Alster370 - 14-3-2013 at 13:22
A few months ago I processed a small amount of methyl ethyl ketone peroxide (~8ml). Once I had completed the reaction and extracted the mekp, I put
the remaining mixture to one side and completely forgot to get rid of it and clean the beaker.
So it has been sat for about two months at cold temperatures (2-6C) and I noticed these colorless crystals floating in the liquid. I don't know what
they are, but i checked the visual description of diacetyl peroxide and it states something very similar to what I have.
The mixture likely contained mostly mek, with small amounts of hydrogen peroxide, sulfuric acid and mekp.
Pictures attached below, any ideas?
Thanks.
Adas - 14-3-2013 at 13:24
Beautiful crystals. They might be some higher polymer of MEKP. Try lighting up one of them.
Alster370 - 14-3-2013 at 13:40
Put a small piece in a foil wrapping and stuck a fuse in it. No explosion, although it seems that when the fuse hit the compound, a the sparks coming
from the aluminium packet turned white, which makes me think the compound contains oxygen, which given the reagents would suggest its some sort of
peroxide.
Bot0nist - 14-3-2013 at 16:28
What was the source of the acid, mek, and H2O2? Were they fairly pure, or was the acid dark drain opener or the MEK dyed or adultuured?
After insuring some safety measures are in place, determine some of the physical and chemical properties of the crystal. That may help garner some
insight.
Alster370 - 14-3-2013 at 16:35
Sulphuric acid was lab grade, bought of ebay, as was the mek and H2O2, all were clean and all glassware used for the mekp synth hadn't been used
before, brand new out the box.
Il see if the crystals are impact sensitive tomorrow afternoon.
Bot0nist - 14-3-2013 at 18:04
I was meaning more along the lines of density, melting or decomposition point, solubilities, etc.
What makes you think it's energetic? I doubt it, but still take precuations.
Trotsky - 14-3-2013 at 22:56
Well, if it was found in aging MEKP, and it was free of impurities, it's reasonable to work from the assume that it may be energetic, especially as
peroxides are known to form on aging.
I have had some MEK that was contaminated with cyclohexanone. After making MEKP and after sitting, cyclohexanone peroxide crystals formed. They were
BIG crystals, too. They looked like those, but were significantly shorter- short and unusually wide for their length.
I don't know if I tried burning them or not, but they were moderately impact sensitive, and far weaker than TATP or MEKP.