A laboratory research technician entered a lab to begin preparing samples that were to ultimately be purged in an anaerobic chamber (glove box) located in that room. As the technician walked into the lab, she looked at the chamber to see if it was adequately inflated. This chamber is equipped with a gas concentration meter, capable of simultaneously displaying the oxygen and hydrogen concentrations of the chamber atmosphere. Under normal operating conditions, the atmosphere inside the chamber is comprised of 0% oxygen (as intended/desired for an anaerobic atmosphere), approximately 2-3% hydrogen, and with the remaining balance being nitrogen (approximately 98-97%). Under such normal operating conditions, the hydrogen concentration inside the chamber is less than the lower explosive view more
While attempting to light the hydrogen flare inside a Metalorganic Chemical Vapor Deposition (MOCVD) system burn box, a small explosion occurred, blowing the back section of the burn box off. Hydrogen flow was shut down immediately, and this MOCVD operation was suspended. Researchers made the determination that this was a minor incident and there were no injuries.
The follow-up investigation determined that the MOCVD HEPA filter had become sufficiently loaded to the point where performance of the burn box exhaust ventilation system was significantly degraded. The static pressure created across the "loaded" HEPA filter equaled the operating static pressure of the exhaust ventilation system servicing the burn box. This resulted in a region of "dead air" in the view more
An individual inadvertently connected a pure hydrogen gas bottle to a chamber/glove box as opposed to a 10% hydrogen (in nitrogen) bottle that should have been used. [The wrong bottle had mistakenly been delivered, and the inexperienced individual did not know the difference.] The hydrogen concentration increased within the chamber to about 9%. Since there was insufficient oxygen in the chamber to support combustion, the hydrogen did not burn, and was quickly diluted with nitrogen.
A hydrogenation experiment was being performed under 60 atm hydrogen, inside a high-pressure reactor cell. The experiment was conducted inside a fume hood and left overnight. The hood caught fire during the night, resulting in fire damage to the fixture, hood, and exhaust duct, as well as water damage to much of the building. Based on the local fire department investigation, the fire started from faulty electrical wiring that was used to provide power for reactor cell heating. The electrical fire ignited solvent that was in a dispensing bottle inside the hood, which subsequently overheated the reactor cell, rupturing the seals. The rupture released hydrogen from the cell and attached supply tank, further fueling the fire. Nobody was injured in the incident, and damages were limited. It view more
NaAlH4 powder mixed with hexane was placed in two metal trays and dried by placement in a glove box antechamber under vacuum. After several days, the trays were moved into the glove box main chamber. As the powder in one of the trays was being transferred to a container involving scraping of a metal sieve and metal milling balls with a metal spatula, a portion of the powder in the tray spontaneously reacted rapidly, creating a pressure pulse which cracked the window at the back of the glove box. No injuries occurred, and the glove box window was resealed using tape within one to two minutes.
As part of preparing for material disposal, a small fire occurred within a fume hood as a researcher was combining several spent ammonia borane (AB) samples that had previously been stored uncovered in the back of the hood for 6+ months. These AB samples consisted primarily of two 40-gram products of a 50wt% AB in silicone oil that had been thermally dehydrogenated. A small amount of unreacted AB slurry is believed to also have been present.
During project clean-up, partially spent (thermally reacted) ammonia borane (AB) residue from a previous experiment was mixed with a small amount of water to rinse the residue from its container. The water reacted with the spent AB resulting initially in a large heat release followed immediately by a fire. It appears that the water addition view more
While performing hydrogen gas release experimentation by thermally reacting a slurry of ammonia borane powder in silicone oil in a plug flow reactor, a discharge port on the test reactor became loose. A foaming white product was leaking from the fitting and discharging in the direction of the heat tape and insulation (back over the reactor). As a result, hot, reacting slurry flowed out of the port and was exposed to air. In the presence of oxygen, the slurry ignited, producing a green flame. A small green flame was noticed at the leak site and flaming product dripped onto the hood deck surface. The flame at the end of the reactor was ~10-12 inches tall at the highest point. The flame on the deck was ~4-6 inches in height.
The incident occurred behind the lowered sashes in the view more
An incident occurred when Ti-doped sodium alanate was exposed to air, apparently resulting in an unstable compound that experienced a rapid exothermic reaction.
The sample consisted of mechanically milled NaAlH4 with 4% TiCl3 dopant which was prepared in an argon atmosphere. The sample was sealed and placed in the probe head of an NMR magic angle-spinning (MAS) rotor and spun at approximately 9,000-13,000 rpm. During the process, the sealing cap dislodged and exposed the sample to ambient air for a little less than 24 hours. When discovered, the sample was visually inspected and showed no evidence of oxidation. The sample was re-capped and returned to an argon environment for removal. Most of the sample material was removed using a small stainless steel needle, but a residual view more