Misc Best way to remove 1,4-Butanediol from a 1,4BD/ GHB Water Mixture

[snowlife]

I had a water mixture that contained both 1,4-Butanediol and GHB. I tested it in a freezer, and after several hours and it did not freeze which (I believe) indicated that there was sufficient amount of G sodium salts to prevent the high freezing point of 1,4BD and/or water. The mixture tasted quite salty, but it also possessed some of the oilyish quality of 1,4. And the physical effects of ingesting 5-7ml did not feel like a pure G (quick onset, 4 hours complete rebound etc.)

Could someone that is much smarter than me propose any ideas or solutions of a way to separate the two substances (or simply remove the 1,4BD) in an aqueous mixture?

I've read that 1,4 is slightly lighter (Molar mass 90.12 g p/ mol) than GHB (126.09 g/mol) -- would that mean that GHB would be heavier and sink to the bottom of the mixture? Allowing me to remove the upper portion of the solution.

Short of removing the 1,4BD all together (if that's not possible), is there any way to check the concentration of 1,4BD to GHB in an aqeuous mixture?

Thanks in advance! (if this should be in ADD Mods, please let me know)

 

[sekio]

The mixture tasted quite salty, but it also possessed some of the oilyish quality of 1,4.

Concentrated aqueous solutions of GHB will have that characteristic. Doesn't mean it has 14b in it.

would that mean that GHB would be heavier and sink to the bottom of the mixture?

No. Both 14B and GHB are miscible with water.

Short of removing the 1,4BD all together (if that's not possible), is there any way to check the concentration of 1,4BD to GHB in an aqeuous mixture?

Not to the layman.
You could always remove all the water and weigh & titrate the residue to see how much of it is an acid and how much is neutral.
Real fancy people would use a GC or HPLC.

I'm sorry, but this seems based on a misconception. (You don't make GHB directly form 14b anyway.) I bet you you probably just have GHB in solution.

For reference, you could seperate it by ion-exchange chromatography on a positive resin, or by distillation. Or you could just oxidise the remainder of the 14b to GHB (but that is synth talk)

 

[snowlife]

Thank you very much for a very informative reply. The reason I asked the question in the first place is a result of receiving a solution that started out as 1,4bd, and then was converted into gbl and then to GHB (I understand that you can't simply go from 14b to GHB). My concern was that the individual performing the conversion, might not be the best chem.

Having said all that, is it likely that a 1,4bd conversion to GBL -> GHB can result in a portion of 'unreacted' 14b? IF so could it be a large %? Because It definitely seemed that way, given the bodily effects of the solution in question, and also when I poured a little out on glass and let it evaporate, I wasn't left with a pure salt residue like when I've seen pure ghb evaporate before, but more of a white oily residue that is somewhat salty to the taste.

You could always remove all the water and weigh & titrate the residue to see how much of it is an acid and how much is neutral.

Could you elaborate a bit more on this, or is this something out of a layman's ability?

Lastly would checking the PH of the solution given the acidity of GHB prove anything in terms of concentration of GHB etc?

Many Thanks -- you've been very helpful.

 

[sekio]

would checking the PH of the solution given the acidity of GHB prove anything in terms of concentration of GHB etc

No, as pH and GHB concentrat ion are not directly related. The GHB can be present as either a free acid (pH low) or a sodium salt (pH high).

(It could also be un reacted GBL, but that's not likely.)

Also, look up indicator titration on wikipedia.

Now that I think more about this, you could also *try* makin it very alkaline (ensuring you have a maximum of the sodium salt, which is charged& polar) & extract it with a nonpolar solvent like hexane or heptane. The Heptane will wash the 14bdo and GBL out, the sodium GHB stays in the water. Adjust the pH back to 7 w/vinegar or somethin for human consumption