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All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Importance of sample preparation on reliable surface characterisation of nano-objects: ISO Standard 20579-4

The international ISO Standard 20579-4, dealing with the history and preparation of nano-objects for surface analysis, has been developed to help address some of the replication and reproducibility issues caused by the fundamental nature of nano-objects. Although all types of samples requiring surface analysis need thoughtful preparation, nano-objects, for which many properties are controlled by their surfaces, present additional challenges in order to avoid variations and artefacts due to the handling and preparation of materials prior to analysis. This international standard is part of a series of standards related to preparation of samples for surface chemical analysis. Parts 1 and 2 of ISO Standard series 20579 address general issues that apply to many samples. Part 4 specifically considers issues that arise due to the inherent nature of nano-objects. Because of sensitivity to their environment, the standard indicates the minimum information that needs to be reported about the handling and preparation of nano-objects prior to surface analysis. This information should become part of sample provenance information that helps assure the reliability and usefulness of data obtained from surface-analysis in the context of the synthesis, processing and analysis history of a batch of material. Application of this standard can help address reproducibility and traceability issues associated with synthesis, processing, and characterization of nano-objects in research and commercial applications.

nano-object characterization, surface analysis, sa↗
NASA NTRS2011

In-Situ XRF Measurements in Lunar Surface Exploration Using Apollo Samples as a Standard

Samples collected during the Apollo lunar surface missions were sampled and returned to Earth by astronauts with varying degrees of geological experience. The technology used in these EVAs, or extravehicular activities, included nothing more advanced than traditional terrestrial field instruments: rock hammer, scoop, claw tool, and sample bags. 40 years after Apollo, technology is being developed that will allow for a high-resolution geochemical map to be created in the field real-time. Handheld x-ray fluorescence (XRF) technology is one such technology. We use handheld XRF to enable a broad in-situ characterization of a geologic site of interest based on fairly rapid techniques that can be implemented by either an astronaut or a robotic explorer. The handheld XRF instrument we used for this study was the Innov-X Systems Delta XRF spectrometer.

Young, Kelsey E.↗
NASA NTRS1974

Gamma-spectrometric analysis of Luna 16 sample of lunar surface material

Using a scintillation gamma spectrometer with shielding against anticoincidences, the content of the natural radioelements (K, U, and Th) and long-lived cosmogenic radioisotopes (Al-26, Na-22, and Mn-54) in a sample of Sea of Fertility regolith was determined. Based on the content data of natural radioelements, an attempt was made to classify this sample in the scale of petrochemical types of terrestrial rocks arranged in accordance with their silicic content and alkalinity. Within the frame of reference of calcium-uranium systematics of lunar samples, a comparison was made of the K/U ratio obtained for the Sea of Fertility sample with analogous data for other regions of the moon. Also discussed are problems on the depthwise distribution of cosmogenic radioisotopes along the regolith profile.

Surkov, Y. A.↗
DOE OSTI2010

Detection and analysis of cyclotrimethylenetrinitramine (RDX) in environmental samples by surface-enhanced Raman spectroscopy

Techniques for rapid and sensitive detection of energetics such as cyclotrimethylenetrinitramine (RDX) are needed both for environmental and security screening applications. Here we report the use of surface-enhanced Raman scattering (SERS) spectroscopy to detect traces of RDX with good sensitivity and reproducibility. Using gold (Au) nanoparticles ( 90 100 nm in diameter) as SERS substrates, RDX was detectable at concentrations as low as 0.15 mg/l in a contaminated groundwater sample. This detection limit is about two orders of magnitude lower than those reported previously using SERS techniques. A surface enhancement factor of 6 104 was obtained. This research further demonstrates the potential for using SERS as a rapid, in situ field screening tool for energetics detection when coupled with a portable Raman spectrometer.

54 ENVIRONMENTAL SCIENCES↗
NASA NTRSDate not supplied

Continued Environmental Microbiology Monitoring of the International Space Station (ISS) Veggie Unit Used for In-Flight, Crop-Based Food Systems

Crewmembers live and work in a closed environment that is monitored to ensure their health and safety. To ensure occupants’ health and safety during their spaceflight residency, Environmental Health System (EHS) microbial samples including air, surface, and water, are collected, enumerated, and analyzed quarterly to monitor on-board system contamination and potential risks to crew health. Quarterly monitoring of the microorganisms in the ISS environment supports crew safety and contributes to a large set of microbial concentration and diversity data. Based upon data historically collected over the years, in-flight microbial requirements have been established to maintain the health and safety of the spacecraft environment. This study leverages quarterly operational Environmental Health System (EHS) sampling by collecting additional microbial samples from the surface of the station’s Veggie plant production system. Microbial surface samples collected from the Veggie plant production system will yield microbial concentration and diversity that can be compared and analyzed with nominal surface samples from the vehicle. The data collected in this study will aid in the development of requirements for spaceflight-based food production systems. Continued surface sampling of the internal and external surfaces of the Veggie locker, along with collaboration from both Johnson Space Center (JSC) & Kennedy Space Center (KSC) scientists studying the microbiome of the veggie-crop systems, will be implemented as part of the future development of crop-based food system requirements for the ISS and beyond. This presentation will include a review of the study procedures and evaluations of the current results.

Christian Mena↗
DOE OSTI2024

Sample mount for electron backscatter diffraction

A sample mount having a bottom surface, a front surface, and a second portion is disclosed. The first portion is perpendicular to the bottom surface. The second portion has an external surface and an internal surface and extends from the first portion to form a 70-degree angle relative to the bottom surface. The sample mount may also have a top surface, an opening extending through the second portion of the front surface, and a receiving area configured to receive a sample, wherein the top surface presents an unimpeded path between the sample and an SEM pole piece. The sample mount may include a spring-loaded handle configured to push the sample against the internal surface of the second portion of the front surface, wherein pushing the sample against the internal surface places the sample at the 70-degree angle relative to the bottom surface.

Wieliczka, David M.↗
NASA NTRS2019

Surface erythemal UV irradiance in the continental United States derived from ground-based and OMI observations: quality assessment, trend analysis and sampling issues

Surface full-sky erythemal dose rate (EDR) from the Ozone Monitoring Instrument (OMI) at both satellite overpass time and local noon time is evaluated against ground measurements at 31 sites from the US Department of Agriculture's (USDA) UV-B Monitoring and Research Program (UVMRP) over the period of 2005–2017. We find that both OMI overpass and solar noon time EDR are highly correlated with the measured counterparts (with a linear correlation coefficient of 0.90 and 0.88, respectively). Although the comparison statistics are improved with a longer time window (0.5–1.0 h) for pairing surface and OMI measurements, both OMI overpass and local noon time EDRs have 7 % overestimation that is larger than 6 % uncertainty in the ground measurements and show different levels of dependence on solar zenith angle (SZA) and to lesser extent on cloud optical depth. The ratio of EDR between local noon and OMI overpass time is often (95 % in frequency) larger than 1 with a mean of 1.18 in the OMI product; in contrast, the same ratio from surface observation is normally distributed with 22 % of the times less than 1 and a mean of 1.38. This contrast in part reflects the deficiency in the OMI surface UV algorithm that assumes constant atmospheric conditions between overpass and noon time. The probability density functions (PDFs) for both OMI and ground measurements of noontime EDR are in statistically significant agreement, showing dual peaks at ∼20 and ∼200 mW/sq. m, respectively; the latter is lower than 220 mW/ sq. m, the value at which the PDF of daily EDR from ground measurements peaks, and this difference indicates that the largest EDR value for a given day may not often occur at local noon. Lastly, statistically significant positive trends of EDR are found in the northeastern US in OMI data, but opposite trends are found within ground-based data (regardless of sampling for either noontime or daily averages). While positive trends are consistently found between OMI and surface data for EDR over the southern Great Plains (Texas and Oklahoma), their values are within the uncertainty of ground measurements. Overall, no scientifically sound trends can be found among OMI data for aerosol total and absorbing optical depth, cloud optical depth and total ozone to explain coherently the surface UV trends revealed either by OMI or ground-based estimates; these data also cannot reconcile trend differences between the two estimates (of EDR from OMI and surface observations). Future geostationary satellites with better spatiotemporal resolution data should help overcome spatiotemporal sampling issues inherent in OMI data products and therefore improve the estimates of surface UV flux and EDR from space.

Ozone Monitoring Instrument (OMI)↗
NASA NTRS2013

Method and Apparatus for Measuring Near-Angle Scattering of Mirror Coatings

Disclosed herein is a method of determining the near angle scattering of a sample reflective surface comprising the steps of: a) splitting a beam of light having a coherence length of greater than or equal to about 2 meters into a sample beam and a reference beam; b) frequency shifting both the sample beam and the reference beam to produce a fixed beat frequency between the sample beam and the reference beam; c) directing the sample beam through a focusing lens and onto the sample reflective surface, d) reflecting the sample beam from the sample reflective surface through a detection restriction disposed on a movable stage; e) recombining the sample beam with the reference beam to form a recombined beam, followed by f) directing the recombined beam to a detector and performing heterodyne analysis on the recombined beam to measure the near-angle scattering of the sample reflective surface, wherein the position of the detection restriction relative to the sample beam is varied to occlude at least a portion of the sample beam to measure the near-angle scattering of the sample reflective surface. An apparatus according to the above method is also disclosed.

Chipman, Russell A.↗
DOE OSTI2010

Determination of Natural Beryllium (Be) in Soil and Swipe Samples Utilizing Yttrium/Beryllium Ratio

1. Objective: A method to determine whether beryllium (Be) components in surface swipe samples are from a natural source is needed. 2. Methods: Soil samples and surface swipes from area facilities were analyzed for marker elements to identify source pathways for beryllium (Be). To be useful, the natural marker element must be present at reasonably consistent levels across the site, must correlate with the Be concentration, and not have the potential to be present from non-natural sources. 3. Results: The research on marker elements used to identify source pathways for beryllium (Be) concentrations demonstrates a clear correlation between Be and yttrium (Y) in natural soils on the Nevada National Security Site. The Y/Be ratio is proposed as a method to characterize the source of Be in soil and surface swipe samples and to aid in recommendations for follow up actions. Swipe samples are analyzed using an ICP/MS method and compared with results from soil samples. Natural soil constituent levels and the Y/Be Ratio range is determined for the occupied and historical facilities and surrounding areas. Y/Be ratios within the statistical range established indicate the Be is from a natural source. Y/Be ratios lower than this range indicate the presence of another Be source, and may then be correlated to alloy, ceramic, or other operational sources by the ratios of copper, nickel, cobalt, uranium, and/or niobium. Example case studies of evaluations of buildings with historical operational beryllium usage, current ongoing technical processes, and heavy equipment used in large building demolitions are included demonstrating the value of the ratio approach. 4. Conclusions: This differentiation is valuable as there is no known correlation between natural beryllium in soil and beryllium disease.

54 ENVIRONMENTAL SCIENCES↗
NASA NTRS1974

Mathematical estimation of the level of microbial contamination on spacecraft surfaces by volumetric air sampling

Microbiological sampling methods presently used for enumeration of microorganisms on spacecraft surfaces require contact with easily damaged components. Estimation of viable particles on surfaces using air sampling methods in conjunction with a mathematical model would be desirable. Parameters necessary for the mathematical model are the effect of angled surfaces on viable particle collection and the number of viable cells per viable particle. Deposition of viable particles on angled surfaces closely followed a cosine function, and the number of viable cells per viable particle was consistent with a Poisson distribution. Other parameters considered by the mathematical model included deposition rate and fractional removal per unit time. A close nonlinear correlation between volumetric air sampling and airborne fallout on surfaces was established with all fallout data points falling within the 95% confidence limits as determined by the mathematical model.

Oxborrow, G. S.↗
NASA NTRS2014

Estimating Major Ion and Nutrient Concentrations in Mangrove Estuaries in Everglades National Park Using Leaf and Satellite Reflectance

Coastal mangrove ecosystems are under duress worldwide because of urban development, sea-level rise, and climate change, processes that are capable of changing the salinity and nutrient concentration of the water utilized by the mangroves. This study correlates long-term water chemistry in mangrove environments, located in Everglades National Park,with mangrove spectral reflectance measurements made at both the leaf and canopy scales. Spectral reflectance measurements were collected using a handheld spectrometer for leaf-level measurements and Landsat 5TMdata for regional coverage. Leaf-level reflectance data were collected from three mangrove species (i.e., red, black and white mangroves) across two regions; a tall mangrove (approximately 18m) and dwarf mangrove (1- 2 m) region. The reflectance data were then used to calculate a wide variety of biophysical reflectance indices (e.g., NDVI, EVI, SAVI) to determine signs of stress. Discrete, quarterly water samples from the surface water, groundwater, and pore water (20 and 85 cm depths) and daily autonomous surface water samples were collected at each site and analyzed for major anions (Cl(−) and SO(2(-)/4)), cations (Na(+), K(+), Mg(sup 2(+)), and Ca(sup 2(+)), total nitrogen (TN) and total phosphorus (TP).Mangrove sites that exhibited the highest salinity and ionic concentrations in the surface and subsurface water also had the lowest near-infrared reflectance at both the leaf and satellite levels. Seasonal reflectance responses were measured in the near-infrared (NIR) wavelengths at both the leaf and canopy scales and were strongly correlated with nutrient and ionic concentrations in the surface and subsurface water, even though there was no significant separability between the three mangrove species. Study sites that experienced the greatest variability in surface and subsurface water ionic concentrations also exhibited the greatest fluctuations in NIR spectral reflectance. Landsat 5TM images were able to detect tall and dwarf mangroves by the differences in spectral indices (e.g., NDVI, NDWI, and EVI) because of the variability in the background conditions amongst the environments. In addition, Landsat 5TM images spanning 16 years (1993- 2009) were successfully used to estimate the seasonal variability in ionic concentrations in the surface water across the Florida Coastal mangrove ecotone. This study has shown that water chemistry can be estimated indirectly by measuring the change in spectral response at the leaf- or satellite-scale. Furthermore, the results of this research may be extrapolated to similar coastal mangrove systems throughout the Caribbean and world-wide wherever red, black, and white mangroves occur.

Mangroves↗
DOE OSTI2016

Effect of surface nanostructuring on corrosion behavior of Ti–6Al–4V alloy

Surface nanostructure was induced in Ti–6Al–4V alloy by ultrasonic shot peening (USSP) for different durations, from 15 s to 30 min, and the modified surface was characterized by optical, scanning, atomic force and transmission electron microscopy. Nano size grains were observed to form on surface of the USSPed samples and surface roughness was increased with duration of USSP. Polarization study was carried out in Ringer's solution to examine the effect of surface nanostructuring on corrosion resistance of this alloy. Electrochemical corrosion was carried out for all the USSPed specimens as well as the non-USSPed sample in Ringer's solution. Surface morphology of the corroded samples was examined by SEM. In general, corrosion resistance was improved by USSP up to the duration of 15 min and there was maximum improvement in the specimen USSPed for 1 min. However, corrosion resistance was drastically reduced due to USSP for long duration of 30 min. - Highlights: •Nanostructure was induced by USSP on alloy Ti–6Al–4V of about 28 nm. •Grain refinement was confirmed by XRD and TEM. •USSP is an effective technique for the improvement in corrosion resistance. •Nanostructured surface promotes formation of protective surface layer of TiO{sub 2}.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Results of Hg speciation testing on tank 39 and 1Q16 tank 50 samples

The Savannah River National Laboratory (SRNL) was tasked with preparing and shipping samples for Hg speciation by Eurofins Frontier Global Sciences, Inc. in Seattle, WA on behalf of the Savannah River Remediation (SRR) Mercury Task Team.i,ii The seventeenth shipment of samples was designated to include two Tank 39 samples and the 1Q16 Tank 50 Quarterly WAC sample. The surface Tank 39 sample was pulled at 262.1” from the tank bottom, and the depth Tank 39 sample was pulled at 95” from the tank bottom. The 1Q16 Tank 50 WAC sample was drawn from the 1-L variable depth sample received by SRNL.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
NASA NTRS1980

Titan probe technology assessment and technology development plan study

The need for technology advances to accomplish the Titan probe mission was determined by defining mission conditions and requirements and evaluating the technology impact on the baseline probe configuration. Mission characteristics found to be technology drivers include (1) ten years dormant life in space vacuum; (2) unknown surface conditions, various sample materials, and a surface temperature; and (3) mission constraints of the Saturn Orbiter Dual Probe mission regarding weight allocation. The following areas were identified for further development: surface sample acquisition system; battery powered system; nonmetallic materials; magnetic bubble memory devices, and the landing system. Preentry science, reliability, and weight reduction and redundancy must also be considered.

Castro, A. J.↗
NASA NTRS2004

Samples of Asteroid Surface Ponded Deposits in Chondritic Meteorites

One of the many unexpected observations of asteroid 433 Eros by the Near Earth Asteroid Rendezvous (NEAR) mission was the many ponds of fine-grained materials [1-3]. The ponds have smooth surfaces, and define equipotential surfaces up to 10's of meters in diameter [4]. The ponds have a uniformly sub-cm grain size and appear to be cohesive or indurated to some degree, as revealed by slumping. The ponds appear to be concentrated within 30 degrees of the equator of Eros, where gravity is lowest. There is some insight into the mineralogy and composition of the ponds surfaces from NEAR spectroscopy [2,4,5,6]. Compared to the bulk asteroid, ponds: (1) are distinctly bluer (high 550/760 nm ratio), (2) have a deeper 1um mafic band, (3) have reflectance elevated by 5%.

Zolensky, M. E.↗
NASA NTRS2014

Microbiology and Crew Medical Events on the International Space Station

The closed environment of the International Space Station (ISS) creates an ideal environment for microbial growth. Previous studies have identified the ubiquitous nature of microorganisms throughout the space station environment. To ensure safety of the crew, microbial monitoring of air and surface within ISS began in December 2000 and continues to be monitored on a quarterly basis. Water monitoring began in 2009 when the potable water dispenser was installed on ISS. However, it is unknown if high microbial counts are associated with inflight medical events. The microbial counts are determined for the air, surface, and water samples collected during flight operations and samples are returned to the Microbiology laboratory at the Johnson Space Center for identification. Instances of microbial counts above the established microbial limit requirements were noted and compared inflight medical events (any non-injury event such as illness, rashes, etc.) that were reported during the same calendar-quarter. Data were analyzed using repeated measures logistic regression for the forty-one US astronauts flew on ISS between 2000 and 2012. In that time frame, instances of microbial counts being above established limits were found for 10 times for air samples, 22 times for surface samples and twice for water. Seventy-eight inflight medical events were reported among the astronauts. A three times greater risk of a medical event was found when microbial samples were found to be high (OR = 3.01; p =.007). Engineering controls, crew training, and strict microbial limits have been established to mitigate the crew medical events and environmental risks. Due to the timing issues of sampling and the samples return to earth, identification of particular microorganisms causing a particular inflight medical event is difficult. Further analyses are underway.

Oubre, Cherie↗