial imaging of organic compounds using ToF/secondary ion mass spectrometry (ToF/SIMS) [11]. The bulk chemical and isotopic compositions of CNS and HO were determined using nano-elemental analysis/isotope ratio mass spectrometry (nanoEA/IRMS) [12] and EA/pyrolysis/IRMS, respectively. We have identified a variety of indigenous organic compounds in the extracts of both A106 and C107 samples. The Ryugu grains host organic molecules under the high-vacuum and cosmic-ray irradiation environment of the asteroid surface. The analysis of extracted molecules is in progress, and the first results will be presented at the symposium.
Hiroshi Naraoka↗
Concerning Apparent Similarity of Structures of Fluoropolymer Surfaces Exposed to an Argon Plasma or Argon Ion Beam
X-ray photoelectron spectroscopy (XPS) C(sub 1s) spectra of fluoropolymers exposed to either an argon plasma or argon ion beam show remarkable similarity, implying that the surface-modification reactions for these two processes likely proceed through comparable mechanisms, revolving predominantly ion-surface interactions. The importance of working with a monochromatized x-ray source for XPS analysis of the surface-modified fluoropolymers is once again emphasized.
Golub, Morton A.↗
Optogalvanic photodetachment spectroscopy
A new extension to optogalvanic spectroscopy, in which electrons detached from negative ions formed in the discharge are observed as a function of incident laser wavelength, has been developed. The determination of the electron affinities of I(-) and Cl(-) atomic ions is described. The potential of the technique for studying the spectroscopy of molecular negative ions is also discussed.
Mcdermid, I. S.↗
Indium Single-Ion Frequency Standard
A single laser-cooled indium ion is a promising candidate for an ultimate resolution optical time or frequency standard. It can be shown that single ions from group IIIA of the periodic table (indium, thallium, etc.) can have extremely small systematic errors. In addition to being free from Doppler, transit-time and collisional shifts, these ions are also quite insensitive to perturbations from ambient magnetic and electric fields (mainly due to the use of a J=0-0 transition for spectroscopy). Of all group IIIA ions, indium seems to be the most practical, since it is heavy enough to have a tolerable intercombination cooling transition rate and (unlike thallium) has transitions which are easily accessible with frequency multiplied continuous-wave lasers. A single indium ion standard has a potential inaccuracy of one part in 10(exp 18) for integration times of 10(exp 6) seconds. We have made substantial progress during the grant period in constructing a frequency standard based upon a single indium ion. At the beginning of the grant period, single indium ions were being successfully trapped, but the lasers and optical systems were inadequate to achieve the desired goal. We have considerably improved the stability of the dye laser used to cool the ions and locked it to a molecular resonance line, making it possible to observe stable cooling-line fluorescence from a single indium ion for reasonable periods of time, as required by the demands of precision spectroscopy. We have substantially improved the single-ion fluorescence signal with significant benefits for the detection efficiency of forbidden transitions using the 'shelving' technique. Finally, we have constructed a compact, efficient UV 'clock' laser and observed 'clock' transitions in single indium ions using this laser system. We will elaborate on these accomplishments.
Nagourney, Warren↗
Mid-Infrared Spectroscopy of Polycyclic Aromatic Nitrogen Heterocycles (PANHS) and their Ions
In recent years, polycyclic aromatic nitrogen heterocycles (PANHs) have attracted a good deal of attention because of their potent carcinogenic and mutagenic properties, and their prevalence in our environment. Such species also play a prominent role in the chemistry of life up to and including the very nucleobases from which our DNA is constructed. Surprisingly, these compounds may even be common outside of our terrestrial environment. To wit, it is now widely accepted that polycyclic aromatic materials are abundant in space and represent a major reservoir of organic carbon in the interstellar medium and developing planetary systems. Given that nitrogen is the fourth most abundant chemically reactive element in space (surpassed only by hydrogen, carbon, and oxygen), it is entirely reasonable to suspect that PANHs may represent an important component of that organic reservoir. Motivated by their intrinsic merit and with special attention toward evaluating their exobiological significance, we have initiated a program to study the spectroscopic and chemical properties of P A " s under conditions relevant to extraterrestrial environments. Here we present the first results of that program-infrared spectroscopic measurements on a series of PANH"s in neutral and cationic forms, isolated in inert matrices at cryogenic temperatures.temperatures. The species studied include: 1 -, and 2-azabenz[a]anthracene, 1-, 2-, and 4- azachrysene, dibenz[a,h]acridine, and dibenz[a,J)acridine. The experimental measurements are also compared with theoretical spectra calculated using density functional theory. General spectroscopic trends observed in this series of compounds are discussed and the implications of these results for Astrophysics and Exobiology are considered.
Mattioda, Andrew L.↗
SPUTTERING ION SOURCE FOR SOLIDS
Sputtering argon ion source used for analysis of solids provides more stable operation than a spark source and allows electrometric recording of the mass spectrum
MASS SPECTROSCOPY↗
Tribological characteristics of nitrogen (N+) implanted iron
The effect of implantation of nitrogen ions (1.5 MeV) on the friction and wear characteristics of pure ion sliding against M-50 steel (unimplanted) was studied in a pin-on-disk sliding friction apparatus. Test conditions included room temperature (25 C), a dry air atmosphere, a load of 1/2 kg (4.9 N), sliding velocities of 0.043 to 0.078 m/sec (15 to 25 rpm), a pure hydrocarbon lubricant (n-hexadecane), or a U.S.P. mineral oil and nitrogen ion implantation doses of 5x10 to the 15th power and 5x10 to the 17th power ions/sq cm. No differences in wear rates were observed in the low dose experiments. In the high dose experiments, small reductions in initial (40 percent) and steady state (20 percent) wear rates were observed for nitrogen implanted iron riders as compared with unimplanted controls. No differences in average friction coefficients were noted for either dose. Auger electron spectroscopy combined with argon ion bombardment revealed a subsurface Gaussian nitrogen distribution with a maximum concentration of 6 atomic percent at a depth of 0.8 microns. Similar analysis within the wear scar of an implanted rider after 20 microns of wear yielded only background nitrogen concentration. No inward migration of nitrogen ions was observed.
Jones, W. R.↗
Tribological characteristics of nitrogen (N+) implanted iron
The effect of implantation of nitrogen ions (1.5 MeV) on the friction and wear characteristics of pure ion sliding against M-50 steel (unimplanted) was studied in a pin-on-disk sliding friction apparatus. Test conditions included room temperature (25 C), a dry air atmosphere, a load of 1/2 kg (4.9 N), sliding velocities of 0.043 to 0.078 m/sec (15 to 25 rpm), a pure hydrocarbon lubricant (n-hexadecane), or a U.S.P. mineral oil and nitrogen ion implantation doses of 5x10 to the 15th power and 5x10 to the 17th power ions/sq cm. No differences in wear rates were observed in the low dose experiments. In the high dose experiments, small reductions in initial (40 percent) and steady state (20 percent) wear rates were observed for nitrogen implanted iron riders as compared with unimplanted controls. No differences in average friction coefficients were noted for either dose. Auger electron spectroscopy combined with argon ion bombardment revealed a subsurface Gaussian nitrogen distribution with a maximum concentration of 6 atomic percent at a depth of 0.8 microns. Similar analysis within the wear scar of an implanted rider after 20 microns of wear yielded only background nitrogen concentration. No inward migration of nitrogen ions was observed. Previously announced in STAR as N82-24322
Jones, W. R., Jr.↗
Zeeman anisotropy fluorescence spectroscopy, characteristic radiative lifetimes, and novel site symmetries in KCl-Sm/2 plus/
Sm double plus ion sites distribution in KCl by spectroscopy
Chilver, C. R.↗