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DOE OSTI2020

Interfacial solvation and slow transport of hydrated excess protons in non-ionic reverse micelles

This work employs molecular dynamics simulations to investigate the solvation and transport properties of hydrated excess protons (with a hydronium-like core structure) in non-ionic Igepal CO-520 reverse micelles of various sizes in a non-polar solvent. Multiscale Reactive Molecular Dynamics (MS-RMD) simulations were used to describe vehicular and hopping diffusion during the proton transport process. As detailed herein, an excess proton shows a marked tendency to localize in the interfacial region of micellar water pools. Slow proton transport was observed which becomes faster with increasing micellar size. Further analysis reveals that the slow diffusion of an excess proton is a combined result of slow water diffusion and the low proton hopping rate. This study also confirms that a low proton hopping rate in reverse micelles stems from the interfacial solvation of hydrated excess protons and the immobilization of interfacial water. The low water density in the interfacial region makes it difficult to form a complete hydrogen bond network near the hydrated excess proton, and therefore locks in the orientation of hydrated proton cations. The immobilization of the interfacial water also slows the relaxation of the overall hydrogen bond network.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

The shard test and nanoporomechanics reverse classical paradigm of cement hydration being contractive

Le Chatelier in 1887 and Powers in 1947 demonstrated that the volume of nanoscale C-S-H (calcium silicate hydrate) particles formed during hydration is smaller than the combined volume of the reactants—the anhydrous Portland cement and water. Hydration has thus been considered as contractive. An experiment shows that the opposite is true above the nanoscale. The porous skeleton of cement paste expands as the growing C-S-H particles push each other apart, similar to crystal growth pressure. This is significant for high-performance concretes (HPC) with low water-cement ratios (w/c ≤ 0.4), where chemical self-desiccation lowers pore relative humidity by 40%, compared to just 1% in traditional concretes (w/c ≈ 0.5). Standard American Society for Testing and Materials (ASTM) C1608 tests, using 10 mm thick water-immersed specimens, show large shrinkage because the half-time of water ingress is many decades, unable to offset shrinkage-causing self-desiccation. The present experiment, using a laser microscopy-topography technique, proves the opposite—expansion, evidenced by measuring the length changes of water-immersed HPC shards 0.5 mm thick in which the diffusion halftime, only about one hour, allows continuous resaturation of pores, canceling self-desiccation. The faster diffusion (halftime of one hour) enables continuous pore resaturation, preventing shrinkage. When sealed with paraffin oil, the shards self-desiccate and shrink. These findings align with studies since 2015, showing that models excluding hydration expansion cannot fit test data across various specimen sizes and sealing conditions. The results suggest that standardized ASTM tests for the so-called chemical shrinkage in modern concretes with very low water-cement ratios are misleading and need revision.

Science & Technology - Other Topics↗

DOE OSTI2021

Characterization of Oil Well Cement Performance during Early Hydration under Simulated Borehole Conditions

Summary Experiments on oil well cement (OWC) slurries were performed using the newly developed laboratory-scale wellbore simulation chamber (WSC). The WSC can simulate hydrostatic pressure reduction in the cemented annulus and possible gas migration under representative conditions. Forensic analysis shows that pressurized fluids can result in porous cement and gas channeling during cement slurry gelation. The effects of different factors on slurry pore pressure were also studied, including formation permeability, initial overburden pressure (OBP) representing the depth of interest, wellbore temperature, water/cement (w/c) ratio, cement composition, and the use of a calcium chloride (CaCl2)-based accelerator. By analyzing the temperature history of hydrating cement using degree of hydration, the evolution of cement hydration was characterized for slurry designs cured at different hydration rates. This provides the opportunity to parameterize the slurry designs and other important factors associated with wellbore conditions.

Engineering↗

NASA NTRS1983

Effect of hydration on nitrogen washout in human subjects

Five subjects were tested to assess the influence of drinking hypotonic water (distilled water) on whole body tissue nitrogen washout. During the test, the subjects breathed aviators' oxygen for three hours. Each subject performed two baseline nitrogen washouts in a two-week period. The third washout, in the third week, was done under a transient hydrated condition. This was accomplished by having the subjects drink 1.5 liters of hypotonic water 30 minutes before the washout. Five-minute plots of tissue nitrogen removal from the three separate washouts were analyzed to ascertain if the hydration technique had any effect. Our results clearly indicate that the hydration technique did not alter the tissue nitrogen washout characteristics to any degree over three hours. An increase in tissue nitrogen washout under a transient hydrated condition using hypotonic fluid was not demonstrated to be the mechanism responsible for the reported benefit of this technique in preventing Type I altitude decompression pain in man.

Waligora, J.↗

NASA NTRS1985

Use of Hydration Inhibitors to Improve Bond Durability of Aluminum Adhesive Joints

An investigation is conducted of the mechanisms by which nitrilotris methylene phosphonic acid (NTMP) and related compounds are adsorbed onto oxidized aluminum surfaces to inhibit hydration and increase the durability of adhesive bonds formed with inhibitor-treated panels. P - O - Al bonds are identified as the basis of adsorption, and it is found that water initially adsorbed onto the etched aluminum surfaces is displaced by the NTMP. The hydration of the NTMP-treated surfaces occurs in three stages, namely the reverisble physisorption of water, the slow dissolution of NTMP followed by rapid hydration of the freshly exposed Al2O3 to AlOOH and further hydration of the surface to Al(OH)3. Five properties of an ideal inhibitor are identified.

Davis, G. D.↗

NASA NTRS1995

Phase equilibria of H2SO4, HNO3, and HCl hydrates and the composition of polar stratospheric clouds

Thermodynamic properties and phase equilibria behavior for the hydrates and coexisting pairs of hydrates of common acids which exist in the stratosphere are assembled from new laboratory measurements and standard literature data. The analysis focuses upon solid-vapor and solid-solid-vapor equilibria at temperatures around 200 K and includes new calorimetric and vapor pressure data. Calculated partial pressures versus 1/T slopes for the hydrates and coexisting hydrates agree well with experimental data where available.

Wooldridge, Paul J.↗

NASA NTRS1994

A cheaper, faster, better way to detect water of hydration on Solar System bodies

The 3.0-micrometers water of hydration absorption feature observed in the IR photometry of many low-albedo and some medium-albedo asteroids strongly correlates with the 0.7-micrometers Fe(+2) to Fe(+3) oxidized iron absorption feature observed in narrowband spectrophotometry of these asteroids. Using this relationship, an empirical algorithm for predicting the presence of water of hydration in the surface material of a Solar System body using photometry obtained through the Eight-Color Asteroid Survey nu (0.550 micrometers), w (0.701 micrometers), and x (0.853 micrometers) filters was developed and applied to the ECAS photometry of asteroids and outer planet satellites. The percentage of objects in low-albedo, outer main-belt asteroid classes that test positively for water of hydration increases from P to B to C to G class and correlates linearly with the increasing mean albedos of those objects testing positively. The medium-albedo M-class asteroids do not test positively in large number using this algorithm. Aqueously altered asteroids dominate the Solar System population between heliocentric distances of 2.6 to 3.5 AU, bracketing the Solar System region where the aqueous alteration mechanism operated most strongly. One jovian satellite, J VI Himalia, and one saturnian satellite. Phoebe, tested positively for water of hydration, supporting the hypothesis that these may be captured C-class asteroids from a postaccretional dispersion. The proposed testing technique could be applied to an Earth-based survey of asteroids or a space-probe study of an asteroid's surface characteristic in order to identify a potential water source.

Vilas, Faith↗

NASA NTRS1995

Phase Equilibria of H2SO4, HNO3, and HCl Hydrates and the Composition of Polar Stratospheric Clouds

Wooldridge, Paul J.↗

NASA NTRS2002

Hydrated Minerals on Asteroids: The Astronomical Record

Knowledge of the hydrated mineral inventory on the asteroids is important for deducing the origin of Earth's water, interpreting the meteorite record, and unraveling the processes occurring during the earliest times in solar system history. Reflectance spectroscopy shows absorption features in both the 0.6-0.8 and 2.5-3.5 micrometers regions, which are diagnostic of or associated with hydrated minerals. Observations in those regions show that hydrated minerals are common in the mid-asteroid belt, and can be found in unexpected spectral groupings, as well. Asteroid groups formerly associated with mineralogies assumed to have high temperature formation, such as M- and E-class asteroids, have been observed to have hydration features in their reflectance spectra. Some asteroids have apparently been heated to several hundred degrees Celsius, enough to destroy some fraction of their phyllosilicates. Others have rotational variation suggesting that heating was uneven. We summarize this work, and present the astronomical evidence for water- and hydroxyl-bearing minerals on asteroids.

Rivkin, A. S.↗

NASA NTRS2003

Hydrated Minerals on Asteroids: The Astronomical Record

Knowledge of the hydrated mineral inventory on the asteroids is important for deducing the origin of Earth's water, interpreting the meteorite record, and unraveling the processes occurring during the earliest times in solar system history. Reflectance spectroscopy shows absorption features in both the 0.6-0.8 and 2.5-3.5-micron regions, which are diagnostic of or associated with hydrated minerals. Observations in those regions show that hydrated minerals are common in the mid-asteroid belt, and can be found in unexpected spectral groupings as well. Asteroid groups formerly associated with mineralogies assumed to have high-temperature formation, such as M- and E-class steroids, have been observed to have hydration features in their reflectance spectra. Some asteroids have apparently been heated to several hundred degrees Celsius, enough to destroy some fraction of their phyllosilicates. Others have rotational variation suggesting that heating was uneven. We summarize this work, and present the astronomical evidence for water- and Hydroxl-bearing minerals on asteroids.

Rivkin, A. S.↗

NASA NTRS2003

Detecting Near-Surface Water and Hydrate Minerals on Mars from a Rover, Penetrator, or Borehole: The HYDRA Instrument

One of the major goals of near term NASA Mars exploration is to identify exact locations of near-surface water or hydrated minerals on Mars. Evidence for the existence of recent nearsurface water on Mars underscores the need for developing instrumentation that can identify water or hydrated minerals very near the surface. Further encouraging evidence of surface and near-surface water and hydrate minerals on Mars comes from neutron spectrometer measurements aboard Mars Odyssey. Preliminary results show very large regions of high hydrogen content poleward of 60 deg. latitude, as well as interesting features closer to the equator. However, spatial resolution from orbit is very poor, approx. 400 km. The next logical step is to use in-situ or near-surface investigations to map in detail some of the most interesting features. Relatively simple instrumentation based on He-3 gas proportional counters were shown to be highly successful on the Lunar Prospector mission in identifying even low levels of enhanced hydrogen abundances. Here we discuss HYDRA, a water- and hydrate-sensing instrument currently being developed under the NASA Mars Instrument Development Program (MIDP). HYDRA is based on Lunar Prospector technology, and is intended as a rover body-mounted instrument, or an instrument on an aerobot, penetrator, hard lander on the surface of Mars, or for borehole stratigraphy applications. Our proposed instrument would be ideal for such platforms as it would be small (less than 7 cm diameter by 10 cm long), low mass (less than 500 g), low power (less than 1W), and have a low data volume per measurement. We use neutron spectrometry (a) because of its proven ability to uniquely detect and quantify hydrogen abundance, and (b) because the resources required by this approach (weight, power, size, telemetry bandwidth, and measurement time) are extremely low. This compact neutron spectrometer package, comprised of two small He-3 gas proportional counters, offers superior sensitivity, extensive flight heritage, and inherent ruggedness. These tubes have survived approx. 1500 g's of acceleration in penetrator tests. In a landed application, HYDRA would help address many topics of interest to the Mars Exploration and Astrobiology communities: (a) nature and origin of stratified deposits; (b) water cycle(s) and temporal changes; (c) early water oceans, aquifers, precipitation; (d) current extent/location/state of water; (e) polar cap processes and temporal changes; (f) where extremeophiles could survive on Mars; (g) paleoclimate surface signatures and modeling; (h) strategies for future Mars exploration.

R C Elphic↗

NASA NTRS2004

Gas Hydrate Stability at Low Temperatures and High Pressures with Applications to Mars and Europa

Gas hydrates are implicated in the geochemical evolution of both Mars and Europa [1- 3]. Most models developed for gas hydrate chemistry are based on the statistical thermodynamic model of van der Waals and Platteeuw [4] with subsequent modifications [5-8]. None of these models are, however, state-of-the-art with respect to gas hydrate/electrolyte interactions, which is particularly important for planetary applications where solution chemistry may be very different from terrestrial seawater. The objectives of this work were to add gas (carbon dioxide and methane) hydrate chemistries into an electrolyte model parameterized for low temperatures and high pressures (the FREZCHEM model) and use the model to examine controls on gas hydrate chemistries for Mars and Europa.

Marion, G. M.↗

NASA NTRS1998

Centrosome structure and function is altered by chloral hydrate and diazepam during the first reproductive cell cycles in sea urchin eggs

This paper explores the mode of action of the tranquillizers chloral hydrate and diazepam during fertilization and mitosis of the first reproductive cell cycles in sea urchin eggs. Most striking effects of these drugs are the alteration of centrosomal material and the abnormal microtubule configurations during exposure and after recovery from the drugs. This finding is utilized to study the mechanisms of centrosome compaction and decompaction and the dynamic configurational changes of centrosomal material and its interactions with microtubules. When 0.1% chloral hydrate or 350-750 microM diazepam is applied at specific phases during the first cell cycle of sea urchin eggs, expanded centrosomal material compacts at distinct regions and super-compacts into dense spheres while microtubules disassemble. When eggs are treated before pronuclear fusion, centrosomal material aggregates around each of the two pronuclei while microtubules disappear. Upon recovery, atypical asters oftentimes with multiple foci are formed from centrosomal material surrounding the pronuclei which indicates that the drugs have affected centrosomal material and prevent it from functioning normally. Electron microscopy and immunofluorescence studies with antibodies that routinely stain centrosomes in sea urchin eggs (4D2; and Ah-6) depict centrosomal material that is altered when compared to control cells. This centrosomal material is not able to reform normal microtubule patterns upon recovery but will form multiple asters around the two pronuclei. When cells are treated with 0.1% chloral hydrate or 350-750 microM diazepam during mitosis, the bipolar centrosomal material becomes compacted and aggregates into multiple dense spheres while spindle and polar microtubules disassemble. With increased incubation time, the smaller dense centrosome particles aggregate into bigger and fewer spheres. Upon recovery, unusual irregular microtubule configurations are formed from centrosomes that have lost their ability to reform normal mitotic figures. These results indicate that chloral hydrate and diazepam affect centrosome structure which results in the inability to reform normal microtubule formations and causes abnormal fertilization and mitosis.

Non-NASA Center↗

NASA NTRS2007

Methane Hydrates: More Than a Viable Aviation Fuel Feedstock Option

Demand for hydrocarbon fuels is steadily increasing, and greenhouse gas emissions continue to rise unabated with the energy demand. Alternate fuels will be coming on line to meet that demand. This report examines the recovering of methane from methane hydrates for fuel to meet this demand rather than permitting its natural release into the environment, which will be detrimental to the planet. Some background on the nature, vast sizes, and stability of sedimentary and permafrost formations of hydrates are discussed. A few examples of the severe problems associated with methane recovery from these hydrates are presented along with the potential impact on the environment and coastal waters. Future availability of methane from hydrates may become an attractive option for aviation fueling, and so future aircraft design associated with methane fueling is considered.

Hendricks, Robert C.↗

NASA NTRS2008

Bonding by Hydroxide-Catalyzed Hydration and Dehydration

A simple, inexpensive method for bonding solid objects exploits hydroxide-catalyzed hydration and dehydration to form silicate-like networks in thin surface and interfacial layers between the objects. The method can be practiced at room temperature or over a wide range of temperatures. The method was developed especially to enable the formation of precise, reliable bonds between precise optical components. The bonds thus formed exhibit the precision and transparency of bonds formed by the conventional optical-contact method and the strength and reliability of high-temperature frit bonds. The method also lends itself to numerous non-optical applications in which there are requirements for precise bonds and/or requirements for bonds, whether precise or imprecise, that can reliably withstand severe environmental conditions. Categories of such non-optical applications include forming composite materials, coating substrates, forming laminate structures, and preparing objects of defined geometry and composition. The method is applicable to materials that either (1) can form silicate-like networks in the sense that they have silicate-like molecular structures that are extensible into silicate-like networks or (2) can be chemically linked to silicate-like networks by means of hydroxide-catalyzed hydration and dehydration. When hydrated, a material of either type features surface hydroxyl (-OH) groups. In this method, a silicate-like network that bonds two substrates can be formed either by a bonding material alone or by the bonding material together with material from either or both of the substrates. Typically, an aqueous hydroxide bonding solution is dispensed and allowed to flow between the mating surfaces by capillary action. If the surface figures of the substrates do not match precisely, bonding could be improved by including a filling material in the bonding solution. Preferably, the filling material should include at least one ingredient that can be hydrated to have exposed hydroxyl groups and that can be chemically linked, by hydroxide catalysis, to a silicate-like network. The silicate-like network could be generated in situ from the filling material and/or substrate material, or could be originally present in the bonding material.

Gwo, Dz-Hung↗

NASA NTRS2004

Permanent Sequestration of Emitted Gases in the Form of Clathrate Hydrates

Underground sequestration has been proposed as a novel method of permanent disposal of harmful gases emitted into the atmosphere as a result of human activity. The method was conceived primarily for disposal of carbon dioxide (CO2, greenhouse gas causing global warming), but could also be applied to CO, H2S, NOx, and chorofluorocarbons (CFCs, which are super greenhouse gases). The method is based on the fact that clathrate hydrates (e.g., CO2 6H2O) form naturally from the substances in question (e.g., CO2) and liquid water in the pores of sub-permafrost rocks at stabilizing pressures and temperatures. The proposed method would be volumetrically efficient: In the case of CO2, each volume of hydrate can contain as much as 184 volumes of gas. Temperature and pressure conditions that favor the formation of stable clathrate hydrates exist in depleted oil reservoirs that lie under permafrost. For example, CO2-6H2O forms naturally at a temperature of 0 C and pressure of 1.22 MPa. Using this measurement, it has been calculated that the minimum thickness of continuous permafrost needed to stabilize CO2 clathrate hydrate is only about 100 m, and the base of the permafrost is known to be considerably deeper at certain locations (e.g., about 600 m at Prudhoe Bay in Alaska). In this disposal method, the permafrost layers over the reservoirs would act as impermeable lids that would prevent dissociation of the clathrates and diffusion of the evolved gases up through pores.

Duxbury, N.↗

NASA NTRS2012

Thermal Regeneration of Sulfuric Acid Hydrates after Irradiation

In an attempt to more completely understand the surface chemistry of the jovian icy satellites, we have investigated the effect of heating on two irradiated crystalline sulfuric acid hydrates, H2SO4 4H2O and H2SO4 H2O. At temperatures relevant to Europa and the warmer jovian satellites, post-irradiation heating recrystallized the amorphized samples and increased the intensities of the remaining hydrate's infrared absorptions. This thermal regeneration of the original hydrates was nearly 100% efficient, indicating that over geological times, thermally-induced phase transitions enhanced by temperature fluctuations will reform a large fraction of crystalline hydrated sulfuric acid that is destroyed by radiation processing. The work described is the first demonstration of the competition between radiation-induced amorphization and thermally-induced recrystallization in icy ionic solids relevant to the outer Solar System.

Loeffler, Mark J.↗

NASA NTRS2019

Experimental Investigation of Cement Hydration in Gravity-Free Environment

In this work, cement hydration in terrestrial and microgravity environment was compared. This was for the first time, when the International Space Station was utilized to fully investigate the complex process of cement solidification. Microstructural development of hydrating cement occurs in stages during the hydration reaction and hardening process, which results in elaborate combinations of amorphous and crystalline phases. The morphology, volume fraction, and distribution of these phases ultimately determine the hardened cement’s material properties. Minimizing gravity-driven phenomena, such as thermosolutal convective flow and sedimentation ensures crystal growth strictly by diffusion and a microstructure forms differently from that observed in typical laboratory conditions on Earth. A test matrix was developed that includes samples with various w/c ratio and various compositions; incorporating alite, pure water and cement system, cement with chemical admixtures, as well as commercial products. This paper reports on main changes initially observed in the microstructural development of hydrated pure compound of tricalcium silicate (C3S).

Neves, Juliana↗