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All sourcesNASA NTRSDOE OSTI
NASA NTRS2015

Sample Acquisition and Analytical Chemistry Challenges to Verifying Compliance to Aviators Breathing Oxygen (ABO) Purity Specification

NASA has been developing and testing two different types of oxygen separation systems. One type of oxygen separation system uses pressure swing technology, the other type uses a solid electrolyte electrochemical oxygen separation cell. Both development systems have been subjected to long term testing, and performance testing under a variety of environmental and operational conditions. Testing these two systems revealed that measuring the product purity of oxygen, and determining if an oxygen separation device meets Aviator's Breathing Oxygen (ABO) specifications is a subtle and sometimes difficult analytical chemistry job. Verifying product purity of cryogenically produced oxygen presents a different set of analytical chemistry challenges. This presentation will describe some of the sample acquisition and analytical chemistry challenges presented by verifying oxygen produced by an oxygen separator - and verifying oxygen produced by cryogenic separation processes. The primary contaminant that causes gas samples to fail to meet ABO requirements is water. The maximum amount of water vapor allowed is 7 ppmv. The principal challenge of verifying oxygen produced by an oxygen separator is that it is produced relatively slowly, and at comparatively low temperatures. A short term failure that occurs for just a few minutes in the course of a 1 week run could cause an entire tank to be rejected. Continuous monitoring of oxygen purity and water vapor could identify problems as soon as they occur. Long term oxygen separator tests were instrumented with an oxygen analyzer and with an hygrometer: a GE Moisture Monitor Series 35. This hygrometer uses an aluminum oxide sensor. The user's manual does not report this, but long term exposure to pure oxygen causes the aluminum oxide sensor head to bias dry. Oxygen product that exceeded the 7 ppm specification was improperly accepted, because the sensor had biased. The bias is permanent - exposure to air does not cause the sensor to return to its original response - but the bias can be accounted for by recalibrating the sensor. After this issue was found, continuous measurements of water vapor in the oxygen product were made using an FTIR. The FTIR cell is relatively large, so response time is slow - but moisture measurements were repeatable and accurate. Verifying ABO compliance for oxygen produced by commercial cryogenic processes has a different set of sample acquisition and analytical chemistry challenges. Customers want analytical chemists to conserve as much as possible. Hygrometers are not exposed to hours of continuous flow of oxygen, so they don't bias, but small amounts of contamination in valves can cause a "fail". K bottles are periodically cleaned and recertified - after cleaning residual moisture can cause a "fail". Operators let bottle pressure drop to room pressure, introduce outside air into the bottle, and the subsequent fill will "fail". Outside storage of K‐bottles has allowed enough in‐leakage, so contents will "fail".

Graf, John↗
NASA NTRS2003

Solar Array in Simulated LEO Plasma Environment

Six different types of solar arrays have been tested in large vacuum chambers. The low earth orbit plasma environment was simulated in plasma vacuum chambers, where the parameters could be controlled precisely. Diagnostic equipment included spherical Langmuir probes, mass spectrometer, low-noise CCD camera with optical spectrometer, video camera, very sensitive current probe to measure arc current, and a voltage probe to register variations in a conductor potential. All data (except video) were obtained in digital form that allowed us to study the correlation between external parameters (plasma density, additional capacitance, bias voltage, etc) and arc characteristics (arc rate, arc current pulse width and amplitude, gas species partial pressures, and intensities of spectral lines). Arc inception voltages, arc rates, and current selections are measured for samples with different coverglass materials and thickness, interconnect designs, and cell sizes. It is shown that the array with wrapthrough interconnects have the highest arc threshold and the lowest current collection. Coverglass design with overhang results in decrease of current collection and increase of arc threshold. Doubling coverglass thickness cases the increase in arc inception voltage. Both arc inception voltage and current collection increase significantly with increasing a sample temperature to 80 C. Sustained discharges are initiated between adjacent cells with potential differences of 40 V for the sample with 300 micron coverglass thickness and 60 V for the sample with 150 micron coverglass thickness. Installation of cryogenic pump in large vacuum chamber provided the possibility of considerable outgassing of array surfaces which resulted in significant decrease of arc rate. Arc sites were determined by employing a video-camera, and it is shown that the most probable sites for arc inception are triple-junctions, even though some arcs were initiated in gaps between cells. It is also shown that the arc rate increases with increasing of ion collection current. The analysis of optical spectra (240-800 nm) reveals intensive narrow atomic lines (Ag, H) and wide molecular bands (OH, CH, SiH, SiN) that confirms a complicated mechanism of arc plasma generation. The results obtained seem to be important for the understanding of the arc inception mechanism, which is absolutely essential for progress toward the design of high-voltage solar array for space application.

Vayner, Boris↗
NASA NTRS2004

Solar Array in Simulated LEO Plasma Environment

Six different types of solar arrays have been tested in large vacuum chambers. The low Earth orbit plasma environment was simulated in plasma vacuum chambers, where the parameters could be controlled precisely. Diagnostic equipment included spherical Langmuir probes, mass spectrometer, low-noise CCD camera with optical spectrometer, video camera, very sensitive current probe to measure arc current, and a voltage probe to register variations in a conductor potential. All data (except video) were obtained in digital form that allowed us to study the correlation between external parameters (plasma density, additional capacitance, bias voltage, etc) and arc characteristics (arc rate, arc current pulse width and amplitude, gas species partial pressures, and intensities of spectral lines). Arc inception voltages, arc rates, and current collections are measured for samples with different coverglass materials and thickness, interconnect designs, and cell sizes. It is shown that the array with wrapthrough interconnects have the highest arc threshold and the lowest current collection. Coverglass design with overhang results in decrease of current collection and increase of arc threshold. Doubling coverglass thickness causes the increase in arc inception voltage. Both arc inception voltage and current collection increase significantly with increasing a sample temperature to 80 C. Sustained discharges are initiated between adjacent cells with potential differences of 40 V for the sample with 300 m coverglass thickness and 60 V for the sample with 150 m coverglass thickness. Installation of cryogenic pump in large vacuum chamber provided the possibility of considerable outgassing of array surfaces which resulted in significant decrease of arc rate. Arc sites were determined by employing a video-camera, and it is shown that the most probable sites for arc inception are triple-junctions, even though some arcs were initiated in gaps between cells. It is also shown that the arc rate increases with increasing of ion collection current. The analysis of optical spectra (240-800 nm) reveals intensive narrow atomic lines (Ag, H) and wide molecular bands (OH, CH, SiH, SiN) that confirms a complicated mechanism of arc plasma generation. The results obtained seem to be important for the understanding of the arc inception mechanism, which is absolutely essential for progress toward the design of high-voltage solar array for space application.

Vayner, Boris↗
NASA NTRS1977

Analysis of volatile organic compounds

An apparatus and method are described for reproducibly analyzing trace amounts of a large number of organic volatiles existing in a gas sample. Direct injection of the trapped volatiles into a cryogenic percolum provides a sharply defined plug. Applications of the method include: (1) analyzing the headspace gas of body fluids and comparing a profile of the organic volatiles with standard profiles for the detection and monitoring of disease; (2) analyzing the headspace gas of foods and beverages and comparing the profile with standard profiles to monitor and control flavor and aroma; and (3) analyses for determining the organic pollutants in air or water samples.

Zlatkis, A.↗
NASA NTRS2015

Impact of Drilling Operations on Lunar Volatiles Capture: Thermal Vacuum Tests

In Situ Resource Utilization (ISRU) enables future planetary exploration by using local resources to supply mission consumables. This idea of 'living off the land' has the potential to reduce mission cost and risk. On the moon, water has been identified as a potential resource (for life support or propellant) at the lunar poles, where it exists as ice in the subsurface. However, the depth and content of this resource has yet to be confirmed on the ground; only remote detection data exists. The upcoming Resource Prospector mission (RP) will 'ground-truth' the water using a rover, drill, and the RESOLVE science package. As the 2020 planned mission date nears, component level hardware is being tested in relevant lunar conditions (thermal vacuum). In August 2014 a series of drilling tests were performed using the Honeybee Robotics Lunar Prospecting Drill inside a 'dirty' thermal vacuum chamber at the NASA Glenn Research Center. The drill used a unique auger design to capture and retain the lunar regolith simulant. The goal of these tests was to investigate volatiles (water) loss during drilling and sample transfer to a sample crucible in order to validate this regolith sampling method. Twelve soil samples were captured over the course of two tests at pressures of 10(exp-5) Torr and ambient temperatures between -80C to -20C. Each sample was obtained from a depth of 40 cm to 50 cm within a cryogenically frozen bed of NU-LHT-3M lunar regolith simulant doped with 5 wt% water. Upon acquisition, each sample was transferred and hermetically sealed inside a crucible. The samples were later baked out to determine water wt% and in turn volatile loss by following ASTM standard practices. Of the twelve tests, four sealed properly and lost an average of 30% of their available water during drilling and transfer. The variability in the results correlated well with ambient temperature (lower the temperature lower volatiles loss) and the trend agreed with the sublimation rates for the same temperature. Moisture retention also correlated with quantity of sample: a larger amount of material resulted in less water loss. The drilling process took an average of 10 minutes to capture and transfer each sample. The drilling power was approximately 20 Watt with a Weight on Bit of approximately 30 N. The bit temperature indicated little heat input into formation during the drilling process.

drilling↗
NASA NTRS2008

Thermal Performance of Aged and Weathered Spray-On Foam Insulation (SOFI) Materials Under Cryogenic Vacuum Conditions (Cryostat-4)

The NASA Cryogenics Test Laboratory at Kennedy Space Center conducted long-term testing of SOFI materials under actual-use cryogenic conditions with Cryostat-4. The materials included in the testing were NCFI 24-124 (acreage foam), BX-265 (close-out foam, including intertank flange and bipod areas), and a potential alternate material, NCFI 27-68, (acreage foam with the flame retardant removed). Specimens of these materials were placed at two locations: a site that simulated aging (the Vehicle Assembly Building [VAB]) and a site that simulated weathering (the Atmospheric Exposure Test Site [beach site]). After aging/weathering intervals of 3, 6, and 12 months, the samples were retrieved and tested for their thermal performance under cryogenic vacuum conditions with test apparatus Cryostat-4.

Source record↗
NASA NTRS1974

Coercivity maxima at low temperatures

Recent measurements have shown that the magnetic coercive forces of some Apollo lunar samples show an unexpected decrease with decreasing temperature at cryogenic temperatures. This behavior can be explained quantitatively in terms of a model which considers additive contributions from a soft, reversible magnetic phase and from a harder, hysteretic magnetic phase.

Schwerer, F. C.↗
NASA NTRS2012

Measurement of Clathrate Hydrate Thermodynamic Stability in the Presence of Ammonia

There is a lack of data available for the stability of clathrate hydrates in the presence of ammonia for low-to-moderate pressures in the 0-10 MPa range. Providing such data will allow for a better understanding of natural mass transfer processes on celestial bodies like Titan and Enceladus, on which destabilization of clathrates may be responsible for replenishment of gases in the atmosphere. The experimental process utilizes a custom-built gas handling system (GHS) and a cryogenic calorimeter to allow for the efficient testing of samples under varying pressures and gas species.

clathrate hyudrates↗
NASA NTRSDate not supplied

An Overview of Nuclear Thermal Rocket Element Environmental Simulator (NTREES) Capabilities, Upgrades, and Overlaps in Advanced Material Testing Areas

The Nuclear Thermal Rocket Element Environmental Simulator (NTREES) was designed to perform non-nuclear testing of nuclear thermal rocket (NTR) fuel elements and materials. NTREES can simulate the thermal hydraulic environment within the reactor of an NTR and has been leveraged to provide data on the thermochemical, thermomechanical and thermohydraulic performance of components and materials. Active upgrades to the NTREES facility include installing a DC power supply for DC powered joule heating, a supply gas chiller for a cryogenically cool gas supply, gas pre-heaters with sample holders for testing samples too small to be inductively heated by bathing them in hot gas, and a high temperature digital image correlation (DIC) capability for measuring high temperature strains real time. In addition to NTR testing, given the commonality of high enthalpy flow environments between the reactor of an NTP engine and the aerothermal heating of high-speed flight, the unique capabilities of NTREES to provide high temperature gas flows at high pressure without combustion or electrode spallation byproducts may lend itself to additional usage of the facility beyond the original intent.

Michael P Schoenfeld↗
NASA NTRS2017

Testing Tensile and Shear Epoxy Strength at Cryogenic Temperatures

This paper covers cryogenic, tensile testing and research completed on a number of epoxies used in cryogenic applications. Epoxies are used in many different applications; however, this research focused on the use of epoxy used to bond MLI standoffs to cryogenic storage tanks and the loads imparted to the tank through the MLI. To conduct testing, samples were made from bare stainless steel, aluminum and primed aluminum. Testing involved slowly cooling test samples with liquid nitrogen then applying gradually increasing tensile loads to the epoxy. The testing evaluated the strength and durability of epoxies at cryogenic temperatures and serves as a base for future testing. The results of the tests showed that some epoxies withstood the harsh conditions while others failed. The two epoxies yielding the best results were Masterbond EP29LPSP and Scotch Weld 2216. For all metal surfaces tested, both epoxies had zero failures for up to 11.81 kg of mass.

multilayer insulation↗
NASA NTRS2017

Heat Loads Due to Small Penetrations in Multilayer Insulation Blankets

Abstract: This paper covers cryogenic, tensile testing and research completed on a number of epoxies used in cryogenic applications. Epoxies are used in many different applications; however, this research focused on the use of epoxy used to bond MLI standoffs to cryogenic storage tanks and the loads imparted to the tank through the MLI. To conduct testing, samples were made from bare stainless steel, aluminum and primed aluminum. Testing involved slowly cooling test samples with liquid nitrogen then applying gradually increasing tensile loads to the epoxy. The testing evaluated the strength and durability of epoxies at cryogenic temperatures and serves as a base for future testing. The results of the tests showed that some epoxies withstood the harsh conditions while others failed. The two epoxies yielding the best results were Masterbond EP29LPSP and Scotch Weld 2216. For all metal surfaces tested, both epoxies had zero failures for up to 11.81 kg of mass.

multilayer insulation↗
NASA NTRS2017

Testing Tensile and Shear Epoxy Strength at Cryogenic Temperatures

This paper covers cryogenic, tensile testing and research completed on a number of epoxies used in cryogenic applications. Epoxies are used in many different applications; however, this research focused on the use of epoxy used to bond MLI standoffs to cryogenic storage tanks and the loads imparted to the tank through the MLI. To conduct testing, samples were made from bare stainless steel, aluminum and primed aluminum. Testing involved slowly cooling test samples with liquid nitrogen then applying gradually increasing tensile loads to the epoxy. The testing evaluated the strength and durability of epoxies at cryogenic temperatures and serves as a base for future testing. The results of the tests showed that some epoxies withstood the harsh conditions while others failed. The two epoxies yielding the best results were Masterbond EP29LPSP and Scotch Weld 2216. For all metal surfaces tested, both epoxies had zero failures for up to 11.81 kg of mass..

epoxy↗
NASA NTRS2000

Clean and Cold Sample Curation

Curation of Mars samples includes both samples that are returned to Earth, and samples that are collected, examined, and archived on Mars. Both kinds of curation operations will require careful planning to ensure that the samples are not contaminated by the instruments that are used to collect and contain them. In both cases, sample examination and subdivision must take place in an environment that is organically, inorganically, and biologically clean. Some samples will need to be prepared for analysis under ultra-clean or cryogenic conditions. Inorganic and biological cleanliness are achievable separately by cleanroom and biosafety lab techniques. Organic cleanliness to the <50 ng/sq cm level requires material control and sorbent removal - techniques being applied in our Class 10 cleanrooms and sample processing gloveboxes.

Allen, C. C.↗
NASA NTRS1976

Exciton coupling in molecular crystals

The implications of perfect exciton coupling and molecular vibrations were investigated, as well as the effect they have on the lifetime of singlet and triplet excitons coupled in a limiting geometry. Crystalline bibenzyl, Cl4Hl4, provided a situation in which these mechanisms involving exciton coupling can be studied in the limit of perfect coupling between units due to the crystal's geometry. This geometry leads to a coupling between the two halves of the molecule resulting in a splitting of the molecular excited states. The study reported involves an experimental spectroscopic approach and begins with the purification of the bibenzyl. The principal experimental apparatus was an emission spectrometer. A closed cycle cryogenic system was used to vary the temperature of the sample between 20 K and 300 K. The desired results are the temperature-dependent emission spectra of the bibenzyl; in addition, the lifetimes and quantum yields measured at each temperature reveal the effect of competing radiationless processes.

Ake, R. L.↗
NASA NTRS1993

Collecting cometary soil samples? Development of the ROSETTA sample acquisition system

In the reference scenario of the ROSETTA CNRS mission, the Sample Acquisition System is mounted on the Comet Lander. Its tasks are to acquire three kinds of cometary samples and to transfer them to the Earth Return Capsule. Operations are to be performed in vacuum and microgravity, on a probably rough and dusty surface, in a largely unknown material, at temperatures in the order of 100 K. The concept and operation of the Sample Acquisition System are presented. The design of the prototype corer and surface sampling tool, and of the equipment for testing them at cryogenic temperatures in ambient conditions and in vacuum in various materials representing cometary soil, are described. Results of recent preliminary tests performed in low temperature thermal vacuum in a cometary analog ice-dust mixture are provided.

Coste, P. A.↗
NASA NTRS1992

Cryogenic leak testing of tube fittings/valves

A high pressure and variable temperature cryogenic leak testing system was conceived and designed in order to conduct leakage testing of pipe fittings/valves in liquid hydrogen supply lines of the Space Shuttle. The system can create a continuous testing environment of variable temperature, 5.5 to about 300 K, and variable pressure, 0.01 to about 70 x 10 exp 5 Pa, with a large sample space, 90 mm diameter x 228 mm length, and at low operating cost. In terms of cryogenic leak testing the system has a special capability for extensive applications. The system comprised a variable temperature cryostat, a high pressure sample chamber, a vacuum pumping station, gas flow control system, pressure and temperature control systems, and leak detecting and measuring systems. A general discussion of cryogenic leak testing methods is also presented.

Jia, L. X.↗