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NASA NTRS2009

Modern Material Analysis Instruments Add a New Dimension to Materials Characterization and Failure Analysis

Modern analytical tools can yield invaluable results during materials characterization and failure analysis. Scanning electron microscopes (SEMs) provide significant analytical capabilities, including angstrom-level resolution. These systems can be equipped with a silicon drift detector (SDD) for very fast yet precise analytical mapping of phases, as well as electron back-scattered diffraction (EBSD) units to map grain orientations, chambers that admit large samples, variable pressure for wet samples, and quantitative analysis software to examine phases. Advanced solid-state electronics have also improved surface and bulk analysis instruments: Secondary ion mass spectroscopy (SIMS) can quantitatively determine and map light elements such as hydrogen, lithium, and boron - with their isotopes. Its high sensitivity detects impurities at parts per billion (ppb) levels. X-ray photo-electron spectroscopy (XPS) can determine oxidation states of elements, as well as identifying polymers and measuring film thicknesses on coated composites. This technique is also known as electron spectroscopy for chemical analysis (ESCA). Scanning Auger electron spectroscopy (SAM) combines surface sensitivity, spatial lateral resolution (10 nm), and depth profiling capabilities to describe elemental compositions of near and below surface regions down to the chemical state of an atom.

Panda, Binayak↗
NASA NTRS2000

Growth and Morphology of Supercritical Fluids Studied in Microgravity on Mir

The Growth and Morphology of Supercritical Fluids (GMSF) is an international experiment facilitated by the NASA Glenn Research Center at Lewis Field and under the guidance of U.S. principal investigator Professor John Hegseth of the University of New Orleans and three French coinvestigators Daniel Beysens, Yves Garrabos, and Carole Chabot. In early 1999, GMSF experiments were operated for 20 days on the Russian Space Station Mir. Mir astronauts performed experiments One through Seven, which spanned the three science themes of near-critical phase separation rates, interface dynamics in near-critical boiling, and measurement of the spectrum of density fluctuation length scales very close to the critical point. The fluids used were pure CO2 or SF6. Three of the five thermostats used could adjust the sample volume with the scheduled crew time. Such a volume adjustment enabled variable sample densities around the critical density as well as pressure steps (as distinct from the usual temperature steps) to be applied to the sample.

Wilkinson, R. Allen↗
NASA NTRS2001

Growth and Morphology of Supercritical Fluids, a Fluid Physics Experiment Conducted on Mir, Complete

The Growth and Morphology of Supercritical Fluids (GMSF) is an international experiment facilitated by the NASA Glenn Research Center and under the guidance of U.S. principal investor Professor Hegseth of the University of New Orleans and three French coinvestigators: Daniel Beysens, Yves Garrabos, and Carole Chabot. The GMSF experiments were concluded in early 1999 on the Russian space station Mir. The experiments spanned the three science themes of near-critical phase separation rates, interface dynamics in near-critical boiling, and measurement of the spectrum of density fluctuation length scales very close to the critical point. The fluids used were pure CO2 or SF6. Three of the five thermostats used could adjust the sample volume with the scheduled crew time. Such a volume adjustment enabled variable sample densities around the critical density as well as pressure steps (as distinct from the usual temperature steps) applied to the sample. The French-built ALICE II facility was used for these experiments. It allows tightly thermostated (left photograph) samples (right photograph) to be controlled and viewed/measured. Its diagnostics include interferometry, shadowgraph, high-speed pressure measurements, and microscopy. Data were logged on DAT tapes, and PCMCIA cards and were returned to Earth only after the mission was over. The ground-breaking near critical boiling experiment has yielded the most results with a paper published in Physical Review Letters (ref. 1). The boiling work also received press in Science Magazine (ref. 2). This work showed that, in very compressible near-critical two-phase pure fluids, a vapor bubble was induced to temporarily overheat during a rapid heating of the sample wall. The temperature rise in the vapor was 23-percent higher than the rise in the driving container wall. The effect is due to adiabatic compression of the vapor bubble by the rapid expansion of fluid near the boundary during heatup. Thermal diffusivity is low near the critical point, so getting heat out of the compressed bubble is observably slow. This gives the appearance of a backward heat flow, or heat flow from a cold surface to a warm fluid.

Wilkinson, R. Allen↗
NASA NTRS2018

Chlorine Isotopic Compositions of Apatite in Apollo 14 Rocks: Evidence for Widespread Vapor-Phase Metasomatism on the Lunar Nearside ~4 Billion Years Ago

Compared to most other planetary materials in the Solar System, some lunar rocks display high delta (sup 37) Cl signatures. Loss of Cl in a H<<Cl environment has been invoked to explain the heavy signatures observed in lunar samples, either during volcanic eruptions onto the lunar surface or during large scale degassing of the lunar magma ocean. To explore the conditions under which Cl isotope fractionation occurred in lunar basaltic melts, five Apollo 14 crystalline samples were selected (14053,19, 14072,13, 14073,9, 14310,171 along with basaltic clast 14321,1482) for in situ analysis of Cl isotopes using secondary ion mass spectrometry. Cl isotopes were measured within the mineral apatite, with delta (sup 37) Cl values ranging from +14.6 ± 1.6 per mille to +40.0 ± 2.9 per mille. These values expand the range previously reported for apatite in lunar rocks, and include some of the heaviest Cl isotope compositions measured in lunar samples to date. The data here do not display a trend between increasing rare earth elements contents and delta (sup 37) Cl values, reported in previous studies. Other processes that can explain the wide inter- and intra-sample variability of delta (sup 37) Cl values are explored. Magmatic degassing is suggested to have potentially played a role in fractionating Cl isotope in these samples. Degassing alone, however, could not create the wide variability in isotopic signatures. Our favored hypothesis, to explain small scale heterogeneity, is late-stage interaction with a volatile-rich gas phase, originating from devolatilization of lunar surface regolith rocks ~4 billion years ago. This period coincides with vapor-induced metasomastism recorded in other lunar samples collected at the Apollo 16 and 17 landing sites, pointing to the possibility of widespread volatile-induced metasomatism on the lunar nearside at that time, potentially attributed to the Imbrium formation event.

apatit↗
NASA NTRS1976

Electrophoresis experiment, experiment MA-014

A continuous, free flow electrophoresis study was conducted during the Apollo Soyuz Test Project mission to investigate and evaluate the increase in sample flow rate and sample resolution achievable in space. The electrophoresis equipment was designed for the separation of four mixtures of biological cells with variable sample flow rates, buffer flow rates, and electric field gradients. Separation quality was assessed by measuring the light from a quartz lamp through the electrophoresis channel and on to a photodiode system. The preliminary results indicate that all monitored systems operated correctly during the experiment. The optical system produced a light that was too bright to discern true cell distributions, but data were received that show a distribution of separated cells.

Hannig, K.↗
NASA NTRS1977

Electrophoresis experiment. Experiment MA-014

A continuous free-flow electrophoresis study was conducted during the Apollo-Soyuz Test Project Mission to investigate and evaluate the increase in sample flow rate and sample resolution achievable in space. The electrophoresis equipment was designed for the separation of four mixtures of biological cells with variable sample flow rates, buffer flow rates, and electric field gradients. Separation quality was assessed by measuring the light from a quartz lamp through the electrophoresis channel and onto a photodiode system. The data evaluation indicates that all monitored systems operated correctly during the experiment. The optical system produced a light that was too bright to discern true cell distributions, but final analysis of scientific data by computer processing shows the expected distribution of separated cells.

Hannig, K. H.↗
NASA NTRS2017

NASA-STD-6001B Test 1 Upward Flame Propagation; Sample Length Impact on MOC Investigation

Understanding the combustion behavior of materials in the elevated oxygen environments of habitable spacecraft is of utmost importance to crew safety and mission success. Currently, certification for unrestricted flight usage of a material with respect to flammability involves passing the Upward Flame Propagation Test of NASA-STD-6001B (Test 1). This test evaluates materials in a standardized test configuration for two failure criteria: self-extinguishment within 15 cm (6 in.) and the propensity of flame propagation by means of flaming material transfer. By the NASA standard, full-length samples are 30 cm (12 in.) in length; however, factors independent of the test method such as limited material availability or various nonstandard test configurations limit the full pretest sample lengths available for test. This paper characterizes the dependence, if any, of pretest sample length on NASA-STD-6001B Test 1 results. Testing was performed using the Maximum Oxygen Concentration (MOC) Threshold Method to obtain a data set for each sample length tested. In addition, various material types, including cloth (Nomex), foam (TA-301) and solids (Ultem), were tested to investigate potential effects of test specimen types. Though additional data needs to be generated to provide statistical confidence, preliminary findings are that use of variable sample lengths has minimal impact on NASA-STD-6001B flammability performance and MOC determination.

Harper, Susana Tapia↗
NASA NTRS2013

Comparison of Precision of Biomass Estimates in Regional Field Sample Surveys and Airborne LiDAR-Assisted Surveys in Hedmark County, Norway

Airborne scanning LiDAR (Light Detection and Ranging) has emerged as a promising tool to provide auxiliary data for sample surveys aiming at estimation of above-ground tree biomass (AGB), with potential applications in REDD forest monitoring. For larger geographical regions such as counties, states or nations, it is not feasible to collect airborne LiDAR data continuously ("wall-to-wall") over the entire area of interest. Two-stage cluster survey designs have therefore been demonstrated by which LiDAR data are collected along selected individual flight-lines treated as clusters and with ground plots sampled along these LiDAR swaths. Recently, analytical AGB estimators and associated variance estimators that quantify the sampling variability have been proposed. Empirical studies employing these estimators have shown a seemingly equal or even larger uncertainty of the AGB estimates obtained with extensive use of LiDAR data to support the estimation as compared to pure field-based estimates employing estimators appropriate under simple random sampling (SRS). However, comparison of uncertainty estimates under SRS and sophisticated two-stage designs is complicated by large differences in the designs and assumptions. In this study, probability-based principles to estimation and inference were followed. We assumed designs of a field sample and a LiDAR-assisted survey of Hedmark County (HC) (27,390 km2), Norway, considered to be more comparable than those assumed in previous studies. The field sample consisted of 659 systematically distributed National Forest Inventory (NFI) plots and the airborne scanning LiDAR data were collected along 53 parallel flight-lines flown over the NFI plots. We compared AGB estimates based on the field survey only assuming SRS against corresponding estimates assuming two-phase (double) sampling with LiDAR and employing model-assisted estimators. We also compared AGB estimates based on the field survey only assuming two-stage sampling (the NFI plots being grouped in clusters) against corresponding estimates assuming two-stage sampling with the LiDAR and employing model-assisted estimators. For each of the two comparisons, the standard errors of the AGB estimates were consistently lower for the LiDAR-assisted designs. The overall reduction of the standard errors in the LiDAR-assisted estimation was around 40-60% compared to the pure field survey. We conclude that the previously proposed two-stage model-assisted estimators are inappropriate for surveys with unequal lengths of the LiDAR flight-lines and new estimators are needed. Some options for design of LiDAR-assisted sample surveys under REDD are also discussed, which capitalize on the flexibility offered when the field survey is designed as an integrated part of the overall survey design as opposed to previous LiDAR-assisted sample surveys in the boreal and temperate zones which have been restricted by the current design of an existing NFI.

Comparison↗
NASA NTRS2020

Precision Assessment of the HPLC Phytoplankton Pigment Dataset Analyzed by NASA to Quantify Global Variability in Support of Ocean Color Remote Sensing

The ability to generate chlorophyll a (Chl a) assessments from ocean color orbital sensors, such as VIIRS and MODIS, that satisfy the requirements to be climate-quality data record (CDR) quality is contingent in part on the quality of the in situ ground or sea truth observations that serve as datasets for vicarious calibration and algorithm validation activities. NASA has a mandate to collect, analyze, and distribute in situ data of the highest possible quality with documented uncertainties and in keeping with established performance metrics. Using a dataset of over 18,000 HPLC phytoplankton pigment samples representing water collected in all major ocean basins analyzed a central laboratory (Field Support Group (FSG) of the Ocean Ecology Laboratory (OEL) at NASA Goddard Space Flight Center (GSFC)), we performed an assessment of the global precision among sample replicates of Chl a as well as major accessory pigments. We investigated the impacts of filtration volume, water basin, collection technique, pigment concentration, and different filtration volumes for replicate filters on replicate filter precision, as well as investigating any pigment-specific differences. Our results quantify sample variability with the goal of understanding any systemic biases or biogeographic influences.

Thomas, Crystal S.↗
NASA NTRS2012

NASA Tech Briefs, February 2012

This issue contains the following briefs: (1) Optical Comb from a Whispering Gallery Mode Resonator for Spectroscopy and Astronomy Instruments Calibration (2) Real-Time Flight Envelope Monitoring System (3) Nemesis Autonomous Test System (4) Mirror Metrology Using Nano-Probe Supports (5) Automated Lab-on-a-Chip Electrophoresis System (6) Techniques for Down-Sampling a Measured Surface Height Map for Model Validation (7) Multi-Component, Multi-Point Interferometric Rayleigh/Mie Doppler Velocimeter (8) Frequency to Voltage Converter Analog Front-End Prototype (9) Dust-Tolerant Intelligent Electrical Connection System (10) Gigabit Ethernet Asynchronous Clock Compensation FIFO (11) High-Speed, Multi-Channel Serial ADC LVDS Interface for Xilinx Virtex-5 FPGA (12) Glovebox for GeoLab Subsystem in HDU1-PEM (13) Modified Process Reduces Porosity when Soldering in Reduced Gravity Environments (14) Use of Functionalized Carbon Nanotubes for Covalent Attachment of Nanotubes to Silicon (15) Flexible Plug Repair for Shuttle Wing Leading Edge (16) Three Dimensionally Interlinked, Dense, Solid Form of Single-Walled CNT Ropes (17) Axel Robotic Platform for Crater and Extreme Terrain Exploration (18) Site Tamper and Material Plow Tool - STAMP (19) Magnetic Interface for Segmented Mirror Assembly (20) Transpiration-Cooled Spacecraft-Insulation-Repair Fasteners (21) Fluorescence-Based Sensor for Monitoring Activation of Lunar Dust (22) Aperture Ion Source (23) Virtual Ultrasound Guidance for Inexperienced Operators (24) Model-Based Fault Diagnosis: Performing Root Cause and Impact Analyses in Real Time (25) Interactive Schematic Integration Within the Propellant System Modeling Environment (26) Magnetic and Electric Field Polarizations of Oblique Magnetospheric Chorus Waves (27) Variable Sampling Mapping.

Source record↗
NASA NTRS1992

Dependence of Wave-Breaking Statistics on Wind Stress and Wave Development

Incidence of wave breaking for pure wind driven waves has been studied on Lake Washington at wind speeds up to 8 m/s. Video recordings were employed to identify and categorize the breaking events in terms of micro-scale, spilling and plunging breakers. These events were correlated with the magnitude of the wave spectrum measured with a resistance wire wave gauge and band pass filtered between 6 and 10 Hz. An equivalent percentage of breaking crests were found for spilling and plunging events. Wave forcing as measured by wind stress (or friction velocity, u(sub *), squared) and by inverse wave age, u(sub *)/Cp where Cp is the phase velocity of the waves at the peak of the frequency spectrum, were found to be good prerictors of percentage of breaking crests. When combined in a two parameter regression, those two variables gave small standard deviation and had a high correlation coefficient (66 percent). The combination of u(sub *)(exp 2) and u(sub *)/Cp can be understood in physical terms. Furthermore, for the larger values of u(sub *)(exp 2) the dependence of wave braking and wave age was stronger than at the low end of the values u(sub *)(exp 2) and u(sub *)/Cp. Thus, both the level of wave development as determined by inverse wave age, which we may term relative wind effectiveness for wave forcing and the wind forcing on the water surface determine the incidence of wave breaking. Substituting U(sub 10)(sup 3.75) (which is the dependence of whitecap cover found by Monahan and coworkers) an equivalent correlation was found to the prediction by u(sub *)(exp 2). Slightly better standard deviation value and higher correlation coefficient were found by using a Reynolds number as predictor. A two-parameter regression involving u(sub *)(exp 2) and a Reynold's number proposed by Toba and his colleagues which relates u(sub *)(exp 2) and peak wave frequency, improves the correlation even more but is less easy to interpret in physical terms. The equivalent percentage of breaking crests obtained in our previous study was reported at 8.6 percent for a short record obtained at U(sub 10N) of about 6 m/s. Typical values in the current study for similar conditions are 6 percent, which is consistent with the previous study in view of the scatter. In that study we did not have a video recording system, so the observed breaking may include more of the micro-scaic breaking events, and the value, 8.6 percent, is well within the range of highly probable sampling variability.

Katsaros, Kristina B.↗
NASA NTRS2016

Lidar-Based Estimates of Above-Ground Biomass in the Continental US and Mexico Using Ground, Airborne, and Satellite Observations

Existing national forest inventory plots, an airborne lidar scanning (ALS) system, and a space profiling lidar system (ICESat-GLAS) are used to generate circa 2005 estimates of total aboveground dry biomass (AGB) in forest strata, by state, in the continental United States (CONUS) and Mexico. The airborne lidar is used to link ground observations of AGB to space lidar measurements. Two sets of models are generated, the first relating ground estimates of AGB to airborne laser scanning (ALS) measurements and the second set relating ALS estimates of AGB (generated using the first model set) to GLAS measurements. GLAS then, is used as a sampling tool within a hybrid estimation framework to generate stratum-, state-, and national-level AGB estimates. A two-phase variance estimator is employed to quantify GLAS sampling variability and, additively, ALS-GLAS model variability in this current, three-phase (ground-ALS-space lidar) study. The model variance component characterizes the variability of the regression coefficients used to predict ALS-based estimates of biomass as a function of GLAS measurements. Three different types of predictive models are considered in CONUS to determine which produced biomass totals closest to ground-based national forest inventory estimates - (1) linear (LIN), (2) linear-no-intercept (LNI), and (3) log-linear. For CONUS at the national level, the GLAS LNI model estimate (23.95 +/- 0.45 Gt AGB), agreed most closely with the US national forest inventory ground estimate, 24.17 +/- 0.06 Gt, i.e., within 1%. The national biomass total based on linear ground-ALS and ALS-GLAS models (25.87 +/- 0.49 Gt) overestimated the national ground-based estimate by 7.5%. The comparable log-linear model result (63.29 +/-1.36 Gt) overestimated ground results by 261%. All three national biomass GLAS estimates, LIN, LNI, and log-linear, are based on 241,718 pulses collected on 230 orbits. The US national forest inventory (ground) estimates are based on 119,414 ground plots. At the US state level, the average absolute value of the deviation of LNI GLAS estimates from the comparable ground estimate of total biomass was 18.8% (range: Oregon,−40.8% to North Dakota, 128.6%). Log-linear models produced gross overestimates in the continental US, i.e., N2.6x, and the use of this model to predict regional biomass using GLAS data in temperate, western hemisphere forests is not appropriate. The best model form, LNI, is used to produce biomass estimates in Mexico. The average biomass density in Mexican forests is 53.10 +/- 0.88 t/ha, and the total biomass for the country, given a total forest area of 688,096 sq km, is 3.65 +/- 0.06 Gt. In Mexico, our GLAS biomass total underestimated a 2005 FAO estimate (4.152 Gt) by 12% and overestimated a 2007/8 radar study's figure (3.06 Gt) by 19%.

Hybrid 3-Phase sampling↗
NASA NTRS1979

An evaluation of several different classification schemes - Their parameters and performance

The overall objective of this study was to apply and evaluate several of the currently available classification schemes for crop identification. The approaches examined were: (1) a per point Gaussian maximum likelihood classifier, (2) a per point sum of normal densities classifier, (3) a per point linear classifier, (4) a per point Gaussian maximum likelihood decision tree classifier, and (5) a texture sensitive per field Gaussian maximum likelihood classifier. Three agricultural data sets were used in the study: areas from Fayette County, Illinois, and Pottawattamie and Shelby Counties in Iowa. The segments were located in two distinct regions of the Corn Belt to sample variability in soils, climate, and agricultural practices.

Scholz, D.↗
NASA NTRS1979

Multistage variable probability forest volume inventory

The net board foot volume (Scribner log rule) of the standing Ponderosa pine timber on the Defiance Unit of the Navajo Nation's forested land was estimated using a multistage forest volume inventory scheme with variable sample selection probabilities. The inventory designed to accomplish this task required that both LANDSAT MSS digital data and aircraft acquired data be used to locate one acre ground splits, which were subsequently visited by ground teams conducting detailed tree measurements using an optical dendrometer. The dendrometer measurements were then punched on computer input cards and were entered in a computer program developed by the U.S. Forest Service. The resulting individual tree volume estimates were then expanded through the use of a statistically defined equation to produce the volume estimate for the entire area which includes 192,026 acres and is approximately a 44% the total forested area of the Navajo Nation.

Anderson, J. E.↗
NASA NTRS1982

Analysis and interpretation of Viking inorganic chemistry data (Mars data analysis program)

Soil samples gathered by the Viking Lander from the surface of Mars were analyzed. The Martian fines were lower in aluminum, iron, sulfur, and chlorine than typical terrestrial continental soils or lunar mare fines. Sample variabilities were as great within a few meters as between lander locations (4500 km apart) implying the existence of a universal Martian regolith component of constant average composition.

Clark, B. C.↗
NASA NTRS1982

Chemical composition of Martian fines

Of the 21 samples acquired for the Viking X-ray fluorescence spectrometer, 17 were analyzed to high precision. Compared to typical terrestrial continental soils and lunar mare fines, the Martian fines are lower in Al, higher in Fe, and much higher in S and Cl concentrations. Protected fines at the two lander sites are almost indistinguishable, but concentration of the element S is somewhat higher at Utopia. Duricrust fragments, successfully acquired only at the Chryse site, invariably contained about 50% higher S than fines. No elements correlate positively with S, except Cl and possibly Mg. A sympathetic variation is found among the triad Si, Al, Ca; positive correlation occurs between Ti and Fe. Sample variabilities are as great within a few meters as between lander locations (4500 km apart), implying the existence of a universal Martian regolith component of constant average composition. The nature of the source materials for the regolith fines must be mafic to ultramafic.

Clark, B. C.↗
NASA NTRS1989

Probabilities and statistics for backscatter estimates obtained by a scatterometer

Methods for the recovery of winds near the surface of the ocean from measurements of the normalized radar backscattering cross section must recognize and make use of the statistics (i.e., the sampling variability) of the backscatter measurements. Radar backscatter values from a scatterometer are random variables with expected values given by a model. A model relates backscatter to properties of the waves on the ocean, which are in turn generated by the winds in the atmospheric marine boundary layer. The effective wind speed and direction at a known height for a neutrally stratified atmosphere are the values to be recovered from the model. The probability density function for the backscatter values is a normal probability distribution with the notable feature that the variance is a known function of the expected value. The sources of signal variability, the effects of this variability on the wind speed estimation, and criteria for the acceptance or rejection of models are discussed. A modified maximum likelihood method for estimating wind vectors is described. Ways to make corrections for the kinds of errors found for the Seasat SASS model function are described, and applications to a new scatterometer are given.

Pierson, Willard J., Jr.↗