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NASA NTRS2009

Trace Contaminant Testing with the Orion Atmosphere Revitalization Technology

Every spacecraft atmosphere contains trace contaminants resulting from offgassing by cabin materials and human passengers. An amine-based carbon dioxide (CO2) and water vapor sorbent in pressure-swing regenerable beds has been developed by Hamilton Sundstrand and baselined for the Orion Atmosphere Revitalization System (ARS). Part of the risk mitigation effort for this new technology is the study of how atmospheric trace contaminants will affect and be affected by the technology. One particular area of concern is ammonia, which, in addition to the normal spacecraft sources, can also be off-gassed by the amine-based sorbent. In the first half of 2009, tests were performed with typical cabin atmosphere levels of five of the most common trace gases, most of which had not yet been tested with this technology. A subscale sample of the sorbent was exposed to each of the chemicals mixed into a stream of moist, CO2-laden air, and the CO2 adsorption capacity of the sorbent was compared before and after the exposure. After these typical-concentration chemicals were proven to have negligible effect on the subscale sample, tests proceeded on a full-scale test article in a sealed chamber with a suite of eleven contaminants. To isolate the effects of various test rig components, several extended-duration tests were run: without injection or scrubbing, with injection and without scrubbing, with injection and scrubbing by both the test article and dedicated trace contaminant filters, and with injection and scrubbing by only the test article. The high-level results of both the subscale and full-scale tests are examined in this paper.

Button, Amy Lin↗

NASA NTRS2010

Trace Contaminant Testing with the Orion Atmosphere Revitalization Technology

Every spacecraft atmosphere contains trace contaminants resulting from offgassing by cabin materials and human passengers. An amine-based carbon dioxide (CO2) and water vapor sorbent in pressure-swing regenerable beds has been developed by Hamilton Sundstrand and baselined for the Orion Atmosphere Revitalization System (ARS). Part of the risk mitigation effort for this new technology is the study of how atmospheric trace contaminants will affect and be affected by the technology. One particular area of concern is ammonia, which, in addition to the normal spacecraft sources, can also be offgassed by the amine-based sorbent. In the spring of 2009, tests were performed at Johnson Space Center (JSC) with typical cabin atmosphere levels of five of the most common trace gases, most of which had not yet been tested with this technology. A subscale sample of the sorbent was exposed to each of the chemicals mixed into a stream of moist, CO2-laden air, and the CO2 adsorption capacity of the sorbent was compared before and after the exposure. After these typical-concentration chemicals were proven to have negligible effect on the subscale sample, tests proceeded on a full-scale test article in a sealed chamber with a suite of eleven contaminants. To isolate the effects of various test rig components, several extended-duration tests were run: without injection or scrubbing, with injection and without scrubbing, with injection of both contaminants and metabolic CO2 and water vapor loads and scrubbing by both the test article and dedicated trace contaminant filters, and with the same injections and scrubbing by only the test article. The high-level results of both the subscale and full-scale tests are examined in this paper.

Button, Amy B.↗

NASA NTRS2015

Coming of Age: Polarization as a Probe of Plant Canopy Water Status

We tested the hypothesis that the relative water content (RWC) of the sunlit leaves in a plant canopy may be estimated from polarized canopy imagery. Recently (IGARSS, July 27-31, 2015, Milan, Italy), we reported the results of laboratory polarization measurements of single detached leaves during dry down. We found that RWC was linearly related to the ratio of the reflectance of the interior of the leaf and the leaf transmittance. Here we report application of the laboratory results to estimate RWC for sunlit leaves in a plant canopy. Using a commercial-off-the-shelf (COTS) Nikon 810 camera with Nikkor 300 mm lens and Polaroid type HN-22 linear polarizer, we photographed in the principle plane a plant canopy displaying a gradient of water stress and collected, at each of multiple points along the gradient, two images, one with the polarization filter oriented for maximum scene response and a second with the filter oriented for minimum scene response. We converted the digital values in the two images to reflectance factor with reference to images of a white, flat, horizontal Spectralon surface. We classified the polarization imagery, identifying reflecting leaves, transmitting leaves, other sunlit vegetation and shadows. For each image pair we normalized the leaf internal reflectance by dividing by the cosine of the angle of incidence of the sunlight on the leaf, selected the leaf maximum transmittance in the scene and divided to obtain the ratio reflectance/transmittance, which we compared with leaf RWC. We determined the leaf relative water content by harvesting a section of leaf and immediately placing it in a sealed container in an ice chest. Later in the laboratory the leaf sample was weighed, rehydrated, weighed, dried and again weighed. RWC was determined using the standard formula. Our experimental results support our hypothesis, suggesting that the RWC of sunlit leaves in a plant canopy may be estimated from analysis of polarization imagery collected by a COTS camera system. Unlike remotely sensed estimates of canopy equivalent water thickness, our estimates of the RWC of sunlit canopy leaves provide leaf physiological information. We propose RWC estimates based upon sunlit leaves are more relevant to assessing the water status of a plant canopy than would be RWC estimates based upon large FOV canopy measurements.

estimates↗

NASA NTRS2016

First Detection of Non-Chlorinated Organic Molecules Indigenous to a Martian Sample

The Sample Analysis at Mars (SAM) instrument onboard Curiosity can perform pyrolysis of martian solid samples, and analyze the volatiles by direct mass spectrometry in evolved gas analysis (EGA) mode, or separate the components in the GCMS mode (coupling the gas chromatograph and the mass spectrometer instruments). In addition, SAM has a wet chemistry laboratory designed for the extraction and identification of complex and refractory organic molecules in the solid samples. The chemical derivatization agent used, N-methyl-N-tert-butyldimethylsilyl- trifluoroacetamide (MTBSTFA), was sealed inside seven Inconel metal cups present in SAM. Although none of these foil-capped derivatization cups have been punctured on Mars for a full wet chemistry experiment, an MTBSTFA leak was detected and the resultant MTBSTFA vapor inside the instrument has been used for a multi-sol MTBSTFA derivatization (MD) procedure instead of direct exposure to MTBSTFA liquid by dropping a solid sample directly into a punctured wet chemistry cup. Pyr-EGA, Pyr-GCMS and Der-GCMS experiments each led to the detection and identification of a variety of organic molecules in diverse formations of Gale Crater.

Freissinet, C.↗

DOE OSTI2020

In Situ Chemical Monitoring and Imaging of Contents within Microfluidic Devices Having a Porous Membrane Wall Using Liquid Microjunction Surface Sampling Probe Mass Spectrometry

The ability to observe dynamic chemical processes (e.g., signaling, transport, etc.) in vivo or in situ using nondestructive chemical imaging opens a new door to understanding the complex dynamics of developing biological systems. With the advent of “biology-on-a-chip” devices has come the ability to monitor dynamic chemical processes in a controlled environment, using these engineered habitats to capture key features of natural systems while allowing visual observation of system development. Having the capability to spatially and temporally map the chemical signals within these devices may yield new insights into the forces that drive biosystem development. Here, a porous membrane sealed microfluidic device was designed to allow normal microfluidic operation while enabling continuous, location specific sampling and chemical characterization by liquid microjunction surface sampling probe mass spectrometry (LMJ-SSP MS). LMJ-SSP was used to extract fluids with nL-to-μL/min flow rates directly from selected areas of the microfluidic device without negatively impacting the device function. These extracts were subsequently characterized using MS. This technique was used to acquire MS images of the entirety of several multi-input microfluidic devices having different degrees of fluid mixing. LMJ-SSP MS imaging visualized the spatial distribution of chemical components within the microfluidic channels and could visualize chemical reactions occurring in the device. These microfluidic devices with a porous membrane wall are wholly compatible with the construction of biology-on-a-chip devices. This ultimately would enable correlation of biosystem physical structure with an evolving chemical environment

47 OTHER INSTRUMENTATION↗

NASA NTRS1979

Multiple-sample holder for IC testing

Carrousel tray speeds up testing process by feeding mass spectrometer up to 12 sealed integrated circuit packages in rapid succession for analysis of contaminants and total gas composition.

Haack, R. F.↗

NASA NTRS2021

Sample Return Containerization and Planetary Protection Using Brazing for Breaking the Chain of Contact to Mars

Planetary protection of Mars samples returned to Earth in a future NASA mission is a critical part of preventing uncontrolled biological materials being released from the samples. The planetary protection process requires addressing the potential risks and would involve “breaking the chain of contact (BTC)”, where any returned material reaching Earth for further analysis would have to be sealed inside a container with extremely high confidence. The sterilization process would require destroying any potential biological materials that may contaminate the external surface of the container. A novel process for containing the returned samples has been conceived and developed at JPL. The process consists of using induction heated brazing to synchronously sterilize, separate, seam and seal the container. In this case. the braze material is heated to the level of melting at temperatures higher than 500°C to assure sterilizing exposed areas since carbon bonds are broken above this temperature. The container that encloses the samples consists of double walls with interstitial space that is Earth-clean. The process consists of two-steps, where one was intended to be prepared on Earth and the second potentially executed on orbit around Mars. The latest results of this study that established the needed capability are described and discussed in this manuscript.

Shirajian, Nareg↗

DOE OSTI2022

Self-contained, automated, long-term sensor system for monitoring of soil and water nutrients in fields

An automated, fieldable ion-selective sensor system for frequent detection of nutrients in soils or water is set forth. In one aspect, an integrated small form-factor housing includes a battery, processor, a fluid manipulation unit and reservoirs, and a chemical species detection cell. A flow-through sampling head can be connected to the detection cell and a waste reservoir by flexible tubing sealingly connected at opposite ends of the tube. In one aspect, improved performance of the ion-selective sensor includes adding an ion-to-electron transfer interlayer between an ion-selective membrane and its working electrode. In one aspect, the sensor is solid-state and uses printed polymeric composite of POT-MoS$_{2}$. The use of a porous tube for a sampling head and fluid connection at opposite ends allows not only fluid to be removed from the head to the detection cell for measurement but also flow in an opposite direction and out to a waste reservoir to clean and reset for a next sample measurement.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2020

COMBLE-ISLAS water isotopes in precipitation (COMBLEISLASISO)

During the measurement period, precipitation was sampled on daily to sub-daily basis with a sampling kit consiting of a clear plastic box (60x40x40 cm) mounted to a ground structure. Daily sampling lasted from 22 Feb to 24 Mar 2020. At a fixed time of day (10 UTC), samples were collected and the sampling box cleaned for the next sample. Additionally, during intense observations periods (IOPs) announced by ISLAS, ARMS scientists increased sampling frequency to sub-daily sampling. During the campaign period, 2 IOPs were conducted, with in total 12 samples taken. IOP1 lasted from 27 Feb 10 to 02 Mar 2020, and IOP2 lasted from 12 Mar to 14 Mar 2020. Solid precipitation in the box was then melted, transferred to an 8 ml glass vial, sealed and shipped to FARLAB (University of Bergen, Norway) for stable water isotope analysis. Measured stable isotope composition of precipitation samples will be related to conditions at other sampling locations, and at the evaporation site to inform about conservation of water isotope quantities. In the period from 22 Feb to 24 Mar, 23 daily samples were collected at 10 UTC for stable water isotope analysis. During the entire sampling period, a high variability of precipitation phase was encountered. Most samples were recovered in the form of graupel/snow (12 samples), as rain (7 samples), and the remaining samples fell as graupel, snow, rain or frozen rain. Precipitation amounts varied between <1 mm (26 Feb) and 140 mm (25 Feb) within the sampling box. Furthermore, higher-resolution sampling was conducted during 2 intense observation periods (IOPs). During IOP1, lasting from 27 Feb 10 UTC to 02 Mar 10 UTC, 7 samples were collected, all of them as solid phase precipitation. IOP2 lasted from 12 Mar 10 UTC to 14 Mar 09 UTC, and 5 samples (all as graupel/snow) were collected. Samples were processed according to FARLAB standard measurement procedures. In short, samples were transferred to 1.5 ml glass vials with rubber/PTFE septa (part #548-0907, VWR, USA). An autosampler (A0325, Picarro Inc) transferred ca. 2µl per injection into a high-precision vapourizer (A0211, Picarro Inc, USA) heated to 110°C. After blending with dry N2 (< 5 ppm H2O) the gas mixture was directed into the measurement cavity of a Cavity-Ring Down Spectrometer (L2140-i, Picarro Inc) for about 7 min with a typical water concentration of 20 000 ppm. Memory effects were reduced by two times measuring a vapour mixture at a mixing ratio of 50 000 ppm, obtained from 2 injections of 2 µl for 5 min at the beginning of each new sample vial. Thereafter, another 6 injections of 2 µl per sample were measured individually as described above, and averages of the last 5 injections were used for further processing. Three standards were measured at the beginning and end of each batch, including a drift standard DI2 (δD: -50.72±0.73 permil, δ18O: -7.63±0.10 permil), and for calibration the laboratory standards GLW (δD: -307.79±0.75 permil, δ18O: -40.02±0.07 permil) and EVAP2 (δD: 9.52±0.65 permil, δ18O: 1.81±0.13 permil). A detailed calibration report is included with the final uploaded data set.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS1989

Method of preparing radially homogeneous mercury cadmium telluride crystals

Hg(1-x)Cd(x)Te is prepared in an improved directional solidification method in which a precast alloy sample containing predetermined amounts of Hg, Cd, and Te is disposed in a sealed ampule and a furnace providing two controlled temperature zones is translated upward past the ampule to provide melting and resolidification. The present improvement is directed to maintaining the zones at temperatures determined in accordance with a prescribed formula providing a thermal barrier between the zones with a maximum thickness and translating the furnace past the zones at a rate less the 0.31 micron/sec.

Lehoczky, Sandor L.↗

NASA NTRS1994

Light Weight Ceramic Ablators for Mars Follow-on Mission Vehicle Thermal Protection System

New Light Weight Ceramic Ablators (LCA) were produced by using ceramic and carbon fibrous substrates, impregnated with silicone and phenolic resins. The special infiltration techniques (patent pending) were developed to control the amount of organic resins in the highly porous fiber matrices so that the final densities of LCA's range from 0.22 to 0.24 g/cc. This paper presents the thermal and ablative performance of the Silicone Impregnated Reusable Ceramic Ablators (SIRCA) in simulated entry conditions for Mars-Pathfinder in the Ames 60 MW Interaction Heating Facility (I HF). Arc jet test results yielded no evidence of char erosion and mass loss at high stagnation pressures to 0.25 atm. Minimal silica melt was detected on surface char at a stagnation pressure of 0.31 atm. Four ceramic substrates were used in the production of SIRCA's to obtain the effective of boron oxide present in substrate so the thermal performance of SIRCA's. A sample of SIRCA was also exposed to the same heating condition for five cycles and no significant mass loss or recession was observed. Tensile testing established that the SIRCA tensile strength is about a factor of two higher than that of the virgin substrates. Thermogravimetric Analysis (TGA) of the char in nitrogen and air showed no evidence of free carbon in the char. Scanning Electron Microscopy of the post test sample showed that the char surface consists of a fibrous structure that was sealed with a thin layer of silicon oxide melt.

Tran, Huy K.↗

DOE OSTI2021

Integrated sample-handling and mounting system for fixed-target serial synchrotron crystallography

Serial synchrotron crystallography (SSX) is enabling the efficient use of small crystals for structure–function studies of biomolecules and for drug discovery. An integrated SSX system has been developed comprising ultralow background-scatter sample holders suitable for room and cryogenic temperature crystallographic data collection, a sample-loading station and a humid `gloveless' glovebox. The sample holders incorporate thin-film supports with a variety of designs optimized for different crystal-loading challenges. These holders facilitate the dispersion of crystals and the removal of excess liquid, can be cooled at extremely high rates, generate little background scatter, allow data collection over >90° of oscillation without obstruction or the risk of generating saturating Bragg peaks, are compatible with existing infrastructure for high-throughput cryocrystallography and are reusable. The sample-loading station allows sample preparation and loading onto the support film, the application of time-varying suction for optimal removal of excess liquid, crystal repositioning and cryoprotection, and the application of sealing films for room-temperature data collection, all in a controlled-humidity environment. The humid glovebox allows microscope observation of the sample-loading station and crystallization trays while maintaining near-saturating humidities that further minimize the risks of sample dehydration and damage, and maximize working times. This integrated system addresses common problems in obtaining properly dispersed, properly hydrated and isomorphous microcrystals for fixed-orientation and oscillation data collection. Its ease of use, flexibility and optimized performance make it attractive not just for SSX but also for single-crystal and few-crystal data collection. Fundamental concepts that are important in achieving desired crystal distributions on a sample holder via time-varying suction-induced liquid flows are also discussed.

47 OTHER INSTRUMENTATION↗

NASA NTRS2013

Fluorocarbon Contamination from the Drill on the Mars Science Laboratory: Potential Science Impact on Detecting Martian Organics by Sample Analysis at Mars (SAM)

Polytetrafluoroethylene (PTFE or trade name: Teflon by Dupont Co.) has been detected in rocks drilled during terrestrial testing of the Mars Science Laboratory (MSL) drilling hardware. The PTFE in sediments is a wear product of the seals used in the Drill Bit Assemblies (DBAs). It is expected that the drill assembly on the MSL flight model will also shed Teflon particles into drilled samples. One of the primary goals of the Sample Analysis at Mars (SAM) instrument suite on MSL is to test for the presence of martian organics in samples. Complications introduced by the potential presence of PTFE in drilled samples to the SAM evolved gas analysis (EGA or pyrolysisquadrupole mass spectrometry, pyr-QMS) and pyrolysis- gas chromatography mass spectrometry (Pyr- GCMS) experiments was investigated.

fluorocarbon contamination↗

DOE OSTI2024

Initial Testing of an In Situ Load Retention Aging Vessel

A thermal aging vessel instrumented with load cells was fabricated. The primary function of the vessel is to continuously monitor the in situ load retention of up to three compressed polymer coupons undergoing thermally accelerated aging under nitrogen. A secondary function is to enable gas sampling of the vessel headspace during thermal aging. Heating of the vessel is achieved using a custom heater jacket. To improve upon our conventional aging study methods which require periodic interruption of aging to perform load testing in an Instron machine at room temperature, this technology aims to automate/facilitate data acquisition/analysis, improve data quality, and enable uninterrupted compression of the polymer which represents the service condition. As an example case to assess functionality of the in situ vessel, the load retention of a siloxane elastomer material additively manufactured by direct-ink-writing (DIW) was measured at three different isothermal aging temperatures for ~1 month. Initial compression of the coupons while near the aging temperature was achieved by temporarily opening the heated vessel to access the interior chamber and manually tightening four nuts to drive the heated compression plate down onto the heated coupons. Initial testing demonstrated achievement of the primary load retention monitoring function. Unfortunately, the vessel leaked which prevented gas sampling; an active purge was used to maintain a nitrogen atmosphere. Welded or otherwise sealed joints, which could be implemented in a future design, would likely eliminate leak paths. To apply time-temperature superposition (TTS), a technique used to provide long-term prediction of the load retention from short-term isothermal data, the load retention needed to be calculated relative to the load at an estimated “equilibrium” time, after most of the transient viscoelastic physical relaxation occurred. The peak load immediately after compression could not be used as the load retention basis for two reasons: (1) age-related changes must be isolated from non-age-related physical relaxation before applying TTS and (2) the manual mechanism used to compress the specimens at the aging temperature was neither smooth nor repeatable which affected the peak load value. To better understand the effect of the mode of initial compression on the measured load, and possibly better estimate “equilibrium” physical relaxation times, systematic stress relaxation experiments were performed using an Instron machine with a thermal chamber. At a given temperature, the DIW polymer was compressed to a fixed strain in either a stepped or continuous manner at two different rates, then held at that strain for 24 hrs. The results indicated that, at a given temperature, the different stress relaxation curves appeared to converge to the same curve at some “equilibrium” time when the non-age-related physical relaxation was mostly complete. Though this observation suggests that the discontinuous manual compression employed by the vessel is feasible, a compression mechanism that is rapid, smooth, and repeatable would enhance its use.

36 MATERIALS SCIENCE↗

DOE OSTI2025

lllinois Storage Corridor CarbonSAFE Phase III: Pre-drilling Site Assessment: Prairie State Generating Company

The Illinois Storage Corridor project will drill a stratigraphic test well as part of the Illinois Storage Corridor CarbonSAFE Phase 3 project near the Prairie State Generating Company coal-fired power plant near Marissa, Illinois. The pre-drilling site evaluation has considered the primary target reservoirs, the Potosi Dolomite and St. Peter Sandstone, and primary seal, the Maquoketa Group. Data to be collected from the well include core, fluid samples, in situ well tests, geophysical logs intended to provide information on lithologic, geomechanical, and geophysical characteristics to determine the feasibility for the geologic sequestration of 50 million metric tons or more of injected carbon dioxide. The planned drilling site has been evaluated using available subsurface geologic data and analyses from the Illinois Basin. These data provide lithologic and structural information, shallow groundwater resource distribution, location of known nearby wellbores, and regional drilling characteristics. The data were used to generate geologic structure and isopach maps for the target reservoir and caprock strata and for prognosing the tops of major lithologic units to aid drilling and coring procedures. The regional analyses indicate that no known structural features are expected to negatively impact the target storage reservoir or caprock. No protected and sensitive areas, groundwater resources, or existing resource development are expected to be impacted by the proposed well drilling activities. The well is planned to be drilled to a total depth of approximately 5,600 feet (1,707 m) and terminate in the Precambrian. Cores (up to 5 intervals) will be collected from the Maquoketa Group, confining units above the St. Peter Sandstone, St. Peter Sandstone, confining units of the Potosi Dolomite and the Potosi Dolomite. Water samples will be attempted to be collected from the St. Peter Sandstone and Potosi Dolomite. Potential impact on drilling progress is a lost circulation zone in the Potosi Dolomite, which has been demonstrated to have intermittent cavernous porosity from karstification elsewhere in the Illinois Basin. This document also presents a preliminary coring and sampling program, proposed logging suite, and well testing program, all of which will be reviewed during drilling.

01 COAL, LIGNITE, AND PEAT↗

NASA NTRS1976

Integrated Real Time Contamination Monitor IRTCM

Engineering and design work was performed on a monitoring device for particulate and gas contamination to be used in the space shuttle cargo area during launch at altitudes up to 50 km and during return phases of the flight. The gas sampling device consists of ampules filled with specific absorber materials which are opened and/or sealed at preprogrammed intervals. The design eliminates the use of valves which, according to experiments, are never sealing properly at hard vacuum. Methods of analysis including in-flight measuring possibilities are discussed.

Luttges, W. E.↗

NASA NTRS1983

The Antaeus Project - An orbital quarantine facility for analysis of planetary return samples

A design is presented for an earth-orbiting facility for the analysis of planetary return samples under conditions of maximum protection against contamination but minimal damage to the sample. The design is keyed to a Mars sample return mission profile, returning 1 kg of documented subsamples, to be analyzed in low earth orbit by a small crew aided by automated procedures, tissue culture and microassay. The facility itself would consist of Spacelab shells, formed into five modules of different sizes with purposes of power supply, habitation, supplies and waste storage, the linking of the facility, and both quarantine and investigation of the samples. Three barriers are envisioned to protect the biosphere from any putative extraterrestrial organisms: sealed biological containment cabinets within the Laboratory Module, the Laboratory Module itself, and the conditions of space surrounding the facility.

Sweet, H. C.↗

NASA NTRS1996

An NMR Study of Microvoids in Polymers

An understanding of polymer defect structures, like microvoids in polymeric matrices, is most crucial to their fabrication and application potential. In this project guest atoms are introduced into the microvoids in PMR-15 and NMR is used to determine microvoid sizes and locations. Xenon is a relatively inert probe that would normally not be found naturally in polymer or in NMR probe materials. There are two NMR active Xenon isotopes, Xe-129 and Xe-131. The Xe atom has a very high polarizability, which makes it sensitive to the intracrystalline environment of polymers. Interactions between the Xe atoms and the host matrix perturb and Xe electron cloud, deshielding the nuclei, and thereby expanding the range of the observed NMR chemical shifts. This chemical shift range which may be as large as 5000 ppm, permits subtle structural and chemical effects to be studied with high sensitivity. The Xe-129-NMR line shape has been found to vary in response to changes in the pore symmetry of the framework hosts in Zeolites and Clathrasil compounds. Before exposure to Xe gas, the PMR-15 samples were dried in a vacuum oven at 150 C for 48 hours. The samples were then exposed to Xe gas at 30 psi for 72 hours and sealed in glass tubes with 1 atmosphere of Xenon gas. Xenon gas at 1 atmosphere was used to tune up the spectrometer and to set up the appropriate NMR parameters. A series of spectra were obtained interspersed with applications of vacuum and heating to drive out the adsorbed Xe and determine the role of Xe-Xe interactions in the observed chemical shift.

Toy, James↗