Search NASA⌕ Search

SEARCH · Search NASA

Results for “residual solvent”

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

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

98 records · Page 6

Use of GC/MS and Microtome Techniques as Methods to Evaluate ODC Free Cleaner Diffusion and Evaporation in Insulation and Phenolic Case Material

Because of the 1990 Clean Air Act Amendment (CAAA) many chlorinated solvents used in the aerospace industry are being phased out. Replacement of the ODC (ozone-depleting chemicals) with less volatile, non-ozone depleting cleaners has been extensively studied over the past seven years at Thiokol Propulsion, a Division of Cordant Technologies, Inc. The down selection of ODC replacement cleaners has been based on several factors including the diffusion evaporation of the cleaners in selected substrates. Methodologies were developed to evaluate the cleaner content in substrates. Methods of cutting thin slices of material (microtoming) were combined with GC/MS (gas chromatography/mass spectroscopy) analysis. Substrates evaluated in this study include potential solid rocket motor materials: ASNBR (asbestos-filled nitrile butadiene rubber) and CFEPDM (carbon-filled ethylene propylene dimonomer) insulation and glass (GCP), carbon (CCP) and silica (SCP) cloth phenolic substrates with fibers either parallel (0 deg) or perpendicular (90 deg) to the surface. Residue profiles indicate both cleaner and substrate composition affect the diffusion and subsequent evaporation of the cleaner from the substrate surface.

Biegert, L. L.↗

Sol-Gel Process for Making Pt-Ru Fuel-Cell Catalysts

A sol-gel process has been developed as a superior alternative to a prior process for making platinum-ruthenium alloy catalysts for electro-oxidation of methanol in fuel cells. The starting materials in the prior process are chloride salts of platinum and ruthenium. The process involves multiple steps, is time-consuming, and yields a Pt-Ru product that has relatively low specific surface area and contains some chloride residue. Low specific surface area translates to incomplete utilization of the catalytic activity that might otherwise be available, while chloride residue further reduces catalytic activity ("poisons" the catalyst). In contrast, the sol-gel process involves fewer steps and less time, does not leave chloride residue, and yields a product of greater specific area and, hence, greater catalytic activity. In this sol-gel process (see figure), the starting materials are platinum(II) acetylacetonate [Pt(C5H7O2)2, also denoted Pt-acac] and ruthenium(III) acetylacetonate [Ru(C5H7O2)3, also denoted Ru-acac]. First, Pt-acac and Ru-acac are dissolved in acetone at the desired concentrations (typically, 0.00338 moles of each salt per 100 mL of acetone) at a temperature of 50 C. A solution of 25 percent tetramethylammonium hydroxide [(CH3)4NOH, also denoted TMAH] in methanol is added to the Pt-acac/Ruacac/ acetone solution to act as a high-molecular-weight hydrolyzing agent. The addition of the TMAH counteracts the undesired tendency of Pt-acac and Ru-acac to precipitate as separate phases during the subsequent evaporation of the solvent, thereby helping to yield a desired homogeneous amorphous gel. The solution is stirred for 10 minutes, then the solvent is evaporated until the solution becomes viscous, eventually transforming into a gel. The viscous gel is dried in air at a temperature of 170 C for about 10 hours. The dried gel is crushed to make a powder that is the immediate precursor of the final catalytic product. The precursor powder is converted to the final product in a controlled-atmosphere heat treatment. Desirably, the final product is a phase-pure (Pt phase only) Pt-Ru powder with a high specific surface area. The conditions of the controlled- atmosphere heat are critical for obtaining the aforementioned desired properties. A typical heat treatment that yields best results for a catalytic alloy of equimolar amounts of Pt and Ru consists of at least two cycles of heating to a temperature of 300 C and holding at 300 C for several hours, all carried out in an atmosphere of 1 percent O2 and 99 percent N2. The resulting powder consists of crystallites with typical linear dimensions of <10 nm. Tests have shown that the powder is highly effective in catalyzing the electro-oxidation of methanol.

Narayanan, Sekharipuram↗

Hypergol Maintenance Facility North, SWMU 090, Year 3 Air Sparge System Performance Monitoring Report, Kennedy Space Center, Florida

This Performance Monitoring Report (PMR) presents Year 3 Air Sparge (AS) System operation, maintenance, and monitoring (OM&M) activities and performance monitoring results for the AS Interim Measure (IM) at the Hypergol Maintenance Facility North (HMFN) at Kennedy Space Center (KSC), Florida. HMFN has been designated Solid Waste Management Unit (SWMU) 090 under the KSC Resource Conservation and Recovery Act Corrective Action Program. The timeframe for activities included in this report extends from September 2022 to August 2023. The HMFN AS IM was implemented in 2019-2020 to treat a chlorinated solvent groundwater plume that resulted from historical operations supporting the National Aeronautics and Space Administration (NASA) Space Program. The system includes 213 AS wells, with screen depths ranging from 25 feet to 45 feet below land surface (bls) and treats approximately 1.62 acres of contaminated groundwater. The objective of the AS IM is to actively reduce groundwater concentrations exceeding Florida Department of Environmental Protection Natural Attenuation Default Concentrations (NADCs) (identified as the High Concentration Plume [HCP]) to levels that facilitate transition into a Long-Term Monitoring program. The AS IM targets all of the HCP, except for a source zone area within the HCP where trichloroethene (TCE) concentrations exceed 11,000 micrograms per liter (μg/L) at depths greater than 45 feet bls. This is because site lithology was found to not be conducive to the AS treatment technology at these deeper depths. NASA will re-visit plans for potentially utilizing another remedial technology for residual deeper contamination following completion of the AS IM. OM&M activities and results from Year 3 indicate that the AS system at HMFN is operating as designed and is meeting performance criteria. Groundwater performance monitoring results indicate that following the third year of AS system operation, TCE concentrations in wells across all treated depth intervals have been reduced by an average of more than 99 percent. Overall, the areal extent of the plume showed a reduction following Year 3 of AS operations; however, continued operation of the AS system is required to meet the IM objective.

VOCs↗

Genesis Solar Wind Sample 61422: Experiment in Variation of Sequence of Cleaning Solvent for Removing Carbon-Bearing Contamination

The recovered Genesis collector fragments are heavily contaminated with crash-derived particulate debris. However, megasonic treatment with ultra-pure-water (UPW; resistivity (is) greater than18 meg-ohm-cm) removes essentially all particulate contamination greater than 5 microns in size [e.g.1] and is thus of considerable importance. Optical imaging of Si sample 60336 revealed the presence of a large C-rich particle after UPW treatment that was not present prior to UPW. Such handling contamination is occasionally observed, but such contaminants are normally easily removed by UPW cleaning. The 60336 particle was exceptional in that, surprisingly, it was not removed by additional UPW or by hot xylene or by aqua regia treatment. It was eventually removed by treatment with NH3-H2O2. Our best interpretation of the origin of the 60336 particle was that it was adhesive from the Post-It notes used to stabilize samples for transport from Utah after the hard landing. It is possible that the insoluble nature of the 60336 particle comes from interaction of the Post-It adhesive with UPW. An occasional bit of Post-It adhesive is not a major concern, but C particulate contamination also occurs from the heat shield of the Sample Return Capsule (SRC) and this is mixed with inorganic contamination from the SRC and the Utah landing site. If UPW exposure also produced an insoluble residue from SRC C, this would be a major problem in chemical treatments to produce clean surfaces for analysis. This paper reports experiments to test whether particulate contamination was removed more easily if UPW treatment was not used.

Allton, J. H.↗

Double-Vacuum-Bag Process for Making Resin-Matrix Composites

A double-vacuum-bag process has been devised as a superior alternative to a single-vacuum-bag process used heretofore in making laminated fiber-reinforced resin-matrix composite-material structural components. This process is applicable to broad classes of high-performance matrix resins including polyimides and phenolics that emit volatile compounds (solvents and volatile by-products of resin-curing chemical reactions) during processing. The superiority of the double-vacuum-bag process lies in enhanced management of the volatile compounds. Proper management of volatiles is necessary for making composite-material components of high quality: if not removed and otherwise properly managed, volatiles can accumulate in interior pockets as resins cure, thereby forming undesired voids in the finished products. The curing cycle for manufacturing a composite laminate containing a reactive resin matrix usually consists of a two-step ramp-and-hold temperature profile and an associated single-step pressure profile as shown in Figure 1. The lower-temperature ramp-and-hold step is known in the art as the B stage. During the B stage, prepregs are heated and volatiles are generated. Because pressure is not applied at this stage, volatiles are free to escape. Pressure is applied during the higher-temperature ramp-and-hold step to consolidate the laminate and impart desired physical properties to the resin matrix. The residual volatile content and fluidity of the resin at the beginning of application of consolidation pressure are determined by the temperature and time parameters of the B stage. Once the consolidation pressure is applied, residual volatiles are locked in. In order to produce a void-free, high-quality laminate, it is necessary to design the curing cycle to obtain the required residual fluidity and the required temperature at the time of application of the consolidation pressure.

Bradford, Larry J.↗

Organic Products of Fatty Acid and Magnesium Sulfate Mixtures after Gamma Radiolysis: Implications for Missions to Europa

If ocean-derived materials are present at Europa’s surface, they would represent accessible records of ocean chemistry and habitability, but such materials would be further processed by the moon’s harsh radiation environment. In this study, saturated fatty acids were precipitated onto a Europa-relevant hydrated magnesium sulfate and exposed to gamma radiation doses up to 2 MGy at -196° C. Alkane chains, with carbon numbers one less than those of the starting fatty acids, were the most abundant radiolysis products in solvent and thermal extracts analyzed by gas chromatography mass spectrometry. Detections of monounsaturated fatty acids and combined radiolysis products were attributed to the experiment’s Europa-like parameters. Additionally, elevated concentrations of shorter-chain saturated fatty acids suggest that gamma radiation induced charge remote fragmentation of the alkyl chains of some starting fatty acids under these experimental conditions. Quantitation of fatty acid concentrations in the irradiated samples enabled the calculation of a radiolysis constant that indicated exposure to a 5 MGy dose of gamma radiation would have resulted in a ~90% loss of the initial fatty acid population. The samples were further studied by Raman spectroscopy and laser desorption and ionization mass spectrometry, which characterized the distribution of fatty acids and their radiolysis products on sulfate surfaces. The substantial loss of starting fatty acids typically seen with increasing radiation dose, along with the remarkable diversity of radiolysis products identified, suggest that the detection of fatty acids in irradiated sulfate deposits on Europa will be challenged by rapid destruction of any initial fatty acid populations and scrambling of their residual signals by a myriad of organic radiolysis products. If missions to Europa encounter sulfate deposits, targeting minimally irradiated units may still enable the detection of surviving fatty acid signatures that could inform about Europa’s subsurface chemistry and habitability.

James M T Lewis↗

Flight Validation of Atomic Oxygen Resistant Resistant Polymers

Because of its high reactivity, atomic oxygen causes surface erosion on polymeric materials. although the reaction efficiency depends on the chemical structure of the polymer. We have found an organotin compound, bis(triphenyltin) oxide (BTO), which has an unusually high solubility in solutions of a number of commercial high performance polymers. Films of these polymers containing BTO showed a substantial reduction in erosion by atomic oxygen when compared with films of the pure material. Analysis has shown that in the presence of atomic oxygen, erosion of the exposed surfaces of the BTO-containing films leaves a residual protective tin oxide coating . Since the additive is uniformly distributed throughout the polymeric material, any break or puncture in the protective coating is "healed" by the material below. Samples were exposed to the environment of the low earth orbit (LEO) on two Space Shuttle flights, STS-46, in June of 1992, and STS-51 in September of 1993. The analysis of these samples has been reported previously. For both flights, the samples were small (1.3 cm and 1.9 cm respectively) thus limiting the scope of analysis. In the research under this cooperative agreement, films of a polyetherimide, were exposed to the LEO environment on Space Shuttle flight STS-85 in August of 1997 as part of the Evaluation of Space Environment and Effects on Materials (ESEM) experiment. The polyetherimide chosen is available commercially as Ultem, registered to the General Electric Company. Films of pure Ultem, Ultem with 10% BTO by mass, and Ultem with 20% BTO by mass were exposed in the ram direction for 40 hours during STS-85. Ultem has a Tg of 215 deg C and is soluble in common chlorinated solvents. Granules of the polymer were dried at 120 deg C, but otherwise were used as received. Films were cast on a glass plate from a solution of the polymer in a 60/40 (w/w) mixture of chloroform and 1,1,2,2-tetrachloroethane. The plate was placed in a dust-free box for at least 24 hours to allow much of the solvent to evaporate, and then was moved to a vacuum oven and slowly heated from 20 to 220 deg C over a period of two weeks to completely remove all solvent. Each exposed sample was 7.6 cm long and 2.2 cm wide and about 0.025 mm thick. The structures of Ultem and bis(triphenyltin) oxide are shown.

Kiefer, Richard L.↗

KSC Headquarters Building Area SWMU 104 Soil Interim Measure Report for LOC 2D and LOC 2E Kennedy Space Center, Florida

This Interim Measure (IM) Report for Location of Concern (LOC) 2D and LOC 2E summarizes the activities associated with implementation of an IM to address soil and concrete contamination at the Kennedy Space Center (KSC) Headquarters Building Area (KHQA) located at KSC, Florida. KHQA has been designated Solid Waste Management Unit (SWMU) 104 under KSC’s Resource Conservation and Recovery Act Corrective Action Program. The IM consisted of excavating/removing residual polychlorinated biphenyl (PCB) contamination in soil and concrete from two separate areas, LOC 2D and LOC 2E, which were associated with electrical transformer locations. IM activities were conducted in accordance with the Interim Measure Work Plan (IMWP), Revision 1, for KHQA dated June 2018, which was approved by the Florida Department of Environmental Protection in a correspondence letter dated April 2016 and the United States Environmental Protection Agency in a correspondence letter dated August 2018. The objective of the IM was to remove all remaining contaminated media with total PCB concentrations greater than the State of Florida Residential Soil Cleanup Target Level (RSCTL) (0.5 milligrams per kilogram [mg/kg]). This cleanup goal meets unrestrictive re-use conditions in Florida, and is below federal regulations for PCB Bulk Remediation Waste Cleanup of 1 mg/kg for high occupancy, unrestricted use areas, as outlined in 40 Code of Federal Regulations (CFR) 761.61(a). The timeline of the IM was coordinated with demolition of the former KSC Headquarters Building (demolished in 2021) in order to safely remove contaminated media after electrical equipment was de-energized and removed from the site. Excavation activities were conducted between January 10, 2022, and February 8, 2022, and included two waste streams for off-site disposal: (1) PCB-remediation waste greater than or equal to 50 mg/kg, and (2) PCB-remediation waste less than 50 mg/kg. A total of approximately 347 cubic yards (478 tons) of PCB-contaminated soil and concrete was initially removed from the LOC 2D and LOC 2E areas, as defined in the IMWP. An additional 4.35 tons of soil and concrete were removed based on verification sampling, which was conducted until the cleanup goal was achieved. The total area of excavation from both LOC 2D and LOC 2E was approximately 5,186 square feet (0.12 acres), and excavation depths ranged from 0.5 to 4.0 feet below land surface Excavated soils and concrete were stockpiled based on waste stream and subsequently transported and disposed of at Waste Connections of Osceola County, LLC – JED Landfill in St. Cloud, Florida (PCBs less than 50 mg/kg) or the Chemical Waste Management Landfill in Emelle, Alabama (PCBs greater than or equal to 50 mg/kg). Following excavation, clean backfill was brought to the site and provided to the Demolition Contractor to complete backfill and grading in conjunction with their final site restoration activities from building demolition. Post-IM groundwater sampling was conducted in May 2022 at three monitoring wells installed in April 2022 to confirm that PCBs did not leach into groundwater. These wells were installed where the highest PCB concentrations were detected at LOC 2D, LOC 2E, and from the Building Perimeter IM (previously completed in 2020). All PCB results in groundwater were non-detect. Volatile organic compounds were also analyzed based on potential past use of solvents in transformers with PCB-dielectric fluids and the potential release of dielectric fluids containing volatile organic compounds, and all results were non-detect. Based on completion of a successful IM at LOC 2D and LOC 2E, as well as previous remedial actions that have addressed other contamination at KHQA (SWMU 104), No Further Action without controls will be recommended for SWMU 104. NASA will submit separate Site Rehabilitation Completion Order request documentation for SWMU 104 to support an NFA without controls recommendation.

PCB↗