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Hydrogen Storage -Ammonia Borane (AB) Loaded onto Mesoporous Carbon

Severity
Incident
Was Hydrogen Released?
Uncertain
Was There Ignition?
Yes
Incident Date
Incident Attributes
Setting
Equipment
Damage and Injuries
When Incident Was Discovered
Describe the incident, including corrective steps taken and their result.

During preparation of a new hydrogen storage material, ammonia borane (AB) loaded onto mesoporous carbon, an unexpected incident was observed. As with all procedures with new materials the work is conducted on a small scale and in a laboratory fume hood. They followed the procedures that they had used for absorption of ammonia borane onto mesoporous silica without incident.

To absorb the solid AB into a scaffold material they dissolve AB in a dry aprotic polar solvent, THF. The saturated solution of AB in THF is added to the mesoporous carbon material in a round bottom flask, stirred for 10 minutes to saturate the mesoporous scaffold with AB and then the solvent is slowly removed under vacuum. At this point the sample is assumed to be prepared and ready for transfer to a sample vial for storage.

The material (1:1 mesoporous carbon:AB) was exposed to the atmosphere for close to five minutes without incident and the round bottom flask containing the material was cool to the touch as they have always noted for the silica materials. In order to transfer the material from the round bottom flask to the storage vessel a stainless steel spatula was introduced to the round bottom flask. Upon touching the stainless steel spatula against the inside of the flask, the flask became warm to touch and then a small flame was observed to arise from the round bottom flask. The flask was immediately placed under a large glass crystallizing dish to remove oxygen and the flame was extinguished. After the flame was extinguished, the flask was then placed under nitrogen atmosphere.

Dry carbon materials have been reported to develop a static charge under vacuum. It is likely that using the metal spatula provided a grounding source to release the charge. This static charge may have been responsible for the flame and any exothermic reaction. Likely residual THF ignited.

Lessons Learned

In the future, this mesoporous carbon material and ammonia borane:mesoporous carbon material will be handled under anaerobic conditions (glove box) to prevent further incidents.

Key:

  • = No Ignition
  • = Explosion
  • = Fire
Hydrogen Incident Summaries by Equipment and Primary Cause/Issue
Equipment / CauseEquipment Design or SelectionComponent FailureOperational ErrorInstallation or MaintenanceInadequate Gas or Flame DetectionEmergency Shutdown ResponseOther or Unknown
Hydrogen Gas Metal Cylinder or Regulator 3/31/2012
4/30/1995
2/6/2013
4/26/201012/31/1969  3/17/1999
11/1/2001
12/23/2003
Piping/Valves4/4/2002
2/2/2008
5/11/1999
4/20/1987
11/4/1997
12/31/1969
8/19/1986
7/27/1991
12/19/2004
2/6/2008
10/3/2008
4/5/2006
5/1/2007
9/19/2007
10/31/1980
2/7/20091/24/1999
2/24/2006
6/8/1998
12/31/1969
2/7/2009
9/1/1992
10/31/1980
10/3/2008 
Tubing/Fittings/Hose 9/23/1999
8/2/2004
8/6/2008
9/19/2007
1/1/19829/30/2004
10/7/2005
 10/7/2005 
Compressor 10/5/2009
6/10/2007
8/21/2008
1/15/2019
  10/5/20098/21/2008 
Liquid Hydrogen Tank or Delivery Truck4/27/198912/19/2004
1/19/2009
8/6/200412/31/1969 1/1/197412/17/2004
Pressure Relief Device7/25/2013
5/4/2012
1/15/2002
1/08/2007
12/31/1969    
Instrument1/15/20193/17/1999
12/31/1969
2/6/2013
  11/13/73  
Hydrogen Generation Equipment7/27/1999  10/23/2001   
Vehicle or Lift Truck 7/21/2011    2/8/2011
12/9/2010
Fuel Dispenser 8/2/2004
5/1/2007
6/11/2007
9/19/2007
 2/24/2006
1/22/2009
   
Fuel Cell Stack      5/3/2004
12/9/2010
2/8/2011
Hydrogen Cooled Generator   12/31/1969
2/7/2009
   
Other (floor drain, lab
anaerobic chamber,
heated glassware,
test chamber,
gaseous hydrogen
composite cylinder,
delivery truck)
 11/14/1994
7/21/2011
7/27/1999
6/28/2010
8/21/2008
12/31/1969
3/22/2018
  6/10/2019
  • = No Ignition
  • = Explosion
  • = Fire
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