Nitration with 100% nitric and 96% sulfuric acid is always a bi tricky, it could easily end up with something what you would like to avoid, just as in this case.

The phenolic compound what was nitrated was first dissolved in 250 ml sulfuric acid, sulfonated at 110 °C, then 200 ml of 1:1 mixture of 100% nitric and 96% sulfuric acid was added slowly, while the reactions temperature was maintained at 60 °C. During the reaction a massive foam was generated what unfortunately left the flask on a sidearm with some nitrogen oxides what generated from the reaction mixture.

So what is seen on the pictures: the yellow thing in the flask is the foam of the reaction product suspended in a lot sulfuric and nitric acid; the reddish-black thing at the side of the flask is some gunk and the green colored foam is a reaction intermediate what sadly escaped from the flask (bottom picture).

9:30 pm • 4 February 2015 • 246 notes • View comments