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DOE OSTI2026

Ammonolysis with N 2 -diluted NH 3 suppresses Ta( IV ) defects in BaTaO 2 N and enhances photocatalytic water oxidation

BaTaO 2 N stands out among oxynitride photocatalysts because of its ability to capture visible light and to drive the photoelectrochemical water oxidation reaction. However, its solar energy conversion performance is limited by electron–hole recombination at Ta( IV ) defects in the material. These defects are formed by overreduction of the Ta(v) oxide precursor by excess ammonia under the high temperature conditions during ammonolysis. Here we show for the first time that Ta( IV ) defect concentrations can be lowered by conducting the ammonolysis reaction in mixed NH 3 /N 2 gas. The obtained BaTaO 2 N samples crystallize in the cubic CaTiO 3 structure type and form 200–300 nm faceted nanocrystals, based on X-ray diffraction, scanning electron microscopy, and HRTEM. Electron paramagnetic resonance spectra observe the Ta( IV ) defects at g = 1.999 and confirm an 11-fold reduction for the product synthesized in mixed (0.13 : 1.0 vol) NH 3 /N 2 gas, equivalent to 1.14 × 10 16 cm −3 Ta( IV ) ions. This optimized BaTaO 2 N has nearly twice the photocatalytic oxygen evolution activity (AQE of 6.78% at 400 nm) of a reference material made with 1.0 atm ammonia and 78% higher photoelectrochemical water oxidation photocurrent (0.9 mA cm −2 at 1.23 V vs. RHE) under simulated sunlight. According to X-ray photoelectron spectroscopy, remaining Ta( IV ) defects are concentrated in the surface region of the BaTaO 2 N particles, where >50% of all Ta ions are found in the +4 oxidation state. This surface Ta( IV ) population can be directly observed in Vibrating Kelvin Probe Surface Photovoltage Spectra (VK-SPV) via its 1.2–1.4 eV photovoltage onset. Here, it suggests that the surface Ta( IV ) ions contribute empty d-states 0.5–0.7 eV below the BaTaO 2 N conduction band edge. These findings highlight how the energetics and concentrations of Ta( IV ) defects influence the photoelectrochemical water oxidation ability of BaTaO 2 N. Additionally, the work establishes ammonolysis with diluted NH 3 as a new tool to minimize defects in BaTaO 2 N and to raise its solar energy conversion efficiency toward its theoretical limit. Because of its simplicity, the reduced ammonia pressure strategy will likely be applicable to other oxynitrides, which generally suffer from overreduction problems during ammonolysis.

Salmanion, Mahya [University of California, Davis,↗

NASA NTRS2014

Use Of The Operational Air Quality Monitor (AQM) For In-Flight Water Testing Project

A primary requirement for manned spaceflight is Environmental Health which ensures air and water contaminants, acoustic profiles, microbial flora, and radiation exposures within the cabin are maintained to levels needed for crew health and for vehicle system functionality. The reliance on ground analyses of returned samples is a limitation in the current environmental monitoring strategy that will prevent future Exploration missions beyond low-Earth orbit. This proposal attempts to address this shortcoming by advancing in-flight analyses of water and air. Ground analysis of in-flight, air and water samples typically employ vapor-phase analysis by gas chromatography-mass spectrometry (GC-MS) to identify and quantify organic compounds present in the samples. We envision the use of newly-developed direct ionization approaches as the most viable avenue leading towards an integrated analytical platform for the monitoring of water, air, and, potentially bio-samples in the cabin environment. Development of an in-flight instrument capable of analyzing air and water samples would be the logical next step to meeting the environmental monitoring needs of Exploration missions. Currently, the Air Quality Monitor (AQM) on-board ISS provides this specific information for a number of target compounds in the air. However, there is a significant subset of common target compounds between air and water. Naturally, the following question arises, "Can the AQM be used for both air and water quality monitoring?" Previous directorate-level IR&D funding led to the development of a water sample introduction method for mass spectrometry using electrothermal vaporization (ETV). This project will focus on the integration of the ETV with a ground-based AQM. The capabilities of this integrated platform will be evaluated using a subset of toxicologically important compounds.

Macatangay, Ariel↗

DOE OSTI2022

Impact of Tree Age and Anatomical Fraction on Forest Residue Pyrolysis and Hydrotreating

Utilization of cost-advantaged biomass and waste resources to produce clean, domestic biofuels will be a key factor in decarbonizing transportation in the United States. This study investigates how the distribution of anatomical fractions (stem wood, bark, needles, branches) from pine forest residues of different ages impacts pyrolysis and hydrotreating processes, including product composition, carbon efficiency, economics, and overall sustainability. Commercially sourced 13- and 23-year-old loblolly pine residues were chosen to represent available resources; whole tree thinnings, and tops and branches from merchantable timber, respectively. Detailed characterization of the residue samples, product distributions, bio-oil, char, and gas characterization data are presented for 13 experiments, including the individual fractions, blends, and air-classified samples to reduce ash content. Pyrolysis mass balances averaged 97 +/- 3%. As expected, bio-oil yields were lower for the bark, needles, and blends with high proportions of these (53-56% dry basis), and highest for the debarked stem wood (67-71% dry basis). Lower yields were attributed to the high ash content of the needles, but also to the high lignin content in the bark (>50%), which is hypothesized to have led to increased char formation during pyrolysis. Higher-oil yield was generally correlated with total volatiles, hydrogen, oxygen, glucan, and mannan; somewhat correlated with xylan and acetyl content; and negatively correlated with total carbon, fixed carbon, nitrogen, sulfur, and extractives. Air classification of the residues was effective in reducing ash content (1.5% to 0.64%), extractives (~7% to 2%), and sulfur (0.04% to 0.02%), resulting in a small increase in yield, a significant increase in the GC-detectable proportion of oil (27% to 34%) and a net economic benefit. These experimental results were used to conduct technoeconomic and life cycle analyses, which are also summarized here.

biofuels↗

NASA NTRS1984

Fabrication of glass gas cells for the HALOE and MAPS satellite experiments

The Halogen Occultation Experiment (HALOE) and the Measurement of Air Pollution from Satellites (MAPS) experiment are satellite-borne experiments which measure trace constituents in the Earth's atmosphere. The instruments which obtain the data for these experiments are based on the gas filter correlation radiometer measurement technique. In this technique, small samples of the gases of interest are encapsulated in glass cylinders, called gas cells, which act as very selective optical filters. This report describes the techniques employed in the fabrication of the gas cells for the HALOE and MAPS instruments. Details of the method used to fuse the sapphire windows (required for IR transmission) to the glass cell bodies are presented along with detailed descriptions of the jigs and fixtures used during the assembly process. The techniques and equipment used for window inspection and for pairing the HALOE windows are discussed. Cell body materials and the steps involved in preparing the cell bodies for the glass-to-sapphire fusion process are given.

Sullivan, E. M.↗

NASA NTRS2006

The Evolution of the Cluster X-ray Scaling Relations in the Wide Angle ROSAT Pointed Survey Sample at 0.6 < z < 1.0

The X-ray properties of a sample of 11 high-redshift (0.6 < z < 1 .O) clusters observed with Chardm and/or XMM-Newton are used to investigate the evolution of the cluster scaling relations. The observed evolution in the normalization of the L-T, M-T, M(sub 2)-T and M-L relations is consistent with simple self-similar predictions, in which the properties of clusters reflect the properties of the Universe at their redshift of observation. Under the assumption that the model of self-similar evolution is correct and that the local systems formed via a single spherical collapse, the high-redshift L-T relation is consistent with the high-z clusters having virialized at a significantly higher redshift than the local systems. The data are also consistent with the more realistic scenario of clusters forming via the continuous accretion of material. The slope of the L-T relation at high redshift (B = 3.32 +/- 0.37) is consistent with the local relation, and significantly steeper than the self-similar prediction of B = 2. This suggests that the same non-gravitational processes are responsible for steepening the local and high-z relations, possibly occurring universally at z is approximately greater than 1 or in the early stages of the cluster formation, prior to their observation. The properties of the intracluster medium at high redshift are found to be similar to those in the local Universe. The mean surface-brightness profile slope for the sample is Beta = 0.66 +/- 0.05, the mean gas mass fractions within R(sub 2500(z)) and R(200(z)) are 0.069 +/- 0.012 and 0.11 +/- 0.02, respectively, and the mean metallicity of the sample is 0.28 +/- 0.11 Z(sub solar).

Maughan, B. J.↗

NASA NTRS2014

Nanophase Carbonates on Mars: Formation, Detection, and Implications

Despite having an atmosphere composed primarily of CO2 and evidence for abundant water in the past, carbonate minerals have only been discovered on Mars in small amounts in martian dust, in soils in the Northern Plains, and in outcrops of limited spatial extent. Recently, carbonates have been identified as the possible source of CO2 released during thermal analysis of material from an aeolian deposit named Rocknest and drilled sample from the sheepbed mudstone, both samples analyzed by the Mars Science Laboratory (MSL) in Gale Crater. Both the Phoenix lander and MSL carry thermal analysis instruments, the Thermal and Evolved Gas Analyzer (TEGA) on Phoenix and the Sample Analysis at Mars (SAM) instrument on MSL. While thermal analysis does not provide definitive mineralogy, it can detect volatile-bearing minerals present at very low abundance and the temperature profiles of evolved gases can reveal physical properties of the sample. For example, the decomposition temperature of volatilebearing minerals depends heavily on the particle size of the mineral.

Archer, P. D.↗

DOE OSTI2025

Diffusion kinetics of 3 He in pyroxene and plagioclase and applications to cosmogenic exposure dating and paleothermometry in mafic rocks

In this study, we investigate the diffusivity of cosmogenic 3 He in a variety of plagioclase and pyroxene compositions, and its application to paleothermometry and exposure dating in these minerals, through stepwise degassing experiments. While cosmogenic 3 He has been utilized for exposure dating in pyroxene for decades due to its retentivity, plagioclase, often found along with pyroxene in mafic rocks, is generally less retentive of cosmogenic noble gas. However, the diffusivity of 3 He in either plagioclase or pyroxene has not yet been measured quantitatively. A challenge in measuring diffusion kinetics by step-degassing experiments in poorly retentive minerals is the fact that significant amounts of He can be lost prior to the experiment. To address this issue, we apply a forward “multiple diffusion domain” (MDD) inversion model that includes model predictions of initial gas loss during irradiation and storage of the samples to account for this observation and add constraints to the diffusion parameters. We find that 3 He diffusivity in plagioclase appears to be highly variable. This variability can be explained by the MDD inversion models' inability to constrain the diffusion parameters when significant gas has been lost during irradiation and/or prolonged storage prior to experiment analysis, resulting in an overestimation of 3 He retentivity. Plagioclase samples that were kept frozen after irradiation, to limit this initial gas loss, yielded the most reliable estimate of diffusion kinetics. We find that 3 He in plagioclase is diffusively lost at Earth's surface temperatures on a timescale of 100 years and is therefore unsuitable for surface temperature paleothermometry. On the contrary, we find cosmogenic 3 He in pyroxene to be retentive at Earth's surface temperatures on a 1-million-year timescale.

Bergelin, Marie [Berkeley Geochronology Center (BG↗

NASA NTRS1976

Atmospheric rare gases in lunar rock 60015

Aliquots of lunar rock 60015 were subjected to various types of exposure and handling designed to produce terrestrial contamination, in order to test the possibility of a terrestrial origin for the terrestrial-like trapped Xe reported for lunar rock samples. Crushing the rock produced up to order-of-magnitude increases in the abundances of Ar, Kr, and Xe relative to the millimeter-sized chips of 60015 previously analyzed. Contrary to expectations for atmospheric contamination, high temperatures (above 1000 C) were necessary to remove about 75% of the trapped Kr and Xe, and the rare-gas elemental abundance ratios differed from those in terrestrial samples believed to have occluded atmospheric gases. It is concluded, on the basis of similar temperature-release profiles and elemental-fractionation patterns, that the trapped Xe observed in all these 60015 analyses is atmospheric contamination. Such a conclusion cannot unequivocally be drawn for other lunar rocks containing terrestrial-like Xe, but the present results demonstrate that arguments based on high extraction temperatures and elemental abundance ratios cannot be useful to rule out rare-gas atmospheric contamination in such samples.

Niemeyer, S.↗

NASA NTRS1982

Noble gas trapping by laboratory carbon condensates

Trapping of noble gases by carbon-rich matter was investigated by synthesizing carbon condensates in a noble gas atmosphere. Laser evaporation of a solid carbon target yielded submicron grains which proved to be efficient noble gas trappers (Xe distribution coefficients up to 13 cu cm STP/g-atm). The carbon condensates are better noble gas trappers than previously reported synthetic samples, except one, but coefficients inferred for meteoritic acid-residues are still orders of magnitude higher. The trapped noble gases are loosely bound and elementally strongly fractionated, but isotopic fractionations were not detected. Although this experiment does not simulate nebular conditions, the results support the evidence that carbon-rich phases in meteorites may be carriers of noble gases from early solar system reservoirs. The trapped elemental noble gas fractionations are remarkably similar to both those inferred for meteorites and those of planetary atmospheres for earth, Mars and Venus.

Niemeyer, S.↗

NASA NTRS1988

Formic and acetic acid over the central Amazon region, Brazil. I - Dry season

The concentrations of formic and acetic acids in the gas phase, atmospheric aerosol, and rainwater samples collected in Amazonia at ground level and in the atmosphere during the Amazon Boundary Layer Experiment in July/August 1985 were analyzed by ion exchange chromatography. The diurnal behavior of both acids at ground level and their vertical distribution in the forest canopy point to the existence of vegetative sources as well as to production by chemical reactions in the atmosphere. The concentrations of formic and acetic acids in the gas phase were about 2 orders of magnitude higher than the corresponding concentrations in the atmospheric aerosol. In rainwater, the total formate and acetate represented about one half of the anion equivalents, in contrast to less than 10 percent of the soluble anionic equivalents contributed by these acids in the atmospheric aerosol. The observed levels of these ions in rainwater are considered to be the result of a combination of chemical reactions in hydrometeors and the scavenging of the gaseous acids by cloud droplets.

Andreae, M. O.↗

NASA NTRS2009

Combustion of Organic Molecules by the Thermal Decomposition of Perchlorate Salts: Implications for Organics at the Mars Phoenix Scout Landing Site

The Mars 2007 Phoenix Scout Mission successfully landed on May 25, 2008 and operated on the northern plains of Mars for 150 sols. The primary mission objective was to study the history of water and evaluate the potential for past and present habitability in Martian arctic ice-rich soil [1]. Phoenix landed near 68 N latitude on polygonal terrain created by ice layers that are a few centimeters under loose soil materials. The Phoenix Mission is assessing the potential for habitability by searching for organic molecules in the ice or icy soils at the landing site. Organic molecules are necessary building blocks for life, although their presence in the ice or soil does not indicate life itself. Phoenix searched for organic molecules by heating soil/ice samples in the Thermal and Evolved-Gas Analyzer (TEGA, [2]). TEGA consists of 8 differential scanning calorimeter (DSC) ovens integrated with a magnetic-sector mass spectrometer with a mass range of 2-140 daltons [2]. Endothermic and exothermic reactions are recorded by the TEGA DSC as samples are heated from ambient to ~1000 C. Evolved gases, including any organic molecules and their fragments, are simultaneously measured by the mass spectrometer during heating. Phoenix TEGA data are still under analysis; however, no organic fragments have been identified to date in the evolved gas analysis (EGA). The MECA Wet Chemistry Lab (WCL) discovered a perchlorate salt in the Phoenix soils and a mass 32 peak evolved between 325 and 625 C for one surface sample dubbed Baby Bear [3]. The mass 32 peak is attributed to evolved O2 generated during the thermal decomposition of the perchlorate salt. Perchlorates are very strong oxidizers when heated, so it is possible that organic fragments evolved in the temperature range of 300-600 C were combusted by the O2 released during the thermal decomposition of the perchlorate salt. The byproduct of the combustion of organic molecules is CO2. There is a prominent release of CO2 between 200-600 C for several of the Phoenix soils analyzed by TEGA. This low temperature release of CO2 might be any combination of 1) desorption of adsorbed CO2, 2) thermal decomposition of Fe- and Mg-carbonates, and 3) combustion of organic molecules [2].

Ming, D.W.↗

NASA NTRS1982

Irradiation records of Acapulco and other small meteorites derived from Mn-53 and rare gas measurements

Attempts have been made recently to resolve the problem of depth and size dependences of the production rates of cosmogenic radionuclides within meteorites. The present investigation is concerned with Mn-53 and Al-25 measurements in samples of eight meteorite falls with small recovered masses. The recovered masses of the chondrites lie in the range from 0.35 to 8.4 kg, which corresponds to effective postatmospheric radii in the range from 2.9 to 8.3 cm. The He-3/Ne-21 ratios observed in these stones lie in the range from 6.33 to 8.62, and the Ne-22/Ne-21 ratios lie in the range from 1.132 to 1.248, thus generally indicating lightly shielded samples. The obtained results together with rare gas data are used as a basis for the discussion of the irradiation histories.

Englert, P.↗

NASA NTRS2001

SNC Meteorites, Organic Matter and a New Look at Viking

Recently, evidence has begun to grow supporting the possibility that the Viking GC-MS would not have detected certain carboxylate salts that could have been present as metastable oxidation products of high molecular weight organic species. Additionally, despite the instrument's high sensitivity, the possibility had remained that very low levels of organic matter, below the instrument's detection limit, could have been present. In fact, a recent study indicates that the degradation products of several million microorganisms per gram of soil on Mars would not have been detected by the Viking GC-MS. Since the strength of the GC-MS findings was considered enough to dismiss the biology packet, particularly the LR results, any subsequent evidence suggesting that organic molecules may in fact be present on the Martian surface necessitates a re-evaluation of the Viking LR data. In addition to an advanced mass spectrometer to look for isotopic signatures of biogenic processes, future lander missions will include the ability to detect methane produced by methanogenic bacteria, as well as techniques based on biotechnology. Meanwhile, the identification of Mars samples already present on Earth in the form of the SNC meteorites has provided us with the ability to study samples of the Martian upper crust a decade or more in advance of any planned sample return missions. While contamination issues are of serious concern, the presence of indigenous organic matter in the form of polycyclic aromatic hydrocarbons has been detected in the Martian meteorites ALH84001 and Nakhla, while there is circumstantial evidence for carbonaceous material in Chassigny. The radiochronological ages of these meteorites are 4.5 Ga, 1.3 Ga, and 165 Ma respectively representing a span of time in Earth history from the earliest single-celled organisms to the present day. Given this perspective on organic material, a biological interpretation to the Viking LR results can no longer be ruled out. In the LR experiment, a solution containing C-14 labeled organic compounds was injected into soil samples. The detection of radioactivity in the overhead space would indicate that one or more of the substrates had been chemically converted into a carbon-containing gas. To serve as a control, some samples were heated enough to destroy most known terrestrial microbes so that an indication for life would be a positive response from unheated samples and a negative response from heated samples. On Mars, the LR results had met minimum criteria for a biological interpretation but due to the GC-MS results, the LR responses were later attributed to putative soil inorganic oxidants. Since the time of Viking, studies have been carried out with the objective of determining an oxidant or combination of oxidants that might exist on Mars and have produced the observed kinetics of the LR response. To date, no such agent has been found that produces all aspects of the LR results on Mars. While the above considerations in no way imply the existence of life forms at the two Viking landing sites, inorganic and biological explanations for the Viking LR data should now be considered equally plausible until more complete studies of the Martian surface are carried out. Therefore, in light of the SNC meteorites data and their implications for the possibility of organic matter near or on the Martian surface the Viking biology experiments should thus be seen, not as failures for their inability to provide unambiguous evidence for or against Martian life, but as a foundation for the development of future life-detection instruments. Additional information is contained in the original extended abstract.

Warmflash, David M.↗

NASA NTRS1994

Noble gas isotopes and halogens in volatile-rich inclusions in diamonds

Application of the (40)Ar-(39)Ar method and noble gas studies to diamonds has increased our understanding of their age relationships to the host kimberlite or lamproite, and of the source and composition of volatile-rich fluids in the upper mantle. The properties of diamond (inert, high mechanical strength and low gas diffusivities) means they are especially useful samples for studying gases trapped deep within the earth (less than 150 km) as they are unlikely to have undergone loss or exchange of entrapped material since formation. Volatile-rich fluids (H2O-CO2) are important agents for metasomatic processes in the upper mantle, and the noble gases and halogens preferentially partition into this phase leading to a strong geochemical coherence between these groups of elements. The abundances of the halogens in the major reservoirs of the Earth shows a marked progression from chlorine, concentrated in the oceans, through to iodine which, through its affinity to organic material, is concentrated mainly in sediments. Abundances in the upper mantle are low. This is particularly true for iodine which is of special interest in view of its potential significance as an indicator of sediment recycling and by way of its link to (129)Xe amomalies in the mantle through the low extinct isotope (129)I. Extensions of the (40)Ar-(39)Ar technique enable measurements of halogens and other elements (K, Ca, Ba, U) by production of noble gas isotopes from these species during neutron irradiation. Samples analyzed in this way include 15 coated stones from an unknown source in Zaire, 3 boarts from the Jwaneng and 1 boart from the Orapa kimberlites, both in Botswana.

Burgess, Raymond↗

NASA NTRS2024

Investigating Bennu’s Volatile Accretion History Through Step-Heating N-Ne-Ar Analyses of Single Aggregate Particles

NASA’s OSIRIS-REx spacecraft delivered a sample from the carbonaceous asteroid (101955) Bennu to Earth on September 24, 2023. Since Bennu presumably accreted in the outer protoplanetary disk, beyond Jupiter’s orbit, the collected material is expected to be rich in highly volatile elements such as H, C, N, and noble gases—similar to Ivuna-type (CI) carbonaceous chondrites and material from asteroid (162173) Ryugu returned by JAXA’s Hayabusa2 spacecraft. This type of material may have contributed to the volatile inventory of Earth and the other terrestrial planets. Bulk CI chondrites record a narrow range of δ 15 N values (i.e., the permil difference from the atmospheric 15 N/ 14 N ratio), averaging between +42 and 49‰. In contrast, recent analyses at CRPG’s noble gas facility revealed that two pelletized Ryugu samples have lower δ 15 N values of +18.1 ± 0.9‰ and +19.5 ± 0.9‰. Together with the low measured N abundances, this observation suggests that Ryugu has lost a 15 N-rich, labile organic phase due to pervasive aqueous alteration. Subsequent high-resolution step-heating analyses of an additional Ryugu particle demonstrated that the δ 15 N value varies significantly during successive extraction steps (between +1.0 ± 1.0‰ and 65.8 ± 1.1‰); the variable N isotopic composition points to the presence of several isotopically distinct N-carrier phases in CI-type material. Here, we report preliminary N-Ne-Ar results obtained for individual particles from an aggregate Bennu sample using the Noblesse-HR (Nu Instruments) noble gas mass spectrometer at CRPG’s noble gas facility. In a companion abstract, we will present the noble gas (He, Ne, Ar, Kr, Xe) characteristics of other aggregate particles determined with a HELIX MC Plus. Whereas the abundance and isotopic composition of noble gases permit detection of various presolar phases and the so-called phase Q, as well as quantification of solar wind–derived and cosmogenic components, the abundance and isotopic composition of N are expected to provide further insights into the origin and evolution of N-bearing phases in carbonaceous asteroids.

E Füri↗

NASA NTRS1973

Argon in Apollo 15 green glass spherules /15426/ - Ar-40-Ar-39 age and trapped argon

The results of thermal-release argon analyses of neutron-irradiated green glass spherules separated from the lunar sample 15426 are discussed. It is shown that the gas-retention age determined by the Ar-40-Ar-39 method is similar to that of local mare basalts, and differs from the ages of Appenine Front samples recovered from the same region as 15426. Trapped argon is present in near-surface regions of the spherules, and can be resolved into at least two components requiring separate origins: a shallow (0.1 micron) component with Ar-40/Ar-39 not less than 30, and a deeper (2.0 micron) component with an Ar-40/Ar-39 ratio of 2.9. The ratio of trapped Ar-40 to Ar-36 is higher than in any lunar soil samples, and suggests that the trapped gas was implanted early in the spherules history.

Podosek, F. A.↗

NASA NTRS1990

Optical characterization of clouds of fine liquid-nitrogen particles

Characteristic drop size, D sub 32, of clouds of fine liquid nitrogen particles was measured with a scattered light scanning instrument developed at NASA-Lewis. Calibration of the instrument was accomplished with suspensions of monosized polystyrene spheres and the scattered light scanner was then used to investigate the mechanism of liquid nitrogen jet disintegration in high velocity gas flow. The Sauter mean diameter, D sub 32, was found to vary inversely with nitrogen gas mass-flux raised to the 1.33 power. Values of D sub 32 varied from 5 to 25 microns and the mass-flux exponent 1.33 agrees well with theory for liquid jet breakup in high velocity gas flow. Loss of fine particles due to the high vaporization rate of liquid nitrogen was avoided by sampling the spray 1.3 cm downstream of the nozzle orifice. The presence of high velocity and thermal gradients in the gas phase also made sampling of the particles quite difficult. As a result, it was necessary to correct the measurements for background noise produced by both highly turbulent gas flow and thermally induced density gradients in the gas phase.

Ingebo, Robert D.↗

DOE OSTI2023

Pore connectivity influences mass transport in natural rocks: Pore structure, gas diffusion and batch sorption studies

For this work, six rocks (one granodiorite, one limestone, two chalks, one mudstone, and one dolostone) with different extents of heterogeneity at six different particle sizes (from 75 to 8000 μm) were studied to describe the effects of pore connectivity on mass transport. The methods applied were (i) porosity measurement of granular rocks, (ii) analyses of gas-phase diffusive transport in a bed of packed particles, along with a solid quartz method at these six particle sizes being developed to identify the contribution of intraparticle diffusion, and (iii) batch sorption tests of multiple ions (anions and cations) with subsequent analyses of inductively coupled plasma-mass spectrometry. Granular porosity measurement results reveal that with decreasing particle sizes, the effective porosities for the “heterogenous” group of rocks (Grimsel granodiorite and Edwards limestone) increase, whereas the porosities of another “homogeneous” group (two Israel chalk samples, Japan mudstone, and Wyoming dolostone) remain constant. Gas diffusion results show that the intraparticle gas diffusion coefficient among these two sample groups, varying in the magnitude of 10 -8 to 10 -6 m 2 /s, are not directly correlated to the porosity differences. Moreover, the batch sorption work displays a different affinity of rocks for various tracers. For Grimsel granodiorite, Japan mudstone, and Wyoming dolostone, the adsorption capacity of Sm 3+ and Eu 3+ increases as the particle size decreases. In general, this integrated research of grain size distribution, granular rock porosity, intraparticle diffusivity, and ionic sorption capacity gives insights into the pore connectivity effect on both physical and chemical transport behaviors for different lithologies and/or different particle sizes.

58 GEOSCIENCES↗