Author Topic: GBL purification from OTC product  (Read 2181 times)

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raybeez

  • Guest
GBL purification from OTC product
« on: February 20, 2004, 02:19:00 AM »
Questions similar to this have been asked before, but none seem to have really been answered. Swim has obtained an OTC product that lists butryolactone as an ingredient. Other ingredients consist of such things as ethyl acetate, butyl acetate, isopropanol, etc. Boiling points have been checked, and all found to have a lower BP then GBL.

Swim had the following plan to purify:

1) When H2O is added to the product and shaken, two layers form. Would it be reasonable to discard the non aqeuous layer, since GBL is miscible with H2O? Or would GBL stay in the non-aqueous layer? Something definately moves into the aqeous layer, as it becomes kind of oily. Would the GBL partition between the two layers?

2) If the top layer is discarded, and the remaining liquid is heated to 100degC, and boiled for a while, would it be safe to add NaOH, and synth NaGHB? Would this hydrolyse the acetate esters into carboxylics and alcohols, which would then boil off easier?

SWIM has a friend with access to a GC, can check out the final product for any other wierd impurities... That friend could also frac. distill it, but SWIM doesn't want to go there unless they have to.

I'd appreciate any suggestions.

silenziox

  • Guest
Distill
« Reply #1 on: February 20, 2004, 02:34:00 AM »
Why not just to distill the whole stuff and collect different fractions? It would be good distilling/purifying excercise and you'd get also other chems to play with?


raybeez

  • Guest
RE: Distill
« Reply #2 on: February 20, 2004, 03:08:00 AM »
Swim would love to, but again, it's Swim's friend that works in a lab with access to equipment, and Swim doesn't want to enlist his help, and have him risk a job unless Swim has to.

silenziox

  • Guest
Well then go to your favourite internet based...
« Reply #3 on: February 20, 2004, 03:13:00 AM »
Well then go to your favourite internet based auctionsite and buy the distillation setup from there and Do It Yourself  :) ...  I wouldn't want to consume anything without properly purified to get high..

Think the bright side of this.. Get the equipment, then do practice some basic skills, then work out the gbl out from the product and when you get that done advance to harder synths...

It WILL reward you  :)


Osmium

  • Guest
> Would the GBL partition between the two...
« Reply #4 on: February 20, 2004, 12:36:00 PM »
> Would the GBL partition between the two layers?

Yes. Repeated distillation is the only way to get what you want. Distill the GBL containing fractions too, simply boiling away the other stuff will not be sufficient to purify the GBL.


placebo

  • Guest
Vacuum distill first to rid most of the crap,...
« Reply #5 on: February 27, 2004, 06:08:00 AM »
Vacuum distill first to rid most of the crap, then slowly do STP distilation with a column. Then you will have relatively pure GBL, but still too dirty. Next, slowly titrate with 50% NaOH solution and you will probably notice discoloration of the solution proportional to the amount of impurities left.
Then boil off the H20 on a hotplate which will steam distill off most remaining impurities, then raise temp to 200c to drive off any remaining crap.

If you do not vac distill first, the STP dist will have too much crap in it and burn your product and most probably ruin a flask.