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At least 109 records · Page 6
All sourcesNASA NTRSDOE OSTI
NASA NTRS2011

The Laser Ablation Ion Funnel: Sampling for in situ Mass Spectrometry on Mars

A considerable investment has been made by NASA and other space agencies to develop instrumentation suitable for in situ analytical investigation of extra terrestrial bodies including various mass spectrometers (time-of-flight, quadrupole ion trap, quadrupole mass filters, etc.). However, the front-end sample handling that is needed to collect and prepare samples for interrogation by such instrumentation remains underdeveloped. Here we describe a novel approach tailored to the exploration of Mars where ions are created in the ambient atmosphere via laser ablation and then efficiently transported into a mass spectrometer for in situ analysis using an electrodynamic ion funnel. This concept would enable elemental and isotopic analysis of geological samples with the analysis of desorbed organic material a possibility as well. Such an instrument would be suitable for inclusion on all potential missions currently being considered such as the Mid-Range Rover, the Astrobiology Field Laboratory, and Mars Sample Return (i.e., as a sample pre-selection triage instrument), among others.

Johnson, Paul V.↗
NASA NTRS2010

Mars Science Laboratory Sample Acquisition, Sample Processing and Handling: Subsystem Design and Test Challenges

The Sample Acquisition/Sample Processing and Handling subsystem for the Mars Science Laboratory is a highly-mechanized, Rover-based sampling system that acquires powdered rock and regolith samples from the Martian surface, sorts the samples into fine particles through sieving, and delivers small portions of the powder into two science instruments inside the Rover. SA/SPaH utilizes 17 actuated degrees-of-freedom to perform the functions needed to produce 5 sample pathways in support of the scientific investigation on Mars. Both hardware redundancy and functional redundancy are employed in configuring this sampling system so some functionality is retained even with the loss of a degree-of-freedom. Intentional dynamic environments are created to move sample while vibration isolators attenuate this environment at the sensitive instruments located near the dynamic sources. In addition to the typical flight hardware qualification test program, two additional types of testing are essential for this kind of sampling system: characterization of the intentionally-created dynamic environment and testing of the sample acquisition and processing hardware functions using Mars analog materials in a low pressure environment. The overall subsystem design and configuration are discussed along with some of the challenges, tradeoffs, and lessons learned in the areas of fault tolerance, intentional dynamic environments, and special testing

Jandura, Louise↗
NASA NTRS1994

Purity and cleanness of aerogel as a cosmic dust capture medium

The capability for capturing micrometeoroids intact through laboratory simulations and in space in passive underdense silica aerogel offers a valuable tool for cosmic dust research. The integrity of the sample handling medium can substantially modify the integrity of the sample. Intact capture is a violent hypervelocity event: the integrity of the capturing medium can cause even greater modification of the sample. Doubts of the suitability of silica aerogel as a capture medium were raised at the 20th LPSC, and questions were raised again at the recent workshop on Particle Capture, Recovery, and Velocity Trajectory Measurement Technologies. Assessment of aerogel's volatile components and carbon contents have been made. We report the results of laboratory measurements of the purity and cleanliness of silica aerogel used for several Sample Return Experiments flown on the Get Away Special program.

Tsou, P.↗
NASA NTRS1994

Purity and Cleanness of Aeorgel as a Cosmic Dust Capture Medium

The capability for capturing micrometeoroids intact through laboratory simulations [Tsou 1988] and in space [Tsou 1993] in passive underdense silica aerogel offers a valuable tool for cosmic dust research. The integrity of the sample handling medium can substantially modify the integrity of the sample. Intact capture is a violent hypervelocity event: the integrity of the capturing medium can cause even greater modification of the sample.

micrometeoroids cosmic dust silica aerogel↗
NASA NTRS2009

Improved Instrument for Detecting Water and Ice in Soil

An instrument measures electrical properties of relatively dry soils to determine their liquid water and/or ice contents. Designed as a prototype of instruments for measuring the liquid-water and ice contents of lunar and planetary soils, the apparatus could also be utilized for similar purposes in research and agriculture involving terrestrial desert soils and sands, and perhaps for measuring ice buildup on aircraft surfaces. This instrument is an improved version of the apparatus described in Measuring Low Concentrations of Liquid Water and Ice in Soil (NPO-41822), NASA Tech Briefs, Vol. 33, No. 2 (February 2009), page 22. The designs of both versions are based on the fact that the electrical behavior of a typical soil sample is well approximated by a network of resistors and capacitors in which resistances decrease and capacitances increase (and the magnitude and phase angle of impedance changes accordingly) with increasing water content. The previous version included an impedance spectrometer and a jar into which a sample of soil was placed. Four stainless-steel screws at the bottom of the jar were used as electrodes of a fourpoint impedance probe connected to the spectrometer. The present instrument does not include a sample jar and can be operated without acquiring or handling samples. Its impedance probe consists of a compact assembly of electrodes housed near the tip of a cylinder. The electrodes protrude slightly from the cylinder (see Figure 1). In preparation for measurements, the cylinder is simply pushed into the ground to bring the soil into contact with the electrodes.

Buehler, Martin↗
NASA NTRS2016

Preserving, Enhancing, and Continuing the Scientific Legacy of the Apollo Sample Suite

From 1969 to 1972, Apollo astronauts collected 382 kg of rocks, soils, and core samples from six geologically diverse locations on the Moon. In the nearly 50 years since the samples were collected, over 3000 different studies have been conducted using the nearly 2200 different Apollo samples. Despite the maturity of the sample collection, many new studies of lunar samples are undertaken each year, with an average of more than 55 requests and more than 600 distinct subsamples allocated annually over the past five years. The Apollo samples are a finite resource, however. Although new studies are encouraged, it is important that new studies do not duplicate previous studies, and where possible, leverage previous results to inform and enhance the current studies. This helps to preserve the samples and scientific funding, both of which are precious resources. We have initiated several new efforts to rescue some of the early analyses from these samples, including unpublished analytical data. We are actively scanning NASA documentation in paper form that is related to the Apollo missions and sample processing, and we are collaborating with IEDA to establish a geochemical data base called MoonDB. To populate this database, we are actively working with about a dozen prominent lunar PIs to organize and transcribe years of both published and unpublished data, making it available to all researchers. This effort will also take advantage of new online analytical tools like PetDB. There have already been tangible results from the MoonDB data rescue effort. A pilot project involving the rescue of geochemical data of John Delano on Apollo pyroclastic glasses has already been referenced in multiple Apollo sample requests, and in fact, the compiled data was used as part of one of the new studies. Similarly, scanned sample handling reports have been utilized to find previously analyzed samples that were appropriate to fulfill new sample requests. We have also begun to image the Apollo samples using (1) micro‐CT scanning to document the interior structure of samples, and (2) comprehensive high resolution photography of samples, enabling high resolution 3D reconstructions of the samples. Both efforts will provide comprehensive access to these samples and allow for more targeted requests, and thus better curation of the samples for decades to come.

Zeigler, Ryan↗
NASA NTRS2012

Coring Sample Acquisition Tool

A sample acquisition tool (SAT) has been developed that can be used autonomously to sample drill and capture rock cores. The tool is designed to accommodate core transfer using a sample tube to the IMSAH (integrated Mars sample acquisition and handling) SHEC (sample handling, encapsulation, and containerization) without ever touching the pristine core sample in the transfer process.

Haddad, Nicolas E.↗
DOE OSTI2019

Ambient Metabolic Profiling and Imaging of Biological Samples with Ultrahigh Molecular Resolution using Laser Ablation Electrospray Ionization 21 Tesla FTICR Mass Spectrometry

Mass spectrometry (MS) has been an indispensable analytical tool in capturing the complexity and array of biomolecules within biological systems. However, conventional MS-based analytical workflows are limited in both throughput and measuring the native molecular state these systems, due in large part to sample handling and preparation. The development of ambient ionization methods capable of sampling directly from tissues circumvent many of these issues but requires the use of high-performance MS to resolve the molecular complexity within these samples. Herein, we demonstrate the unique combination of laser ablation electrospray ionization (LAESI) coupled with a 21 Tesla Fourier transform ion cyclotron resonance (21T-FTICR-MS) for MS imaging applications. This analytical platform provides isotopic fine structure information directly from native tissues, delivering a higher degree of confidence for molecular identification. The ability to capture and visualize the complex metabolic behavior of living organisms in situ is a bioanalytical grand challenge that has yet to be fully realized. Due to their excellent sensitivity and selectivity, mass spectrometry (MS)-based platforms offer a unique opportunity to characterize an array of biomolecules from a variety of biological samples.[1] One method in particular, MS imaging (MSI), has demonstrated the ability to simultaneously determine the spatial distributions for hundreds of biomolecules, e. g., metabolites, lipids, peptides, and xenobiotics, within complex biological systems simultaneously.[2-3] Matrix-assisted laser desorption/ionization (MALDI)-MSI remains the most common of these methods.[4] However, the application of an exogenous matrix, and the limited availability of commercial sources that operate under atmospheric pressure,[5] has significantly prohibited the ability of MALDI to be useful for biomolecular mapping of living systems. Ambient ionization methods that require minimal to no sample preparation, like desorption electrospray ionization (DESI and nano-DESI) and laser ablation electrospray ionization (LAESI), demonstrated the ability to spatially map biomolecule distributions within live organisms.

Mass Spectometry, fourier transform ion cyclostron↗
NASA NTRS1978

Self-sterilizing canister

Canister, originally conceived for remote sterilization of spacecraft packages, could be used terrestrially to handle samples in biologically hazardous environments. Multiwalled canister includes inner layer of pyrotechnic powder. For sterilization, electrically activated squib ignites powder, raising temperature of outer surface of canister to 230 degrees centigrade for several minutes. Thermal-buffer inner layer prevents inside temperature for exceeding 100 degrees centigrade to protect contents from damage. Samples in field hospitals and other emergency situations could also be handled by equipment.

Yang, L. C.↗
NASA NTRS2007

Fluence Uniformity Measurements in an Electron Accelerator Used for Irradiation of Extended Area Solar Cells and Electronic Circuits for Space Applications

It is common to have liquid crystal displays and electronic circuit boards with area sizes of the order of 20x20 sq cm on board of satellites and space vehicles. Usually irradiating them at different fluence values assesses the radiation damage in these types of devices. As a result, there is a need for a radiation source with large spatial fluence uniformity for the study of the damage by radiation from space in those devices. Kent State University s Program on Electron Beam Technology has access to an electron accelerator used for both research and industrial applications. The electron accelerator produces electrons with energies in the interval from 1 to 5 MeV and a maximum beam power of 150 kW. At such high power levels, the electron beam is continuously scanned back and forth in one dimension in order to provide uniform irradiation and to prevent damage to the sample. This allows for the uniform irradiation of samples with an area of up to 1.32 sq m. This accelerator has been used in the past for the study of radiation damage in solar cells (1). However in order to irradiate extended area solar cells there was a need to measure the uniformity of the irradiation zone in terms of fluence. In this paper the methodology to measure the fluence uniformity on a sample handling system (linear motion system), used for the irradiation of research samples, along the irradiation zone of the above-mentioned facility is described and the results presented. We also illustrate the use of the electron accelerator for the irradiation of large area solar cells (of the order of 156 sq cm) and include in this paper the electrical characterization of these types of solar cells irradiated with 5 MeV electrons to a total fluence of 2.6 x 10(exp 15) e/sq cm.

Uribe, Roberto M.↗
NASA NTRS2014

Development of a Linear Ion Trap Mass Spectrometer (LITMS) Investigation for Future Planetary Surface Missions

Future surface missions to Mars and other planetary bodies will benefit from continued advances in miniature sensor and sample handling technologies that enable high-performance chemical analyses of natural samples. Fine-scale (approx.1 mm and below) analyses of rock surfaces and interiors, such as exposed on a drill core, will permit (1) the detection of habitability markers including complex organics in association with their original depositional environment, and (2) the characterization of successive layers and gradients that can reveal the time-evolution of those environments. In particular, if broad-based and highly-sensitive mass spectrometry techniques could be brought to such scales, the resulting planetary science capability would be truly powerful. The Linear Ion Trap Mass Spectrometer (LITMS) investigation is designed to conduct fine-scale organic and inorganic analyses of short (approx.5-10 cm) rock cores such as could be acquired by a planetary lander or rover arm-based drill. LITMS combines both pyrolysis/gas chromatograph mass spectrometry (GCMS) of sub-sampled core fines, and laser desorption mass spectrometry (LDMS) of the intact core surface, using a common mass analyzer, enhanced from the design used in the Mars Organic Molecule Analyzer (MOMA) instrument on the 2018 ExoMars rover. LITMS additionally features developments based on the Sample Analysis at Mars (SAM) investigation on MSL and recent NASA-funded prototype efforts in laser mass spectrometry, pyrolysis, and precision subsampling. LITMS brings these combined capabilities to achieve its four measurement objectives: (1) Organics: Broad Survey Detect organic molecules over a wide range of molecular weight, volatility, electronegativity, concentration, and host mineralogy. (2) Organic: Molecular Structure Characterize internal molecular structure to identify individual compounds, and reveal functionalization and processing. (3) Inorganic Host Environment Assess the local chemical/mineralogical makeup of organic host phases to help determine deposition and preservation factors. (4) Chemical Stratigraphy Analyze the fine spatial distribution and variation of key species with depth.

Mars↗
DOE OSTI2018

Advanced detector signal acquisition and electron beam scanning for high resolution SEM imaging

We report the advancement of materials science at the mesoscale requires improvements in both sampling volumes/areas and spatial resolution in order to make statistically significant measurements of microstructures that influence higher-order material properties, such as fatigue and fracture. Therefore, SEM-based techniques have become desirable due to improvements in imaging resolution, large sample handling capability, and flexibility for in-situ instrumentation. By using fast sampling of SEM electron detector signals, intrinsic beam scanning defects have been identified that are related to the response time of the SEM electron beam deflectors and electron detectors. Mitigation of these beam scanning defects using detector sampling approaches and an adaptive model for settling time is shown to produce higher resolution SEM images, at faster image acquisition times, with a means to quantify the different response functions for various beam deflectors and detectors including those for electrons and ions.

47 OTHER INSTRUMENTATION↗
NASA NTRS1980

Study of sample drilling techniques for Mars sample return missions

To demonstrate the feasibility of acquiring various surface samples for a Mars sample return mission the following tasks were performed: (1) design of a Mars rover-mounted drill system capable of acquiring crystalline rock cores; prediction of performance, mass, and power requirements for various size systems, and the generation of engineering drawings; (2) performance of simulated permafrost coring tests using a residual Apollo lunar surface drill, (3) design of a rock breaker system which can be used to produce small samples of rock chips from rocks which are too large to return to Earth, but too small to be cored with the Rover-mounted drill; (4)design of sample containers for the selected regolith cores, rock cores, and small particulate or rock samples; and (5) design of sample handling and transfer techniques which will be required through all phase of sample acquisition, processing, and stowage on-board the Earth return vehicle. A preliminary design of a light-weight Rover-mounted sampling scoop was also developed.

Mitchell, D. C.↗
NASA NTRS2018

Maximum Sample Temperature for Mars Sample Return: A Historical Perspective

Since the first Mars Sample Return (MSR) report published by the Jet Propulsion Laboratory (JPL) in 1974 [1], a series of panels, reports, and white papers have recognized the importance of sample temperature and offered an informed sample maximum temperature (henceforth SMT) limit for returning martian samples to Earth. The Mars Sample Handling and Requirements Panel (MSHARP, 1999) stated that "[t]he main issue in sample preservation is temperature" [2]. More recently, the Mars Exploration Program Analysis Group (MEPAG)'s "Science Priorities for Mars Sample Return" report (2008), declared that "[s]ignificant loss, particularly to biological studies, occurs if samples reach +50C for three hours", whereby "scientific objectives related to life goals could be seriously compromised" [3]. By contrast, the Mars 2020 mission has adopted a SMT of +60C as spelled out in Beaty et al., 2016 [4]. Samples will be collected and then deposited on the surface in sealed tubes for possible retrieval and return to Earth. Beaty et al. [4] calculates that the samples will experience maximum temperatures of ~+30 to +60C, depending on latitude. At present, there is no mission requirement for the measurement/data logging of sample temperature during this period. We will explore the history of martian SMTs, as they have been recorded since 1974 [1], effectively representing input across multiple generations of Mars scientists. Ten separate publications present SMTs for MSR samples [1-10]. One report [10] is for a mission concept specifically designed to exclude life detection investigations, and recommended an SMT of 50C. Another did not specify a temperature, recommending "Mars ambient temperature" [5]. Of the remaining eight, SMTs are given as: -30C [1], -20C [3], 60C [4], -73 to 41C depending on sample type [6], -40C [7], -43 to 13C depending on type [2,8], and -33C [9]. If we restrict the temperatures to samples highlighted in the Mars 2020 mission goals, i.e. organics-bearing and sedimentary rocks, then the average SMT is -28+/-39C (n=8). Applying a Dixon's Q Test at P=0.05 (two-tailed), the 60C SMT [4] fails with Q=0.602 versus Qcrit=0.526. Excluding the outlier produces an average SMT of -40+/-17C (n=7). Therefore, the average SMT expressed by the Mars science community over the past 44 years (two generations) is a sample temperature no greater than -40C. The difference in chemical reaction rates between this average SMT and Beaty et al [4] can be estimated using the Arrhenius equation. Assuming a generic chemical reaction with an activation energy of 50 kJ/mol and a pre-exponential factor invariant with temperature, this reaction will proceed 2300x faster at 60C than at -40C. To illustrate the effects of the increased reaction rate, consider 10 ppb of alanine in a Mars 2020 cache, and assume that it becomes unmeasurable if it degrades to 1 ppb, as per the Mars 2020 Organic Contamination Panel contamination limits [11]. If we illustrate the effect with an arbitrary degradation rate such that the alanine will become undetectable in ten years at -40C, then the same 10 ppb alanine degrades beyond detectability in only 38 days at 60C. Further research is required to quantify expected analyte losses in the cached samples due to thermal processing.

Fries, Marc↗
NASA NTRS2024

Will MSR Samples Cached on the Martian Surface Experience Significantly Greater Thermal Degradation than Samples Retained in the Rover?

Since the first Mars Sample Return (MSR)-related report published by the Jet Propulsion Laboratory (JPL) in 1974, a series of panels, reports, and white papers have recognized the importance of sample temperature in meeting mission goals and defined a sample maximum temperature (henceforth SMT) limit. The Mars Sample Handling and Requirements Panel (MSHARP, 1999) flatly stated that “[t]he main issue in sample preservation is temperature”. The Mars Exploration Program Analysis Group (MEPAG)’s “Science Priorities for Mars Sample Return” report (2008), declared that “[s]ignificant loss, particularly to biological studies, occurs if samples reach +50°C for three hours ” whereby “scientific objectives related to life goals could be seriously compromised”. Overall, a total of seven panels, white papers, and conference reports adopted a SMT of -40±17°C to preserve samples sufficiently to confidently achieve success in studies of past or present Martian life (see more detail in [5]). In contrast, the Mars 2020 rover (M2020) mission adopted a SMT of +60°C for samples stored on the Martian surface and +50°C for samples retained inside the rover, as stated in a conference poster presented by Beaty et al., 2016. M2020 is currently collecting samples for MSR in tubes. Half of those tubes will be retained within the M2020 rover body (hereafter rover samples, or RS) and half will be deposited on the Martian surface (cached samples or CS), with a currently undetermined number of each collected up to ten years later for return to Earth. CS samples can be expected to experience significantly higher temperatures than RS samples based on their exposed location in sunlight. This work will explore differences in deleterious chemical reaction rates due to thermal environment of both tube types. The findings here should be debated openly and considered when deciding which samples to return to Earth.

M Fries↗
DOE OSTI2020

Sample processing and analysis methods and apparatus

Sample handling, processing and analysis methods and apparatus are described. According to one aspect, a sample processing method includes providing a sample, providing a reference frame which comprises a plurality of markers arranged in a predefined pattern, wherein individual ones of the markers are uniquely identifiable from others of the markers, and associating the reference frame comprising the markers with the sample. The markers are amenable to human or machine reading and for computational manipulation in some examples.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Salt Vessel-Sample Generator Interface

The goal of the salt sampling program at Argonne is to develop and deploy automated molten salt sampling approaches for interfacing relevant unit operations with salt analysis to improve the timeliness and accuracy of sampling-based accountancy measurements. One technology under development is a vacuum sampler loop module. In this system, molten salt is drawn from a process vessel through a heated sampling line and into a charge vessel. Next, one or more samples are split from the volume in the charge vessel and the remaining salt is returned to the process. The vacuum sampler loop module is being developed to interface with other sample processing and analysis modules to enable rapid at-line sample characterization. The main purpose of the vacuum sampling loop module is to enable the collection of samples that are more representative of the bulk salt by replacing traditional point samplers (i.e., dip probes) with a sampling approach that captures a larger cross section of salt. Additionally, the vacuum sampling approach eliminates the risk of dross contamination of samples and avoids the use of moving parts in the salt. Two methods of interfacing the vacuum sampling loop with a precision pneumatic sample generator were investigated in FY21. This report covers the testing of fluidic coupling between the two modules. Two iterations of the fluidically coupled modules were tested. The first iteration system coupled the two modules using a freeze valve to seal the vacuum sampler during filling and to control flow into the pneumatic sample generator. While this integrated system functioned as intended, some changes were implemented to make the system more robust and better suited to remote deployment. Specifically, the system was made to be more modular and active control of the vacuum filling operation was replaced with a passive control mechanism. For passive filling, the salt charge vessel was vented to a small gas tank that was at negative pressure, causing salt to be drawn into the vessel until the force of the fluid head was in equilibrium with the gas pressure. The passive control system performed well and will be used in future iterations. Another change in the second system was a newly configured pneumatic sample generator in which sample ejection occurred through a hole in the reservoir’s stainless-steel side wall instead of through a non-wetted sapphire orifice on the bottom. This alternate configuration may be better suited for near-process deployment because it enables on-line orifice maintenance and an orifice bypass drain back to the process. A third change in the second iteration system was the transition to a two-chamber charge vessel which split off a fraction of the sampled salt as a liquid aliquot. The goal was to create a buffer mechanism that would allow reproducible aliquoting of samples, independently of variability in the charge vessel fill height. While the two-chamber design was functional, the sample size reproducibility was below target values. To improve reproducibility and overcome many of the impediments to remote deployment of the vacuum sampling loop module, separate work was conducted to replace the two-chamber liquid aliquoting mechanism with aliquoting into single-use sample tubes. Solid salt transfer in the sample tubes will replace fluidic coupling for integrating the vacuum sampler with downstream modules. Because the proposed operations can all be executed with simple overhead actuation mechanisms or other existing hot-cell technology, there will be no need for large investments in novel hot cell sample handling technologies using this alternate approach. As such, near-term deployment of the vacuum sampling technology will be achievable. This new approach for automated coupling of sample tubes with down-stream modules is covered in a separate FY21 report, and a remotely operated version of the vacuum sampler loop module with the tube aliquoting feature is planned for FY22.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2025

Oxygen stable isotopes in the nuclear fuel cycle: Assessment of the potential for determining the fabrication and provenance history of anhydrous and hydrous uranium oxides

Determining the origin and history of interdicted nuclear materials is a central challenge in nuclear forensics. The oxygen stable isotope composition of uranium oxide compounds has emerged as a promising forensic signature, attracting increasing attention since the early 2000s. This review examines analytical techniques for measuring oxygen isotope compositions in uranium oxides and evaluates how the nuclear fuel production cycle introduces or modifies these isotopic signatures. The potential for forensic geolocation is explored through workflows that calibrate the relationship between environmental water oxygen isotopes and those found in uranium oxides. Key strengths and limitations of this approach are assessed, including gaps in knowledge related to isotope fractionation during specific stages of the fuel cycle, and processing facility water inputs. The importance of proper sample handling and storage under inert atmospheres, as well as a deeper understanding of both intra-sample oxygen isotope heterogeneity, and hydrous uranium oxide phase formation, is highlighted for improving the reliability of forensic interpretations. In conclusion, the development of uranium oxide standards with well-characterized δ 18 O values and international collaboration toward consensus on their use are identified as essential steps for advancing the field.

Attribution↗