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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 37 records · Page 2

Utility of spatially-resolved atmospheric pressure surface sampling and ionization techniques as alternatives to mass spectrometric imaging (MSI) in drug metabolism

1. Tissue distribution studies of drug molecules play an essential role in the pharmaceutical industry and are commonly undertaken using quantitative whole body autoradiography (QWBA) methods. 2. The growing need for complementary methods to address some scientific gaps around radiography methods has led to increased use of mass spectrometric imaging (MSI) technology over the last 5 to 10 years. More recently, the development of novel mass spectrometric techniques for ambient surface sampling has redefined what can be regarded as fit-for-purpose for MSI in a drug metabolism and disposition arena. 3. Together with a review of these novel alternatives, this paper details the use of two liquid microjunction (LMJ)- based mass spectrometric surface sampling technologies. These approaches are used to provide qualitative determination of parent drug in rat liver tissue slices using liquid extraction surface analysis (LESA) and to assess the performance of a LMJ surface sampling probe (LMJ-SSP) interface for quantitative assessment of parent drug in brain, liver and muscle tissue slices. 4. An assessment of the utility of these spatially-resolved sampling methods is given, showing interdependence between mass spectrometric and QWBA methods, in particular there emerges a reason to question typical MSI workflows for drug metabolism; suggesting the expedient use of profile or region analysis may be more appropriate, rather than generating time-intensive molecular images of the entire tissue section.

ambient surface sampling↗

Soil development and sampling strategies for the returned Martian surface samples

Sampling of the Martian surface materials should be based on the experience gained from the study of soils and rocks collected in cold, dry environments, i.e., dry valleys of Antarctica. Previous studies have suggested that some of our best terrestrial analogs of the Martian soils are represented by those found in the polar deserts of Antarctica. Special sampling considerations must be taken into account when obtaining these samples because they represent at least five distinct types of materials. Weathering of planetary regolith materials occurs from both chemical and physical interactions of the planet's surface materials with the atmosphere and, if present, the hydrosphere and biosphere along with extraplanetary objects which may produce the original surface materials and produce secondary materials that are product of equilibrium between the atmosphere and study weathering processes and regolith development occurring on Martian-like surfaces, simulation studies must be carried out in materials in the field.

Gibson, Everett K.↗

Combining Transmission Geometry Laser Ablation and a Non Contact Continuous Flow Surface Sampling Probe/Electrospray Emitter for Mass Spectrometry-Based Chemical Imaging

This paper describes the coupling of ambient pressure transmission geometry laser ablation with a liquid phase sample collection into a continuous flow surface sampling probe/electrospray emitter for mass spectrometry based chemical imaging. The flow probe/emitter device was placed in close proximity to the surface to collect the sample plume produced by laser ablation. The sample collected was immediately aspirated into the probe and on to the electrospray emitter, ionized and detected with the mass spectrometer. Freehand drawn ink lines and letters and an inked fingerprint on microscope slides were analyzed. The circular laser ablation area was about 210 m in diameter and under the conditions used in these experiments the spatial resolution, as determined by the size of the surface features distinguished in the chemical images, was about 100 m.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Hydrophobic Treatment Enabling Analysis of Wettable Surfaces using a Liquid Microjunction Surface Sampling Probe/Electrospray Ionization-Mass Spectrometry System

An aerosol application procedure involving one or more commercially available silicone based products was developed to create hydrophobic surfaces that enable analysis of otherwise wettable, absorbent surfaces using a liquid microjunction surface sampling probe/electrospray ionization mass spectrometry system. The treatment process resulted in a hydrophobic surface that enabled formation of the requisite probe - to - surface liquid microjunction for sampling and allowed efficient extraction of the analytes from the surface, but did not contribute significant chemical background in the mass spectra. The utility of this treatment process was demonstrated with the treatment of wettable high performance thin layer chromatography plates, post plate development, and their subsequent analysis with the sampling probe. The surface treatment process for different surface types was described and explained and the effectiveness of the treatment and subsequent analysis was illustrated using alkaloids from Goldenseal (Hydrastis canadensis) root separated on a normal phase silica gel 60 F254S plate and peptides from protein tryptic digests separated on a Protochrom HPTLC Silica gel 60 F254S plate and a Protochrom HPTLC cellulose sheet. This simple surface treatment process significantly expands the analytical surfaces that can be analyzed with the liquid microjunction surface sampling probe, and therefore, also expands the analytical utility of this liquid extraction based surface sampling approach.

Walworth, Matthew J↗

Liquid microjunction surface sampling probe fluid dynamics: Characterization and application of an analyte plug formation operational mode

The recently discovered sample plug formation and injection operational mode of a continuous flow, coaxial tube geometry, liquid microjunction surface sampling probe (LMJ-SSP) (J. Am. Soc. Mass Spectrom, 2011) was further characterized and applied for concentration and mixing of analyte extracted from multiple areas on a surface and for nanoliter-scale chemical reactions of sampled material. A transparent LMJ-SSP was constructed and colored analytes were used so that the surface sampling process, plug formation, and the chemical reactions could be visually monitored at the sampling end of the probe before being analyzed by mass spectrometry of the injected sample plug. Injection plug peak widths were consistent for plug hold times as long as the 8 minute maximum attempted (RSD below 1.5%). Furthermore, integrated injection peak signals were not significantly different for the range of hold times investigated. The ability to extract and completely mix individual samples within a fixed volume at the sampling end of the probe was demonstrated and a linear mass spectral response to the number of equivalent analyte spots sampled was observed. Lastly, using the color and mass changing chemical reduction of the redox dye 2,6-dichlorophenol-indophenol with ascorbic acid, the ability to sample, concentrate, and efficiently run reactions within the same plug volume within the probe was demonstrated.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

An enhanced droplet-based liquid microjunction surface sampling system coupled with HPLC-ESI-MS/MS for spatially resolved analysis

Droplet-based liquid microjunction surface sampling coupled with high-performance liquid chromatography (HPLC)-electrospray ionization (ESI)-tandem mass spectrometry (MS/MS) for spatially resolved analysis provides the possibility of effective analysis of complex matrix samples and can provide a greater degree of chemical information from a single spot sample than is typically possible with a direct analysis of an extract. Described here is the setup and enhanced capabilities of a discrete droplet liquid microjunction surface sampling system employing a commercially available CTC PAL autosampler. The system enhancements include incorporation of a laser distance sensor enabling unattended analysis of samples and sample locations of dramatically disparate height as well as reliably dispensing just 0.5 μL of extraction solvent to make the liquid junction to the surface, wherein the extraction spot size was confined to an area about 0.7 mm in diameter; software modifications improving the spatial resolution of sampling spot selection from 1.0 to 0.1 mm; use of an open bed tray system to accommodate samples as large as whole-body rat thin tissue sections; and custom sample/solvent holders that shorten sampling time to approximately 1 min per sample. Lastly, the merit of these new features was demonstrated by spatially resolved sampling, HPLC separation, and mass spectral detection of pharmaceuticals and metabolites from whole-body rat thin tissue sections and razor blade (“crude”) cut mouse tissue.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Stereochemistry of amino acids in surface samples of a marine sediment

In two surface samples of marine sediment, the percentages of D-alanine and D-aspartic acid are significantly higher than the other D-amino acids and are similar to the range found in soils. The percentage of D-glutamic acid is also higher than the other amino acids but less than D-alanine and D-aspartic acid. These D-amino acids may come mainly from bacteria.

Pollock, G. E.↗

Detailed Design of an Earth Entry Vehicle for Comet Surface Sample Return

The 2013 Decadal Survey for New Frontiers missions identifies several high-value science missions, including Comet Surface Sample Return (CSSR). A CSSR mission will advance the scientific community's fundamental understanding of the origin of the solar system and the contribution of comets to the volatile inventory of the Earth. An entry capsule, or earth entry vehicle (EEV), is be required to protect the scientific payload from the extreme conditions of atmospheric entry, descent, and landing. The Decadal Survey Mission Concept Study along with an APL (Johns Hopkins University Applied Physics Lab) 2007-2008 Comet Surface Sample Mission Study details several of the driving requirements for a CSSR EEV; these include a payload volume and mass and inertial entry velocity of 9 kilometers per second. The mission concept study selected a Multi-Mission Earth Entry Vehicle (MMEEV) design concept derived from the Mars Sample Return (MSR) entry capsule design because of its increased reliability over a parachute-based vehicle. This presentation will explore detailed design of a CSSR-capable Earth Entry Vehicle, including trajectories, aeroheating predictions and associated thermal protection system masses, and onboard instrumentation for entry science.

Trajectory Analysis↗

A Conceptual Architecture for Venus Surface Sample Return

A conceptual architecture for retrieval of a sample of the surface of Venus is proposed. The mission concept incorporates a high-temperature aircraft to retrieve the sample from the surface and raise it into the upper atmosphere, a balloon-borne platform to produce fuel from the carbon dioxide atmosphere of Venus, and a launch vehicle to bring the sample into Venus orbit, where it is retrieved by an Earth-return vehicle.

Venus↗

Surface Sampling System for Low-Gravity Missions

SpaceWorks has identified several sampling missions that could benefit from the technology developed under this project. Requirements were established for the surface sampling system. SpaceWorks teamed with Virginia Tech to identify and select a baseline adhesive suitable for the surface sampling system. SpaceWorks identified Solimide foam as the baseline substrate material. SpaceWorks conducted extensive testing to characterize the performance of the substrate/adhesive combination. A prototype version of the sampler head was designed and built by SpaceWorks.

Preble, Jeffrey C.↗

Force-Control Algorithm for Surface Sampling

A G-FCON algorithm is designed for small-body surface sampling. It has a linearization component and a feedback component to enhance performance. The algorithm regulates the contact force between the tip of a robotic arm attached to a spacecraft and a surface during sampling.

Acikmese, Behcet↗

Analytical Model of the Nonlinear Dynamics of Cantilever Tip-Sample Surface Interactions for Various Acoustic-Atomic Force Microscopies

A comprehensive analytical model of the interaction of the cantilever tip of the atomic force microscope (AFM) with the sample surface is developed that accounts for the nonlinearity of the tip-surface interaction force. The interaction is modeled as a nonlinear spring coupled at opposite ends to linear springs representing cantilever and sample surface oscillators. The model leads to a pair of coupled nonlinear differential equations that are solved analytically using a standard iteration procedure. Solutions are obtained for the phase and amplitude signals generated by various acoustic-atomic force microscope (A-AFM) techniques including force modulation microscopy, atomic force acoustic microscopy, ultrasonic force microscopy, heterodyne force microscopy, resonant difference-frequency atomic force ultrasonic microscopy (RDF-AFUM), and the commonly used intermittent contact mode (TappingMode) generally available on AFMs. The solutions are used to obtain a quantitative measure of image contrast resulting from variations in the Young modulus of the sample for the amplitude and phase images generated by the A-AFM techniques. Application of the model to RDF-AFUM and intermittent soft contact phase images of LaRC-cp2 polyimide polymer is discussed. The model predicts variations in the Young modulus of the material of 24 percent from the RDF-AFUM image and 18 percent from the intermittent soft contact image. Both predictions are in good agreement with the literature value of 21 percent obtained from independent, macroscopic measurements of sheet polymer material.

Cantrell, John H., Jr.↗

Evaluation of surface sampling method performance for Bacillus Spores on clean and dirty outdoor surfaces.

Recovery of Bacillus atrophaeous spores from grime-treated and clean surfaces was measured in a controlled chamber study to assess sampling method performance. Outdoor surfaces investigated by wipe and vacuum sampling methods included stainless steel, glass, marble and concrete. Bacillus atrophaeous spores were used as a surrogate for Bacillus anthracis spores in this study designed to assess whether grime-coated surfaces significantly affected surface sampling method performance when compared to clean surfaces. A series of chamber tests were carried out in which known amounts of spores were allowed to gravitationally settle onto both clean and dirty surfaces. Reference coupons were co-located with test coupons in all chamber experiments to provide a quantitative measure of initial surface concentrations of spores on all surfaces, thereby allowing sampling recovery calculations. Results from these tests, carried out under both low and high humidity conditions, show that spore recovery from grime-coated surfaces is the same as or better than spore recovery from clean surfaces. Statistically significant differences between method performance for grime-coated and clean surfaces were observed in only about half of the chamber tests conducted.

36 MATERIALS SCIENCE↗

Search for organic and volatile inorganic compounds in two surface samples from the Chryse Planitia region of Mars

Two surface samples collected from the Chryse Planitia region of Mars were heated to temperatures up to 500 C, and the volatiles that they evolved were analyzed with a gas chromatograph-mass spectrometer. Only water and carbon dioxide were detected. This implies that organic compounds have not accumulated to the extent that individual components could be detected at levels of a few parts per billion by weight in the samples. Proposed mechanisms for the accumulation and destruction of organic compounds are discussed in the light of this limit.

Biemann, K.↗

Analysis of the Touch-And-Go Surface Sampling Concept for Comet Sample Return Missions

This paper studies the Touch-and-Go (TAG) concept for enabling a spacecraft to take a sample from the surface of a small primitive body, such as an asteroid or comet. The idea behind the TAG concept is to let the spacecraft descend to the surface, make contact with the surface for several seconds, and then ascend to a safe location. Sampling would be accomplished by an end-effector that is active during the few seconds of surface contact. The TAG event is one of the most critical events in a primitive body sample-return mission. The purpose of this study is to evaluate the dynamic behavior of a representative spacecraft during the TAG event, i.e., immediately prior, during, and after surface contact of the sampler. The study evaluates the sample-collection performance of the proposed sampling end-effector, in this case a brushwheel sampler, while acquiring material from the surface during the contact. A main result of the study is a guidance and control (G&C) validation of the overall TAG concept, in addition to specific contributions to demonstrating the effectiveness of using nonlinear clutch mechanisms in the sampling arm joints, and increasing the length of the sampling arms to improve robustness.

Touch-and-Go (TAG)↗

Using Paraffin PCM, Cryogel and TEC to Maintain Comet Surface Sample Cold from Earth Approach Through Retrieval

An innovative thermal design concept to maintain comet surface samples cold (for example, 263 degrees Kelvin, 243 degrees Kelvin or 223 degrees Kelvin) from Earth approach through retrieval is presented. It uses paraffin phase change material (PCM), Cryogel insulation and thermoelectric cooler (TEC), which are commercially available.

comet surface sample return; thermoelectric cooler↗