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Tetrachloreterephthaloyl chloride reacts with sodium azide in an atmosphere of nitrogen to form a high yield of tetrachloro-p-phenylene diisocyanate. The chlorinated diisocyanate should have application as an intermediate in the preparation of polyurethane foams. The high halogen content would impart added flame resistance to these foams.
Intramolecular formation of azo-linkage accompanying N elimination from bis-azide
A critical appraisal is made of the design, research, development, and operation of the novel UTIAS implosion-driven hypervelocity launchers and shock tubes. Explosively driven (PbN6-lead azide, PETN-pentaerythritetetranitrate) implosions in detonating stoichiometric hydrogen-oxygen mixtures have been successfully developed as drivers for hypervelocity launchers and shock tubes in a safe and reusable facility. Intense loadings at very high calculated pressures, densities, and temperatures, at the implosion center, cause severe problems with projectile integrity. Misalignment of the focal point can occur and add to the difficulty in using small caliber projectiles. In addition, the extreme driving conditions cause barrel expansion, erosion, and possible gas leakage from the base to the head of the projectile which cut the predicted muzzle velocities to half or a third of the lossless calculated values. However, in the case of a shock-tube operation these difficulties are minimized or eliminated and the possibilities of approaching Jovian reentry velocities are encouraging.
The feasibility of operating small thrust level electrothermal thrusters is determined with monopropellants other than MIL-grade hydrazine. The work scope includes analytical study, design and fabrication of demonstration thrusters, and an evaluation test program where monopropellants with freezing points lower than MIL-grade hydrazine are evaluated and characterized to determine their applicability to electrothermal thrusters for spacecraft attitude control. Results of propellant chemistry studies and performance analyses indicated that the most promising candidate monopropellants to be investigated are monomethylhydrazine, Aerozine-50, 77% hydrazine-23% hydrazine azide blend, and TRW formulated mixed hydrazine monopropellant (MHM) consisting of 35% hydrazine-50% monomethylhydrazine-15% ammonia.
The feasibility of operating small thrust level electrothermal thrusters with monopropellants other than MIL-grade hydrazine was studied. Analytical study, design, and fabrication of demonstration thrusters was performed, and an evaluation test program was initiated to evaluate monopropellants with freezing points lower than MIL-grade hydrazine, and to determine their applicability to electrothermal thrusters for spacecraft attitude control. Five demonstration thrusters were fabricated to determine the feasibility of operation with monomethylhydrazine, Aerozine-50, 77 percent hydrazine-23 percent hydrazine azide, and a mixture of hydrazine monopropellants consisting of 35 percent hydrazine-50 percent monomethylhydrazine-15 percent ammonia. The present thruster is designed to produce a steady-state thrust level of 0.344 N at 1.724 x 1 million N/M sq feed pressure. Vacuum specific impulse goals were set at 1961 N-s/kg steady-state and 1716 N-s/kg pulsed-mode.
A process is described for preparing flame resistant, nontoxic vinyl polymers which contain phosphazene groups and which do not emit any toxic or corrosive products when they are oxidatively degraded. Homopolymers, copolymers, and terpolymers of a styrene based monomer are prepared by polymerizing at least one oxidized styrylphosphine monomer from a group of organic azides, or by polymerizing p-diphenylphosphinestyrene and then oxidizing that monomer with an organoazide from the group of (C6H5)2P(O)N3, (C6H5O)2P(O)N3, (C6H5)2C3N3(N3), and C6H5C3N3(N3)2. Copolymers can also be prepared by copolymerizing styrene with at least one oxidized styrylphosphine monomer.
A flame resistant, nontoxic polymer which may be used safely in confined locations where there is inadequate ventilation is prepared either by polymerizing compounds having the formula R-N=P(C6H5)2(C6H4)CH=CH2 where R is an organic moeity selected from the group of (C6H5)2P(O)-, (C6H5O)2P(O)-, (C6H5)2 C3N3-, or their mixtures, or by reacting a polymer with an organic azide such as diphenylphosphinylazide, diphenyl-phosphorylazide, 2-azido-4,6-diphenly-5-triazine, 2,4-diazido-6-phenyl-s-triazine, trimethylsilyoazide, triphenylsilylazine, and phenylazine. The reaction of the styrylphosphine with the organozaide results in the oxidation of the trivalent phosphorus atom to the pentavalent state in the form of an unsaturated P=N linkage known as a phosphazene group.
An antireflection coating (ARC) for use with poly(methyl methacrylate) (PMMA) resist for ArF excimer laser lithography (193 nm) was formulated. It consists of PMMA and a bis-azide, 4.4-prime-diazidodiphenyl sulfone (DDS) which crosslinks the film after deep UV (260 nm) irradiation and subsequent annealing. The reacted DDS then serves as the absorber for the 193 nm radiation and also prevents mixing of the ARC and PMMA during PMMA spin-coating and development. The effectiveness of the ARC was demonstrated by exposing, in PMMA, using achromatic holographic lithography, gratings of 100 nm period (about 50 nm linewidth) that are almost entirely free of an orthogonal standing wave.
The paper reports properties of a sulfite-activated ATPase from Sulfolobus solfataricus, purified using ammonium sulfate precipitation, column chromatography on UltraGel and Sepharose 6B, and SDS-PAGE. The 92-fold purified enzyme had a relative molecular mass of 370,000. It could be dissociated into three subunits with respective molecular masses of 63,000, 48,000, and 24,000. The ATPase activity was found to be inhibitable by nitrate, N-ethylmaleimide (which bound predominantly to the largest subunit), and 4-chloro 7-nitrobenzofurazan, but not by azide, quercetin, or vanadate. While the ATPase from S. solfataricus shared a number of properties with the S. acidocaldarius ATPase, there were also significant differences suggesting the existence of several types of archaeal ATPases.
Several bacterial isolates enriched from seawater using complex media were able to accumulate dimethylsulfoniopropionate (DMSP) from media into cells over several hours without degrading it. Uptake only occurred in metabolically active cells, and was repressed in some strains by the presence of additional carbon sources. Accumulation was also more rapid in osmotically-stressed cells, suggesting DMSP is used as an osmotic solute. Uptake could be blocked by inhibitors of active transport systems (2,4-dinitrophenol, azide, arsenate) and of protein synthesis (chloramphenicol). Some structural analogs such as glycine betaine and S-methyl methionine also blocked DMSP uptake, suggesting that the availability of alternate organic osmolytes may influence DMSP uptake. Stresses such as freezing, heating, or osmotic down shock resulted in partial release of DMSP back to the medium. One strain which contained a DMSP-lyase was also able to accumulate DMSP, and DMS was only produced in the absence of alternate carbon sources. Bacteria containing DMSP were prepared as prey for bacterivorous ciliates and flagellates, to examine the fate of the DMSP during grazing. In all cases, predators metabolized the DMSP in bacteria. In some cases, DMS was produced, but it is not clear if this was due to the predators or to associated bacteria in the non-axenic grazer cultures. Bacterivores may influence DMSP cycling by either modulating populations of DMSP-metabolizing bacteria, or by metabolizing DMSP accumulated by bacterial prey.
As a part of a high energy density materials (HEDM) development, the hot fire tests for Quadricyclane, 1,7 Octadiyne, AFRL-1, Biclopropylidene, and CINCH (Dimethyl amino ethyl azide) have been conducted at NASA/MSFC. The first 4 materials for this task are provided from Air Force Research Laboratory at Edward Air Force Base and US Army provided CINCH. The performance of these fuels is compared with RP-1. The preliminary results of these tests are presented. The preliminary results of Quadricyclane tests indicate that the specific impulse and c-star efficiency for quadricyclane at the mixture ratio 1.94 are approximately 5 sec and 105 ft/sec better than the RP-1 at mixture ratio 1.9. The 1,7 Octadiyne test indicate that the specific impulse and c-star efficiency at the mixture ratio 2.1 are approximately -1 sec and 89 ft/sec differ than the RP-1 at mixture ratio 2.04. The Quadricyclane soot buildup at the combustor is a little more than RP-1, but detail study of soot formation is not considered at this time. There was no visual soot buildup for the 1,7 Octadiyne and AFRL-1.
Naval Surface Warfare Center, Indian Head Division's CAD/PAD Department has been working to remove toxic compounds from our products for about a decade. In 1992, we embarked on an effort to develop a lead-free double base propellant to replace that of a foreign sole source. At the time there were availability concerns. In 1995, the department developed a strategic proposal to include a wider range of products. Efforts included such efforts as removing lead sheathing from linear explosives and replacing lead azide and lead styphnate compounds. This paper will discuss efforts specifically related to developing non-leaded double base propellant for use in various Propellant Actuated Devices (PADs) for aircrew escape systems. The propellants can replace their leaded counterparts, mitigating lead handling, processing, or toxic exposure to the environment and personnel. This work eliminates the use of leaded compounds, replacing them with a more environmentally benign metal-organic salt. Historically double-base propellants have held an advantage over other families of energetic materials through their relative insensitivity of the burning rate to changes in temperature and pressure. This desirable ballistic effect has been obtained with the use of a lead-organic salt alone or in a physical mixture with a copper-organic salt, or more recently with a lead-copper complex. These ballistic modifiers are typically added to the double-base 'paste' prior to gelatinization on heated calendars or one type or another. The effect of constant burning rate over a pressure range is called a 'plateau' while an even more beneficial effect of decreasing burning rate with increasing pressure is termed a 'mesa.' The latter effect results in very low temperature sensitivity of the propellant burning rate. Propellants with such effects are ideal tactical rocket motor propellants. The use of lead compounds poses a concern for the environment and personnel safety due to the metal's toxic nature when introduced into the atmosphere by propellant manufacturing, rocket firings, and disposal. Two separate programs are underway at Indian Head to replace the leaded ballistic modifiers in NOSIH-AA-2 and KU propellants. Although the system requirements were very different, the programs gained valuable information from one another throughout their course.
This was a small-scale, hot-fire test series to make initial measurements of performance differences of five new liquid fuels relative to rocket propellant-1 (RP-1). The program was part of a high-energy-density materials development at Marshall Space Flight Center (MSFC), and the fuels tested were quadricyclane, 1-7 octodiyne, AFRL-1, biclopropylidene, and competitive impulse noncarcinogenic hypergol (CINCH) (di-methyl-aminoethyl-azide). All tests were conducted at MSFC. The first four fuels were provided by the U.S. Air Force Research Laboratory (AFRL), Edwards Air Force Base, CA. The U.S. Army, Redstone Arsenal, Huntsville, AL, provided the CINCH. The data recorded in all hot-fire tests were used to calculate specific impulse and characteristic exhaust velocity for each fuel, then compared to RP-1 at the same conditions. This was not an exhaustive study, comparing each fuel to RP-1 at an array of mixture ratios, nor did it include important fuel parameters, such as fuel handling or long-term storage. The test hardware was designed for liquid oxygen (lox)/RP-1, then modified for gaseous oxygen/RP-1 to avoid two-phase lox at very small flow rates. All fuels were tested using the same thruster/injector combination designed for RP-1. The results of this test will be used to determine which fuels will be tested in future test programs.
The assumption that the acridine orange (AO) color reaction may be used as an index of physiological activity was investigated in laboratory grown Escherichia coli. Spectrofluorometric observations of purified nucleic acids, ribosomes and the microscopic color of bacteriophage-infected cells stained with AO confirmed the theory that single-stranded nucleic acids emit orange to red fluorescence while those that are double-stranded fluoresce green in vivo. Bacteria growing actively in a rich medium could be distinguished from cells in stationary phase by the AO reaction. Cells from log phase appeared red, whereas those in stationary phase were green. However, this differentiation was not seen when the bacteria were grown in a minimal medium or when a variation of the staining method was used. Also, shifting bacteria in stationary phase to starvation conditions rapidly changed their AO staining reaction. Boiling and exposure to lethal concentrations of azide and formalin resulted in stationary-phase cells that appeared red after staining but bacteria killed with chlorine remained green. These findings indicate that the AO staining reaction may be suggestive of physiological activity under defined conditions. However, variables in staining and fixation procedures as well as uncertainties associated with mixed bacterial populations in environmental samples may produce results that are not consistent with the classical interpretation of this reaction. The importance of validating the putative physiological implications of this staining reaction is stressed.
Cell-to-cell transport of small molecules and ions occurs in plants through plasmodesmata. Plant roots are frequently subjected to localized anaerobic stress, with a resultant decrease in ATP. In order to determine the effect of this stress on plasmodesmal transport, fluorescent dyes of increasing molecular weight (0.46 to 1OkDa) were injected into epidermal and cortical cells of 3-day-old wheat roots, and their movement into neighboring cells was determined by fluorescence microscopy. Anaerobiosis was generated by N2 gas or simulated by the presence of sodium azide, both of which reduced the ATP levels in the tissue by over 80%. In the absence of such stress, the upper limit for movement, or size exclusion limit (SEL), of cortical plasmodesmata was <1 kDa. The ATP analogue TNP-ADP (mw 681) moved across the plasmodesmata of unstressed roots, indicating that plasmodesmata may be conduits for nucleotide (ATP and ADP) exchange between cells. Upon imposition of stress, the SEL rose to between 5 and 10 kDa. This response of plasmodesmata to a decrease in the level of ATP suggests that they are constricted by an ATP-dependent process so as to maintain a restricted SEL. When roots are subjected to anaerobic stress, an increase in SEL may permit enhanced delivery of sugars to the affected cells of the root where anaerobic respiration could regenerate the needed ATP.
Halobacterium saccharovorum synthesized ATP in response to a pH shift from 8 to 6.2. Synthesis was inhibited by carbonyl cyanide m-chloro-phenylhydrazone, dicyclohexylcarbodiimide, and azide. Nitrate, an inhibitor of the membrane-bound ATPase previously isolated from this organism, did not inhibit ATP synthesis. N-Ethymaleimide, which also inhibited this ATPase, stimulated the production of ATP. These observations suggested that H. saccharovorum synthesized and hydrolysed ATP using different enzymes and that the vacuolar-like ATPase activity previously described in H. saccharovorum was an ATPase whose function is yet to be identified.
Membranes from Paracoccus halodenitrificans contain an ATPase that is most active in the absence of NaCl. The most unusual characteristic of the enzyme is its pattern of sensitivity to various inhibitors. Azide and rhodamine 6G, inhibitors of F1F0-ATPases, inhibit ATP hydrolysis as do bafilomycin A1, concanamycin A (folimycin), N-ethylmaleimide, and p-chloromercuriphenylsulfonate which are inhibitors of vacuolar ATPases. This indiscriminate sensitivity suggests that this ATPase may be a hybrid and that caution should be exercised when using inhibition as a diagnostic for distinguishing between F1F0-ATPases and vacuolar ATPases.
The effect of microgravity on cellulose synthesis using the model system of Acetobacter xylinum was the subject of recent investigations using The National Aeronautics and Space Administration's Reduced Gravity Laboratory, a modified KC-135 aircraft designed to produce 20 sec of microgravity during the top of a parabolic dive. Approximately 40 parabolas were executed per mission, and a period of 2 x g was integral to the pullout phase of each parabola. Cellulose biosynthesis was initiated on agar surfaces, liquid growth medium, and buffered glucose during parabolic flight and terminated with 2.0% sodium azide or 50.0% ethanol. While careful ground and in-flight controls indicated normal, compact ribbons of microbial cellulose, data from five different flights consistently showed that during progression into the parabola regime, the cellulose ribbons became splayed. This observation suggests that some element of the parabola (the 20 sec microgravity phase, the 20 sec 2 x g phase, or a combination of both) was responsible for this effect. Presumably the cellulose I alpha crystalline polymorph normally is produced under strain, and the microgravity/hypergravity combination may relieve this stress to produce splayed ribbons. An in-flight video microscopy analysis of bacterial motions during a parabolic series demonstrated that the bacteria continue to synthesize cellulose during all phases of the parabolic series. Thus, the splaying may be a reflection of a more subtle alteration such as reduction of intermicrofibrillar hydrogen bonding. Long-term microgravity exposures during spaceflight will be necessary to fully understand the cellulose alterations from the short-term microgravity experiments.