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Thermal degradation of polyoxypropylene glycol- toluene 2, 4-diisocyanate polymer /POPG-TDI/ OCCURS by random scission of urethane linkages to regenerate hydroxyl and isocyanate
Glycols, specifically ethylene glycol and 1,2-propanediol, are some of the major organic compounds found in the humidity condensate samples collected on the International Space Station. The current analytical method for glycols is a GC/MS method with direct sample injection. This method is simple and fast, but it is not very sensitive. Reporting limits for ethylene glycol and 1,2-propanediol are only 1 ppm. A much more sensitive GC/FID method was developed, in which glycols were derivatized with benzoyl chloride for 10 minutes before being extracted with hexane. Using 1,3-propanediol as an internal standard, the detection limits for the GC/FID method was determined to be 50 ppb and the analysis only takes 7 minutes. Data from the GC/MS and the new GC/FID methods shows excellent agreement with each other. Factors affecting the sensitivity, including sample volume, NaOH concentration and volume, volume of benzoyl chloride, reaction time and temperature, were investigated. Interferences during derivatization and possible method to reduce interferences were also investigated.
As part of an investigation of the cooling characteristics of liquid-cooled engines, tests were conducted with an electrically heated single-tube heat exchanger to determine the heat-transfer characteristics of an-e-2 ethylene glycol and other ethylene glycol-water mixtures. Similar tests were conducted with water and commercial butanol (n-butyl alcohol) for check purposes. The results of tests conducted at an approximately constant liquid-flow rate of 0.67 pound per second (Reynolds number, 14,500 to 112,500) indicate that at an average liquid temperature 200 degrees f, the heat-transfer coefficients obtained using water, nominal (by volume) 30 percent-70 percent and 70 percent-30 percent glycol-water mixtures are approximately 3.8, 2.8, and 1.4 times higher, respectively, than the heat-transfer coefficients obtained using an-e-2 ethylene glycol.
A planned use of the Orion space vehicle involves its residence at the International Space Station for six months at a time. One concept of operations involves temporarily venting portions of the idle Orion active thermal control system (ATCS) during the docked phase, preventing freezing. The venting would have to be reasonably complete with few, if any, completely filled pockets of frozen liquid. Even if pockets of frozen liquid did not damage the hardware during the freezing process, they could prevent the system from filling completely prior to its reactivation. The venting of single component systems in a space environment has been performed numerous times and is well understood. Local nucleation occurs at warm, relatively massive parts of the system, which creates vapor and forces the bulk liquid out of the system. The remnants of the liquid will freeze, then evaporate over time through local heating. Because the Orion ATCS working fluid is a 50/50 mixture of water and inhibited propylene glycol, its boiling behavior was expected to differ from that of a pure fluid. It was thought that the relatively high vapor pressure water might evaporate preferentially, leaving behind a mixture enriched with the low vapor pressure propylene glycol, which would be vaporization ]resistant. Owing to this concern, a test was developed to compare the evaporation behavior of pure water, a 50/50 mixture of water and inhibited propylene glycol, and inhibited propylene glycol. The test was performed using room temperature fluids in an instrumented thin walled stainless steel vertical tube. The 1 in x 0.035 in wall tube was instrumented with surface thermocouples and encased in closed cell polyurethane foam. Reticulated polyurethane foam was placed inside the tube to reduce the convection currents. A vacuum system connected to the top of the tube set the pressure boundary condition. Tests were run for the three fluids at back pressures ranging from 1 to 18 torr. During each test, the mass of the test article was measured as it changed over time, as was its temperature and backpressure. The tests were successful. Somewhat surprisingly, the results showed that the evaporation behavior of the three fluids had more similarities than differences. The 50/50 mixture evaporated similarly to the pure water - albeit at a slower rate. The test results indicate that our extensive space - based experience with venting of single component fluids can be applied to the problem of Orion ATCS venting as long as the appropriate puts, takes, and caveats are applied.
A human spacecraft ATCS—especially one using single-phase coolant loops exposed to cabin atmospheric conditions—requires periodic degassing and refilling to support long-duration missions of 15 to 30 years. During initial fill operations, system maintenance, gas permeation, and quick-disconnect mating or de-mating, small amounts of gas can gradually enter the coolant system over time. This can lead to degraded heat transfer performance, pump cavitation, and potentially pump vapor lock if a significant gas volume accumulates over time. Additionally, system leaks and routine fluid sampling can gradually reduce accumulator volumes to unacceptable levels, requiring periodic refills. In more severe cases, catastrophic changes in fluid composition may necessitate emergency draining, refilling, and degassing to ensure continued system functionality. These risks were identified and mitigated on the ISS ITCS through the development of a dual-membrane degasser ORU and a Fluid Servicer System ORU for coolant refilling. These systems were developed for the fully water-based ISS ITCS Coolant[1]. The Gateway space station, the first permanent human habitat in lunar orbit, uses a propylene-glycol/water coolant mixture, which has significantly different fluid properties compared to pure water. Because microgravity degassing technologies are sensitive to fluid surface tension and viscosity, existing ISS hardware is not suitable for servicing a propylene-glycol-based TCS. Unlike the ISS, the Gateway will operate in a higher-radiation environment and must meet stricter mass constraints due to its location outside of low earth orbit. This Government Furnished Equipment (GFE) flight hardware project aims to develop a lightweight, radiation-resistant Coolant Servicer System (CSS) capable of degassing and refilling Gateway’s propylene-glycol water-based IATCS.
A human spacecraft ATCS—especially one using single-phase coolant loops exposed to cabin atmospheric conditions—requires periodic degassing and refilling to support long-duration missions of 15 to 30 years. During initial fill operations, system maintenance, gas permeation, and quick-disconnect mating or de-mating, small amounts of gas can gradually enter the coolant system over time. This can lead to degraded heat transfer performance, pump cavitation, and potentially pump vapor lock if a significant gas volume accumulates over time. Additionally, system leaks and routine fluid sampling can gradually reduce accumulator volumes to unacceptable levels, requiring periodic refills. In more severe cases, catastrophic changes in fluid composition may necessitate emergency draining, refilling, and degassing to ensure continued system functionality. These risks were identified and mitigated on the ISS ITCS through the development of a dual-membrane degasser ORU and a Fluid Servicer System ORU for coolant refilling. These systems were developed for the fully water-based ISS ITCS Coolant[1]. The Gateway space station, the first permanent human habitat in lunar orbit, uses a propylene-glycol/water coolant mixture, which has significantly different fluid properties compared to pure water. Because microgravity degassing technologies are sensitive to fluid surface tension and viscosity, existing ISS hardware is not suitable for servicing a propylene-glycol-based TCS. Unlike the ISS, the Gateway will operate in a higher-radiation environment and must meet stricter mass constraints due to its location outside of low earth orbit. This Government Furnished Equipment (GFE) flight hardware project aims to develop a lightweight, radiation-resistant Coolant Servicer System (CSS) capable of degassing and refilling Gateway’s propylene-glycol water-based IATCS.
A glycol-exuding porous leading edge ice protection system was tested. Results show that the system is very effective in preventing ice accretion (anti-ice mode) or removing ice from an airfoil. Minimum glycol flow rates required for anti-icing are a function of velocity, liquid water content in the air, ambient temperature, and droplet size. Large ice caps were removed in only a few minutes using anti-ice flow rates. It was found that the shed time is a function of the type of ice, size of the ice cap, angle of attack, and glycol flow rate. Wake survey measurements show that there is no significant drag penalty for the installation or operation of the system tested.
Two fluid life tests have been conducted to evaluate propylene glycol-based fluids for use in Constellation habitats and vehicles. The first test was conducted from November 2008 to January 2009 to help determine the compatibility of the propylene glycol-based fluid selected for Orion at the time. When the first test uncovered problems with the fluid selection, an investigation and selection of a new fluid were conducted. A second test was started in March 2010 to evaluate the new selection. For the first test, the fluid was subjected to a thermal fluid loop that had flight-like properties, as compared to Orion. The fluid loop had similar wetted materials, temperatures, flow rates, and aluminum wetted surface area to fluid volume ratio. The test was designed to last for 10 years, the life expectancy of the lunar habitat. However, the test lasted less than two months. System filters became clogged with precipitate, rendering the fluid system inoperable. Upon examination of the precipitate, it was determined that the precipitate composition contained aluminum, which could have only come from materials in the test stand, as aluminum is not part of the original fluid composition. Also, the fluid pH was determined to have increased from 10.1, at the first test sample, to 12.2, at the completion of the test. This high of a pH is corrosive to aluminum and was certainly a contributing factor to the development of precipitate. Due to the problems encountered during this test, the fluid was rejected as a coolant candidate for Orion. A new propylene glycol-based fluid was selected by the Orion project for use in the Orion vehicle. The Orion project has conducted a series of screening tests to help verify that there will be no problems with the new fluid selection. To compliment testing performed by the Orion project team, a new life test was developed to test the new fluid. The new test bed was similar to the original test bed, but with some improvements based on experience gained from the earlier test bed. The surface area of both aluminum and nickel in the test bed were designed to be similar to that of the Orion fluid loop, since the Orion fluid loop was expected to have high concentrations of both metals in the system. Also, additional sample materials were added to the test bed to match recent updates to materials selections for Orion. At the time of this paper publication, approximately five months of testing will have been completed. This paper gives a status of the testing completed to date.
Very low concentrations of ethylene glycol in air or other gases are detected by passing a sample through a glass tube with three partitioned compartments containing reagents which successively convert the ethylene glycol vapor into a colored compound.
Small additions /0.01 percent or less/ of triethanoloamine sodium sulfite adduct to mercapto benzothiazole inhibited glycol water heat transfer solutions containing disulfide precipitate produce marked reduction in amount of precipitate. Adduct is useful as additive in glycol base antifreezes and coolants.
Initial screening tests and the results obtained in developing procedures to determine Al, Cu, Fe, and Pb in glycol formulations are described. Atomic absorption completion was selected for Cu, Fe and Pb, and after comparison with emission spectroscopy, was selected for Al also. Before completion, carbon, iron, and lead are extracted with diethyl dithio carbamate (DDC) into methyl isobutyl ketone (MIBK). Aluminum was also extracted into MIBK using 8-hydroxyquinoline as a chelating agent. As little as 0.02 mg/l carbon and 0.06 mg/l lead or iron may be determined in glycol formulations. As little as 0.3 mg/l aluminum may be determined.
Interstellar ethylene glycol (HOCH2CH2,OH) has been detected in emission toward the Galactic center source Sagittarius B2(N-LMH) by means of several millimeter-wave rotational torsional transitions of its lowest energy conformer. The types and kinds of molecules found to date in interstellar clouds suggest a chemistry that favors aldehydes and their corresponding reduced alcohols-e.g., formaldehyde (H2CO)/methanol (CH3OH), acetaldehyde (CH3CHO)/ethanol (CH3CH2OH). Similarly, ethylene glycol is the reduced alcohol of glycolaldehyde (CH2OHCHO), which has also been detected toward Sgr B2(N-LMH). While there is no consensus as to how any such large complex molecules are formed in the interstellar clouds, atomic hydrogen (H) and carbon monoxide (CO) could form formaldehyde on grain surfaces, but such surface chemistry beyond that point is uncertain. However, laboratory experiments have shown that the gas-phase reaction of atomic hydrogen (H) and solid-phase CO at 10-20 K can produce formaldehyde and methanol and that alcohols and other complex molecules can be synthesized from cometary ice analogs when subject to ionizing radiation at 15 K. Thus, the presence of aldehyde/ reduced alcohol pairs in interstellar clouds implies that such molecules are a product of a low-temperature chemistry on grain surfaces or in grain ice mantles. This work suggests that aldehydes and their corresponding reduced alcohols provide unique observational constraints on the formation of complex interstellar molecules.
The fabrication of hydrogel microstructures based upon poly(ethylene glycol) diacrylates, dimethacrylates, and tetraacrylates patterned photolithographically on silicon or glass substrates is described. A silicon/silicon dioxide surface was treated with 3-(trichlorosilyl)propyl methacrylate to form a self-assembled monolayer (SAM) with pendant acrylate groups. The SAM presence on the surface was verified using ellipsometry and time-of-flight secondary ion mass spectrometry. A solution containing an acrylated or methacrylated poly(ethylene glycol) derivative and a photoinitiator (2,2-dimethoxy-2-phenylacetophenone) was spin-coated onto the treated substrate, exposed to 365 nm ultraviolet light through a photomask, and developed with either toluene, water, or supercritical CO2. As a result of this process, three-dimensional, cross-linked PEG hydrogel microstructures were immobilized on the surface. Diameters of cylindrical array members were varied from 600 to 7 micrometers by the use of different photomasks, while height varied from 3 to 12 micrometers, depending on the molecular weight of the PEG macromer. In the case of 7 micrometers diameter elements, as many as 400 elements were reproducibly generated in a 1 mm2 square pattern. The resultant hydrogel patterns were hydrated for as long as 3 weeks without delamination from the substrate. In addition, micropatterning of different molecular weights of PEG was demonstrated. Arrays of hydrogel disks containing an immobilized protein conjugated to a pH sensitive fluorophore were also prepared. The pH sensitivity of the gel-immobilized dye was similar to that in an aqueous buffer, and no leaching of the dye-labeled protein from the hydrogel microstructure was observed over a 1 week period. Changes in fluorescence were also observed for immobilized fluorophore labeled acetylcholine esterase upon the addition of acetyl acholine.
Bilateral surface-active minerals with excess positive charge concentrate glycolate and trimetaphosphate ion from l0(-3) m aqueous solution to half-saturation of the internal surface sites, and induce phosphorylation of glycolate ion in the mineral with trimetaphosphate, sorbed from l0(-2) m solution. By utilizing reactants from dilute solution at near-neutral pH, and eliminating the need for participating organic nitrogen compounds, the reaction comprises several elements considered necessary for geochemical realism in models for molecular evolution.
Some effects of gravity on early morphogenesis are correlated with microtubule locations within cells. During first cleavage in Ilyanassa obsoleta embryos, a transitory polar lobe constriction forms and then relaxes, allowing the polar lobe to merge with one daughter cell. If the polar lobe is equally divided or removed, morphogenesis is severely disrupted. To examine microtuble locations during early Ilyanassa development, eggs were fixed and stained for polymerized alpha-tubulin during first cleavage. The mitotic apparatus assembles at the animal pole. The cleavage furrow forms between the asters, constricting to a stabilized intercellular bridge encircling midbody-bound microtubules, whereas the polar lobe constriction forms below and parallel to the spindle, constricting to a transitory intercellular bridge encircling no detectable microtubules. At metaphase an alpha-tubulin epitope is distributed throughout the spindle, whereas a beta-tubulin epitope is present predominantly in the asters. Incubation in hexylene glycol, a drug that increases microtubule polymerization, during mitosis causes the polar lobe constriction to tighten around polymerized alpha-tubulin and remain stably constricted. If hexylene glycol is removed, alpha-tubulin staining disappears from the polar lobe constriction, which relaxes, whereas microtubules remain in the cleavage furrow, which remains constricted. These observations suggest that asymmetric distribution of microtubules affects early Ilyanassa cleavage patterns, and that continued presence of microtubules extending through an intercellular bridge is important for stabilization of the bridge constriction prior to completion of cytokinesis. These data provide the basis for further analysis of the role of microtubules in possible microgravity disruptions of Ilyanassa development.
Evaluations of thermal properties and resistance to microbial growth concluded that 50% Propylene Glycol (PG)-based fluid and 50% de-ionized water mixture was desirable for use as a fluid within a vehicle s thermal control loop. However, previous testing with a commercial mixture of PG and water containing phosphate corrosion inhibitors resulted in corrosion of aluminum within the test system and instability of the test fluid. This paper describes a follow-on long duration testing and analysis of 50% Propylene Glycol (PG)-based fluid and 50% de-ionized water mixture with inorganic corrosion inhibitors used in place of phosphates. The test evaluates the long-term fluid stability and resistance to microbial and chemical changes
Ebulliometric and end-group molecular weights of polyoxypropylene and polyoxyethylene glycols
Incipient cavitation studies with ethylene glycol and water over range of flow velocities and liquid temperatures in tunnel-mounted venturi