03-24-02 09:29
No 287230
Well Baal has discovered that using TCE as a DCM 'substitute solvent' along with a Performic acid mixture..........can completely disintegrate a 400mm Allihn condenser in less than 1.5 seconds via excessive peroxide formation. Kaaaabooooooooooomm!!!!!!!!!!!!!
GODISNOWHERE
Shoot Narcs, Not Drugs
(Distinctive Doe)
03-24-02 11:06
No 287268
hope ya had those sun glasses on!!
Those who give up essential liberties for temporary safety deserve neither liberty nor safety
(Chief Bee)
03-24-02 13:18
No 287288
This is very interesting - under which reaction conditions did this happen?
(Master Whacker)
03-24-02 20:42
No 287357
SWIM actually had the same thing happen recently while using hardware store grade TCE in the buffered performic. Funny thing is reagent grade TCE worked fine, so the cheap grade stuff was fractionally distilled and found to be a mixture of chemicals which boiled over 67-95'C with about 5 major fractions in that range!!! God only knows what they're mixing in with the TCE, but whatever it is it catalyzes peroxide decomposition.
(Chef d'Equippe)
03-26-02 10:02
No 288022
Well it started as an experimental standard issue buffered performic oxidation, w/750ml>Iso,3000ml>TCE stirring away in a 10,000ml flask equipped with a 400mm Allihn condenser.Temp was at ~20c during the addition process. Temp was constantly monitored and it remained at ~20c for over 2 hours, so Baal decides to take a break from babysitting thinking that any exothermic tendencies have past. 10 mins later went out to check the temp, all is well @20c. Step out of the garage for 2 mins,upon returning Baal notices steam rolling out of the garage. Ran into the garage and couldnt find a trace of the condenser that used to be on top of the now volcanic flask. This was quickly submerged in the emergency ice bath, and resolvated with DCM right away. After further inspection, Baal found ~20% of the glass that was once a condenser, the rest was literally dusted. It was a rather peculiar experience altogether, but it was still a great time. Chemistry never lets one down, it is always interesting, exciting, and full of surprises. Anyhow, the now red colored Iso was solvated with DCM & was washed numerous times to remove most of the red coloring. 690g's of Iso was recovered, and this time DCM was used, and this was re-reacted with success using the standard performic protocol. Tough molecule I must say to withstand that abuse and still remain viable.
GODISNOWHERE
Shoot Narcs, Not Drugs