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All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Reduced Order Models for Liquid Hydrogen Pooling and Vaporization Supported by Experiments

In the event of a leak of liquid hydrogen, a pool can form that vaporizes, disperses, and eventually dilutes to a non-flammable mixture. In this work, we describe fast-running models for the pooling and vaporization of liquid hydrogen in a steady cross-wind. Several pooling models from the literature are compared to solve for the flow and extent of the pool. The size of the pool can serve as the source for a separate dispersion model, which builds upon the existing one-dimensional Gaussian plume model in HyRAM+. Additional terms for the effects of a cross-wind on momentum and entrainment were added so that the model could handle the effects of a cross-wind on a low-speed flow. The models are compared to experimental data on pooling extent and downwind dispersion for steady flow rates of liquid hydrogen in a steady cross-wind. In the two compared experiments, liquid flow rates of 15 and 45 g/s were spilled onto concrete in cross-winds of approximately 1.8 m/s. The rate of growth of the pool and the downwind concentration boundaries are compared to the models, showing good agreement, although additional tuning is needed. These models can contribute to the advancement of codes and standards for liquid hydrogen systems.

dispersion↗
NASA NTRS1977

Geochemical and mineralogical interpretation of the Viking inorganic chemical results

The current status of geochemical, mineralogical, petrological interpretation of refined Viking Lander data is reviewed, and inferences that can be drawn from data on the composition of Martian surface materials are presented. The materials are dominantly fine silicate particles admixed with, or including, iron oxide particles. Both major element and trace element abundances in all samples are indicative of mafic source rocks (rather than more highly differentiated salic materials). The surface fines are nearly identical in composition at the two widely separated Lander sites, except for some lithologic diversity at the 100-m scale. This implies that some agency (presumably aeolian processes) has thoroughly homogenized them on a planetary scale. The most plausible model for the mineralogical constitution of the fine-grained surface materials at the two Lander sites is a fine-grained mixture dominated by iron-rich smectites, or their degradation products, with ferric oxides, probably including maghemite and carbonates (such as calcite), but not such less stable phases as magnesite or siderite.

Toulmin, P., III↗
NASA NTRS1989

High angle-of-attack aerodynamic characteristics of crescent and elliptic wings

Static longitudinal and lateral-directional forces and moments were measured for elliptic- and crescent-wing models at high angles-of-attack in the NASA Langley 14 by 22-Ft Subsonic Tunnel. The forces and moments were obtained for an angle-of-attack range including stall and post-stall conditions at a Reynolds number based on the average wing chord of about 1.8 million. Flow-visualization photographs using a mixture of oil and titanium-dioxide were also taken for several incidence angles. The force and moment data and the flow-visualization results indicated that the crescent wing model with its highly swept tips produced much better high angle-of-attack aerodynamic characteristics than the elliptic model. Leading-edge separation-induced vortex flow over the highly swept tips of the crescent wing is thought to produce this improved behavior at high angles-of-attack. The unique planform design could result in safer and more efficient low-speed airplanes.

Vandam, C. P.↗
NASA NTRS1989

High-alpha aerodynamic characteristics of crescent and elliptic wings

Static longitudinal and lateral-directional forces and moments were measured for elliptic- and crescent-wing models at high angles of attack in the NASA Langley 14-by-22-ft Subsonic Tunnel. The forces and moments were obtained for an angle-of-attack range including stall and post-stall conditions at a Reynolds number based on the average wing chord of about 1.8 million. Flow-visualization photographs using a mixture of oil and titanium-dioxide were also taken for several incidence angles. The force and moment data and the flow-visualization results indicated that the crescent wing model with its highly swept tips produced much better high-angle-of-attack aerodynamic characteristics than the elliptic model. Leading-edge separation-induced vortex flow over the highly swept tips of the crescent wing is thought to produce this improved behavior at high angles of attack. The unique planform design could result in safer and more efficient low-speed airplanes.

Van Dam, C. P.↗
DOE OSTI2021

Experimental and modeling studies of PR and ND oxalate solubility to high ionic strengths: Insight into actinide(III) oxalates

Actinide oxalates are chemical compounds important to nuclear industry, ranging from actinide separation in waste reprocessing, to production of specialty actinides, and to disposal of high level nuclear waste (HLW) and spent nuclear fuel (SNF). In this study, the solubility constants for Pr 2 (C 2 O 4 ) 3 •10H 2 O and Nd 2 (C 2 O 4 ) 3 •10H 2 O by performing solubility experiments in HNO 3 and mixtures of HNO 3 and H 2 C 2 O 4 at 23.0 ± 0.2 °C have been determined. The targeted starting materials, Pr 2 (C 2 O 4 ) 3 •10H 2 O and Nd 2 (C 2 O 4 ) 3 •10H 2 O, were successfully synthesized at room temperature using PrCl 3 , NdCl 3 and oxalic acid as the source metrials. Then, we utilized the targeted solubility-controlling phases to conduct solubility measurements. There was no phase change over the entire periods of experiments, demonstrating that Pr 2 (C 2 O 4 ) 3 •10H 2 O and Nd 2 (C 2 O 4 ) 3 •10H 2 O were the solubility-controlling phases in our respective experiments. Based on our experimental data, we have developed a thermodynamic model for Pr 2 (C 2 O 4 ) 3 •10H 2 O and Nd 2 (C 2 O 4 ) 3 •10H 2 O in the mixtures of HNO 3 and H 2 C 2 O 4 to high ionic strengths. The model for Pr 2 (C 2 O 4 ) 3 •10H 2 O reproduces well the reported experimental data for Pu 2 (C 2 O 4 ) 3 •10H 2 O, which are not utilized for the model development, demonstrating that Pr(III) is an excellent analog for Pu(III). Similarly, the model for Nd 2 (C 2 O 4 ) 3 •10H 2 O reproduces the solubility of Am 2 (C 2 O 4 ) 3 •10H 2 O and Cm 2 (C 2 O 4 ) 3 •10H 2 O. The Pitzer model was used for the calculation of activity coefficients. Based on the published, well established model for dissociation constants for oxalic acid and stability constants for actinide-oxalate complexes [i.e., AmC 2 O 4 + , and Am(C 2 O 4 ) 2 - ] to high ionic strengths, we have obtained the solubility constants (log 10 K 0 ) for the following reactions at 25 °C, Pr 2 (C 2 O 4 ) 3 •10H 2 O ⇌ 2Pr 3+ + 3C 2 O 4 2- + 10H 2 O(l). Nd 2 (C 2 O 4 ) 3 •10H 2 O ⇌ 2Nd 3+ + 3C 2 O 4 2- + 10H 2 O(l). to be -30.82 ± 0.30 (2σ), and - 31.14 ± 0.35 (2σ), respectively. These values for can be directly applied to Pu 2 (C 2 O 4 ) 3 •10H 2 O, Am 2 (C 2 O 4 ) 3 •10H 2 O and Cm 2 (C 2 O 4 ) 3 •10H 2 O. The model established for actinide oxalates by this study provides the needed knowledge with regard to solubilities of actinide/REE oxalates at various ionic strengths, and is expected to find applications in many fields, including the geological disposal of nuclear waste and the mobility of REE under the surface conditions, as Pr 2 (C 2 O 4 ) 3 •10H 2 O and Nd 2 (C 2 O 4 ) 3 •10H 2 O can be regarded as the pure Pr and Nd end-members of deveroite, a recently discovered natural REE oxalate with the following stoichiometry, (Ce 1.01 Nd 0.33 La 0.32 Pr 0.11 Y 0.11 Sm 0.01 Pb 0.04 U 0.03 Th 0.01 Ca 0.04 ) 2.01 (C 2 O 4 ) 2.99 •9.99H 2 O. Regarding its importance in the geological disposal of nuclear waste, Am 2 (C 2 O 4 ) 3 •10H 2 O/Pu 2 (C 2 O 4 ) 3 •10H 2 O/Cm 2 (C 2 O 4 ) 3 •10H 2 O can be the source-term phase for actinides, as demonstrated by the instance in the disposal in clay/shale formations. This is exemplified by the stability of Am 2 (C 2 O 4 ) 3 •10H 2 O in comparison with Am(OH) 3 (am), Am(OH) 3 (s) and AmCO 3 (OH)(s) under the relevant geological repository conditions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1991

Homogeneity of spatial correlation statistics of tropical oceanic rainfall

The possibility of uniform horizontal correlation scales for tropical oceanic rainfall has been examined by a study of satellite-observed microwave data as a proxy measure of rain rates. From the brightness temperatures from the electrically scanning microwave radiometer on Nimbus 5 near nadir during the year 1974, the mean spatial autocorrelation function as a function of simultaneous pixel separation was calculated in each 5 by 5 deg grid box over the tropical Pacific and Atlantic for each season. The equal-time spatially lagged correlations were compared for geographical dependence to investigate the hypothesis of homogeneity. A simple model of the spatial statistics of the microwave brightness temperatures was used, consisting of a mixture of uncorrelated spatial white noise incoherently superimposed on a spatially correlated field (spatial red noise). The red noise signals are presumed to be generated by convective activity in the tropical atmosphere. The parameters of the red noise are consistent with this scheme over the tropical oceans, yielding a uniform spatial scale of about 50 km throughout.

Shin, Kyung-Sup↗
NASA NTRS2008

Fiber-Optic Determination of N2, O2, and Fuel Vapor in the Ullage of Liquid-Fuel Tanks

A fiber-optic sensor system has been developed that can remotely measure the concentration of molecular oxygen (O2), nitrogen (N2), hydrocarbon vapor, and other gases (CO2, CO, H2O, chlorofluorocarbons, etc.) in the ullage of a liquid-fuel tank. The system provides an accurate and quantitative identification of the above gases with an accuracy of better than 1 percent by volume (for O2 or N2) in real-time (5 seconds). In an effort to prevent aircraft fuel tank fires or explosions similar to the tragic TWA Flight 800 explosion in 1996, OBIGGS are currently being developed for large commercial aircraft to prevent dangerous conditions from forming inside fuel tanks by providing an inerting gas blanket that is low in oxygen, thus preventing the ignition of the fuel/air mixture in the ullage. OBIGGS have been used in military aircraft for many years and are now standard equipment on some newer large commercial aircraft (such as the Boeing 787). Currently, OBIGGS are being developed for retrofitting to existing commercial aircraft fleets in response to pending mandates from the FAA. Most OBIGGS use an air separation module (ASM) that separates O2 from N2 to make nitrogen-enriched air from compressed air flow diverted from the engine (bleed air). Current OBIGGS systems do not have a closed-loop feedback control, in part, due to the lack of suitable process sensors that can reliably measure N2 or O2 and at the same time, do not constitute an inherent source of ignition. Thus, current OBIGGS operate with a high factor-of-safety dictated by process protocol to ensure adequate fuel-tank inerting. This approach is inherently inefficient as it consumes more engine bleed air than is necessary compared to a closed-loop controlled approach. The reduction of bleed air usage is important as it reduces fuel consumption, which translates to both increased flight range and lower operational costs. Numerous approaches to developing OBIGGS feedback-control sensors have been under development by many research groups and companies. However, the direct measurement of nitrogen (N2) is a challenge to most OBIGGS ullage sensors (such as tunable diode laser absorption) as they cannot measure N2 directly but depend on the measurement of oxygen (O2). The problem with a singular measure of O2, is that as the concentration (number density) of O2 decreases due to the inerting process or due to lower pressures from high altitudes, the precision and accuracy of the O2 measurement decreases. However, measuring O2 density in combination with N2 density (which is more abundant in air and in a N2-inerted fuel tank) can provide a much more accurate and reliable determination of the OBIGGS efficacy.

Nguyen, Quang-Viet↗
DOE OSTI2022

Characterizing the Solvation Characteristics of Deep Eutectic Solvents Composed of Active Pharmaceutical Ingredients as a Hydrogen Bond Donor and/or Acceptor

The formation of eutectic mixtures from active pharmaceutical ingredients (APIs) has emerged as an effective technique to develop liquid pharmaceutical formulations. API-based deep eutectic solvents (DESs) enhance the water solubility of APIs and avoid their recrystallization. The physico-chemical properties of API-DESs can be easily modulated by judicious selection of a hydrogen bond acceptor (HBA) or hydrogen bond donor (HBD) excipient that is mixed with the API. Solvation properties of API-DESs can help in understanding the role of ionic and non-ionic excipients towards the overall solvation interactions of these DESs. In this study, the solvation characteristics of three subclasses of API-DESs containing API-HBAs, API-HBDs, or API-HBAs and API-HBDs are investigated. Inverse gas chromatography is employed to study solute-solvent interactions of a variety of probe molecules for twenty different API-DESs. Among the API-DESs comprised of API-HBAs and carboxylic acid or diol-based HBDs, DESs containing diol-based HBDs exhibited stronger dipolar, hydrogen bond basicity, and hydrogen bond acidity interactions compared to carboxylic acid-based HBDs. No significant differences were observed in the solvation properties of DESs comprised of API HBAs and API HBDs. API-DESs comprised of the choline chloride HBA and API-HBDs exhibited stronger hydrogen bond acidity and dipolarity and weaker dispersive-type interactions among the DESs evaluated in this study. An in-depth evaluation of solvation properties for these DESs is important to completely exploit their potential in separation science as well as the fields of biomaterial science, pharmaceutical chemistry, and biotechnology.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Single-Walled Zeolitic Nanotube–Poly(oxazoline) Nanocomposites as Heterogeneous Catalysts for Acid–Base Cascade Reactions

Zeolites with a unique, 1-dimensional form factor were recently discovered − zeolite nanotubes (ZNTs). Here we describe the synthesis and characterization of NaH-ZNTpoly( oxazoline) composites targeting liquid-phase acid−base cascade catalysis. NaH-ZNT, a one-dimensional zeolite analogue with mesoporosity (3−4 nm) associated with nanotubes and inherent Brønsted acid sites associated with the microporous zeolite domains, is functionalized with poly(oxazoline)-based triblock copolymers with varying molecular weights (3−17 kDa). The composites are characterized using N2 sorption, STEM, FTIR, and elemental analysis, confirming successful grafting and preservation of the zeolite nanotube structure. The composites’ catalytic performance is evaluated through separate acid and base reactions, followed by a combined cascade of a deacetalization−Knoevenagel condensation for the synthesis of chalcone compounds. High initial reaction rates are demonstrated, but modest overall cascade product formation rates are observed, attributed to interactions between Brønsted acid sites and base amine groups that occur in the polymer-grafted systems. Physical mixtures of NaH-ZNT-SH and poly(oxazoline)s, lacking covalent linkages between ZNT and the polymer, support this supposition. This work demonstrates the potential of NaH-ZNT-poly(oxazoline) composites for liquid-phase cascade catalysis for synthesizing compounds of potential medicinal interest, highlighting the benefits of the grafting-to approach as well as the need for further optimization of the catalytic performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Development of an In Situ Fission Gas Release Instrument for Fuel Sample Irradiations in the High Flux Isotope Reactor

Experimental measurement of gaseous fission product release with respect to temperature and burnup is a critical aspect of understanding nuclear fuel performance, validating predictive models, and qualifying new fuels. To measure this phenomenon in real-time, Oak Ridge National Laboratory has developed an instrument for measuring in situ fission gas release from small-scale fuel samples irradiated in the High Flux Isotope Reactor (HFIR). The instrument uses a continuous flow of Heover the fuel samples to sweep gaseous fission products from a sealed capsule in the HFIR Be reflector to an instrument station adjacent to the reactor. The instrument station houses two high-purity germanium (HPGe) detectors that measure decay gamma rays from fission products passing through a room temperature dwell chamber placed over the detector crystal. The sealed capsules in the reactor are designed to modulate fuel sample temperatures between 700 and 1,100°C by changing the Ar/He gas mixture surrounding the capsules during irradiation. N-type thermocouples are incorporated into the capsule housing to record real-time fuel temperatures. The capsules are heated primarily by prompt gamma rays emitted from the HFIR core with minimal heat contributions from fission in the fuel samples to minimize temperature gradients in the specimens for separate-effects characterization of the material. This paper describes modeling of time-dependent nuclear heating and fission product formation in fuel samples, thermal characteristics of the in-core capsules, and expected gaseous fission product gamma spectra at the HPGe instrument station.

Mulligan, Padhraic L [ORNL] (ORCID:000000025826540↗
NASA NTRS2024

Enantioselective Three-Dimensional High-Performance Liquid Chromatographic Determination of Amino Acids in the Hayabusa2 Returned Samples from the Asteroid Ryugu

The chirality of amino acids in extraterrestrial materials may provide an insight into the origin of the essential L-enantiopure amino acids in the terrestrial biosphere. In 2020, the Hayabusa2 mission succeeded in bringing back surface materials from the C-type asteroid (162173) Ryugu to the Earth. Amino acids were one of the targeted organic molecules to be studied in the Ryugu samples. To analyze the various structural isomers of amino acids, which were expected to be present, from the limited amount of the returned samples, the development of a highly-sensitive and selective analytical method was necessary. In the present study, a three-dimensional high-performance liquid chromatography (3D-HPLC) system has been developed for the enantioselective determination of five proteinogenic and three non-proteinogenic amino acids in the Ryugu samples, in which amino acids in the sample were separated by reversed-phase, anion-exchange and enantioselective columns after the fluorescence derivatization with 4-fluoro-7-nitro-2,1,3-benzoxadiozole. The applicability of the analytical system to the extraterrestrial samples was evaluated by analyzing several types of carbonaceous meteorites before applying the system to the Ryugu samples. In the analysis of the Ryugu samples, all of the target amino acids were successfully determined quantitatively. Non-proteinogenic amino acids including 2-amino-n-butyric acid, isovaline and norvaline, rarely present in the terrestrial environment, were found as almost racemic mixtures with 47.1 to 55.2%L.

Amino acids↗
NASA NTRS1979

Nuclear-pumped CO2 laser

The He-3 (n,p)T reaction was examined as an energy source for a CO2 laser. For this purpose He-3 was added to a functioning CO2 electrically excited laser. Initially the laser was run electrically with 12 torr total pressure. The gas mixture was 1:1:8, CO2:N2:He. At zero reactor power, the laser was tested in place next to the core of the Georgia Tech. Research Reactor. After verification of laser action He-3 was added to the system. The He-3 partial pressures of 10 torr, 50 torr, and 300 torr were added in three separate reactor runs. Reactor power ranged from zero to 5 million watts, which corresponds to a peak flux of 10 to the 14th power/sq cm. At reactor powers greater than 10 kW, gain of up to 30 percent was shown. However, indications are this may be due to gamma excitation rather than caused by the He-3 (n,p)T reaction. These results do agree with the data of past CO2 nuclear pumped laser experiments.

Rowe, M.↗
NASA NTRS1987

Spectroscopy of the Kleinmann-Low nebula - Scattering in a solid absorption band

Spectroscopic observations (2.4-3.6 microns) of BN, IRc 2, 3, and 4, and three scattering locations in the KL reflection nebula are reported. A previous report (Knacke et al., 1982) of a 2.97-micron spectral feature in the BN object is not confirmed in the new data. The 2.97-micron feature is observed in sources in the KL nebula, and the spectrum is distorted by a nearby hydrogen line. All the spectra are dominated by absorption along the radiation path, making scattering effects difficult to separate. Scattering could broaden the 3.1-micron interstellar-ice feature, but the effects appear to be small. Except for a long-wavelength wing, the spectra can be modeled reasonably well with core-mantle, silicate-water-ice grains. The wing position and intensity indicate bands of C-H groups of ammonia-ice mixtures.

Knacke, R. F.↗
NASA NTRS1994

Noble gases in presolar diamonds II: Component abundances reflect thermal processing

Using the isotopic compositions derived in Huss and Lewis, 1994a, abundances of the P3, HL, and P6 noble-gas components were determined for 15 diamonds separates from primitive chondrites of 8 chondrite classes. Within a meteorite class, the relative abundances of these components correlate with the petrologic subtype of the host meteorite, indicating that metamorphism is primarily responsible for the variations. Relative abundances of P3, HL, and P6 among diamond samples can be understood in terms of thermal processing of a single mixture of diamonds like those now found in CI and CM2 chondrites. With relatively gentle heating, primitive diamonds first lose their low-temperature P3 gases and a 'labile' fraction of the HL component. Mass loss associated with release of these components produces an increase in the HL and P6 content of the remaining diamond relative to unprocessed diamond. Higher temperatures initiate destruction of the main HL carrier, while the HL content of the surviving diamonds remains essentially constant. At the same time, the P6 carrier begins to preferentially lose light noble gases. Meteorites that have experienced metamorphic temperatures greater than or = 650 C have lost essentially all of their presolar diamond through chemical reactions with surrounding minerals. The P3 abundance seems to be a function only of the maximum temperature experienced by the diamonds and thus is independent of the nature of the surrounding environment. If all classes inherited the same mixture of primitive diamonds, then P3 abundances would tie together the metamorphic scales in different meteorite classes. However, if the P3 abundance indicates a higher temperature than do other thermometers applicable to the host meteorite, then the P3 abundance may contain information about heating prior to accretion. Diamonds in the least metamorphosed EH, CV, and CO chondrites seem to carry a record of pre-accretionary thermal processing.

Huss, Gary R.↗
NASA NTRS2011

Precipitation Characteristics of ISCCP Cloud Regimes for Improving Model Hydrological Budgets

The key in unraveling relationships between precipitation and atmospheric circulations is their common linkage to clouds. Clouds can be described in a variety of ways and several approaches can be adopted to examine their connections to precipitation. We claim that when cloud regimes (aka weather states) from the International Satellite Cloud Climatology Project (ISCCP) are used to conditionally sample/sort and average precipitation data, useful insight and GCM-appropriate diagnostics on the origins and distribution of precipitation can be obtained. The ISCCP cloud regimes are mesoscale (2.5 ) cloud mixtures determined by cluster analysis on joint histograms of cloud optical thickness and cloud top pressure inferred from geostationary and polar orbiter satellite passive retrievals. The ISCCP cloud regime data are combined with GPCP IDD merged surface precipitation data and/or higher temporal and spatial resolution TRMM Multi-Satellite Precipitation Analysis (TMPA) data. The analysis is performed separately for three geographical zones, tropics, and northern/southern midlatitudes (for GPCP; only the tropics can be examined with TMPA data). Our presentation aspires to provide answers to the following questions: (l) What is the mean and variability of surface precipitation produced by each cloud regime at the time of regime occurrence? (2) What is the relative contribution of each cloud regime to the total precipitation within its geographical zone? (3) What is the geographical distribution of precipitation corresponding to particular cloud regime? (4) To what extent are the cloud regimes distinct in terms of their precipitation characteristics and is the regime ordering in terms of convective strength consistent with the observed precipitation intensity?

Lee, D.↗
DOE OSTI2022

Developing a High Value Chemical Coproduct: Bio-Base Insecticides from Catalytic Fast Pyrolysis

Coproduction of biochemicals from the thermochemical conversion of biomass is a strategy to reduce biofuel costs and improve bio-oil quality in an integrated biorefinery. (Challenge) Cost effective separations of coproducts from thermochemical conversion streams remains a challenge largely due to the heterogenous nature and stability of thermochemical conversion streams. (Solution) Bio-based insecticides isolated from catalytic fast pyrolysis (CFP) oils are a viable coproduct that can overcome the oil is more stable, they are a high value product, and they can remain a mixture of components. (Approach) This work focuses on the development of a bio-based insecticide coproduct that is distilled from a catalytic fast pyrolysis bio-oil produced using a platinum on titanium dioxide (Pt/TiO2) catalyst to upgrade pyrolysis vapors.

BIOMASS FUELS↗
DOE OSTI2022

Phase separation in mullite-composition glass

Aluminosilicates (AS) are ubiquitous in ceramics, geology, and planetary science, and their glassy forms underpin vital technologies used in displays, waveguides, and lasers. In spite of this, the nonequilibrium behavior of the prototypical AS compound, mullite (40SiO 2 -60Al 2 O 3 , or AS60), is not well understood. By deeply supercooling mullite-composition liquid via aerodynamic levitation, we observe metastable liquid–liquid unmixing that yields a transparent two-phase glass, comprising a nanoscale mixture of AS7 and AS62. Extrapolations from X-ray scattering measurements show the AS7 phase is similar to vitreous SiO 2 with a few Al species substituted for Si. The AS62 phase is built from a highly polymerized network of 4-, 5-, and 6-coordinated AlO x polyhedra. Polymerization of the AS62 network and the composite morphology provide essential mechanisms for toughening the glass.

36 MATERIALS SCIENCE↗
DOE OSTI2024

A method for generating quantitative vapor-phase infrared spectra of solids: results for phenol, camphor, menthol, syringol, dicyclopentadiene and naphthalene

Here, a method is presented to generate quantitative vapor-phase infrared spectra from substances that naturally occur as solids with moderate volatility. The solid is gravimetrically dissolved into a solvent that has few infrared spectral features, typically CS 2 and CCl 4 separately. The solution is flowed at a constant rate from a linearly pumped syringe into a metered stream of nitrogen carrier gas regulated by a mass flow controller. The analyte/solvent mix is flash vaporized by volatilizing the solution across a heated stainless-steel surface as it emanates from the syringe tip. The N 2 gas-solution mixture is flowed into a long-path White cell thermostatted at a desired temperature, the long optical path compensating for the modest analyte mixing ratio. A composite spectrum is generated from typically ten or more 760-Torr pressure-broadened spectra over the 600 to 6500 cm -1 spectral range at 0.1 cm -1 spectral resolution. The solid analytes reported here using this novel technique include dicyclopentadiene, menthol, syringol, phenol, camphor, and naphthalene.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗