Scale-up accident
Wednesday, February 10, 2016
A reaction was increased in scale from 1 g to 10 g and the reaction mixture was not fully neutralized before beginning extraction in a separatory funnel. During extraction, pressure built up and the reaction mixture ended up all over the researcher and parts of the lab. Fortunately the researcher was wearing proper PPE. The reaction mixture also contained formaldehyde which created an inhalation hazard. Cleanup was done while wearing a respirator.
Review best practices for using separatory funnels
Fully neutralize acidic mixtures before adding to the funnel
Fill less than half full.
Vent from the stopper end (not the stopcock) toward the back of a hood.
For more tips see http://www.chem.ucla.edu/~bacher/General/30BL/tips/Sepfunnel.html.
When scaling up reactions ensure that all concentrations remain the same, prepare for greater temperature and pressure changes and rates of reaction.