(Official Hive Translator)
|Separation of GBL/butanediol - quick help needed!||Bookmark|
I have a purely hypothetical question for you. The question of uttermost importance and urgency. It already has been asked a year ago (Post 241813 (placebo: "GBL - BDO seperation?", Methods Discourse)), but 'nuffin come of it', alas.
So. Suppose, one had a mixture containing of, say, 90+% GBL and 10-% 1,4-butanediol.
How would one go about thorough cleaning of GBL w/out fractional distilling? (suppose, one has no means of fractional distillation)
Thus far i have two thoughts:
1) Dump in some baking soda (as in Post 283023 (Chromic: "GHB synthesis - a must read", Methods Discourse)), convert to Na-GHB. Then extract the remaining butanediol with some NP solvent.
- what solvent will extract BDO better than water? Will any?
- can steam-distillation bee substituted for extraction, i.e. - DOES BDO steam-distill?
2) Another possibility - that is, in case BDO is REALLY hydrophyllic is to dilute the mixtr w/water and salt GBL out.
The questions are:
- how efficient this could bee? (i.e., how much GBL is going to bee wasted)
- will this work at all?
PLEASE, bees, help SWIM in this hypothetical situation if you can, and as soon as you can!
Thanx in advance,
(Stoni's sexual toy)
|Extraction will not work well, BDO is pretty ...||Bookmark|
Extraction will not work well, BDO is pretty polar.
You could evaporate everything down after basifying, and dry the solids in a desiccator over conc. H2SO4. It will absorb the BDO, so it is lost.
Both compounds don't steam-distill very well, I think that won't work either.
Maybe NaGHB can be purified by crystallization from IPA, evaporation of the solvent should leave a mixture rich in BDO behind.
> Another possibility - that is, in case BDO is REALLY
> hydrophyllic is to dilute the mixtr w/water and salt GBL
I think you might rather salt out the BDO, I guess it will separate first from a strong aqueous NaGHB solution.
> how efficient this could bee? (i.e., how much GBL is going to bee wasted)
I wouldn't expect a lot of efficiency, it might take quite a while to work out the best separation conditions.
> will this work at all?
Why do you want to separate the two at all? Just go ahead, drink the GBL/BDO mixture dissolved in a small amount of pepsi. Have more pepsi around, the taste is evil!
No need to convert it into the Na salt first and separate them from each other.
I'm not fat just horizontally disproportionate.
I'd just drink it as it is, if it's pure enough to be drank in the first place. If not, go ahead and steam distill (throw out a bit of the "heads" just as with ethanol if you're concerned there might be any low BP crap in it). If you get any BDO over, don't worry, it's not going to hurt you. In fact, it tastes better than GBL/GHB and adds to the buzz.
Don't be surprised if your distillate smells very sour, that's the taste of the GHB... and remember it's quite nasty tasting (in ways, I find it worse than GBL). Rancid butter apparently has a close cousin of GHB in it -- butyric acid. Although the sodium salt is quite agreeable to the palate, the free acid is not.
If you insist on making NaGHB and removing most of the BDO, add the baking soda, ten parts water, let it reflux 30 minutes and then distill off most of the water (or, if you have it A.C.S. grade NaOH and you can drop the reflux time to about 3-5 minutes). I'm pretty sure BDO's BP is around GBL and it should boil off at somewhere around 1 part BDO / 10 parts water.
(not quite as irritable lately)
|Assuming you did the conversion with the copper ...||Bookmark|
Assuming you did the conversion with the copper chromite catalyst (thanks Rhod) and then distilled, you have a mix of both, but now free of the insidious catalyst. The two can't be seperated by fract. dist. as they are only about 5c apart anyway. But if you make up a concentrated solution of NaOH and add slowly to convert the GBL to NaGHB the BDO will seperate nicely and could be seperated easily with a sep funnel. But any time SWIM did it the reaction was so succesful (i.e. >95%) that it was not worth the trouble, and due to BDO's longer onset and effect, the small amount was a welcome combination. It was such a small amount overall as to not effect the taste, but add to the experience. i.e. smooth out the comedown.
As for taste, we know the tiny difference in PH up or down makes significant difference, but at it's best, I would describe the taste of NaGHB as that of sherbet, slightly tart but sweet and actually pleasant, I could eat a spoonful without a drink.
Intelligence is not the recall of knowledge, but the ability to use it. (Rainman was a retard)
|Well, I guess there is no accounting for taste.||Bookmark|
Well, I guess there is no accounting for taste. In my oppionion, GHB didn't taste like sweet sherbet. It tasted like very salty soap. I hate that stuff, but the effect is pretty cool compared to alcohol. I guess you're all going to tell me it's because your stuff is cleaner.
I have heard several other people compare the effects of GBL and NaGHB as well, but I guess maybe they have been too drunk when doing the comparison, because GHB is a lot different from GBL and much nicer.
By the way, to completely mask the taste of BDO or GBL, drawn some up into a syringe and inject it into a closed gelcap. The gelatine stays solid at least for long enough to swallow it. Easy as abc and no pain! You know who to thank.
And just to clarify, BDO and GBL are not 5 C apart but 25.
(Official Hive Translator)
|Thank you, guys! I really appreciate your help.||Bookmark|
Thank you, guys!
I really appreciate your help.
Too bad SWIM has nothing to report thus far. Here's what happened; maybee someone who's had experience w/this rxn (Placebo?) can give him an advice.
A 250 ml flask was equipped w/a thermometer & a air condenser (well, sort of - a 25cm x 1cm tube). A hose leading to outside of the apartment was attached to the condenser as not to accidentally blow the place apart
55mls BDO + 4g catalyst.
(Guess the making of it is the most important part, but SWIM's followed Placebo's directions as close as possible, care being taken as not to contaminate the catalyst w/SO42- and Cl- at all times).
Heated on a gas stove (metallic net interposed above the flame).
Dehydrogenation started at ~175 C! Yes! Tiny fine bubbles, which definitely created pressure (H2 evolution was tested by briefly plugging the out-hose w/SWIM's tongue).
Heating was cont'd for 4 hrs - the temp gradually rose to 210 C (it seemed that in the beginning, increasing the heat just led to more H2 effervescence, but not to temp. increase! SWIM's not 100% positive about that, though.)
Some liquid was definitely boiling/refluxing inside the flask at the time (i assume, GBL). Also there was noted a specific, very unpleasant smell (SWIM's never tasted/smelled GBL (nor has he ever had GHB, for that matter)) - it was completely unlike 'gasoline', rather like.... Well, i'm not sure. Somewhat similar to spoiled butter (is that GBL or some imputity? Help!). The taste of the insides was bitter (however, some BDO'ic taste was also present).
Another thing SWIM noted is that the catalyst changed in appearance from utterly black to sorta brownish, just a lil' bit. To check if it's lost activity, some more catalyst was added and it did NOT lead to any more H2 evolution. Some 4mls BDO was added and it DID lead to more H2 evolution. The mixtr was heated for further 2hrs.
When it was cooled and measured, it amounted to only 40mls! (WTF? Where did the rest go? Got carried away w/hydrogen? Definitely it wasn't boiled off as the 'condenser' held the temperature well - still, i guess, will have to try a water condenser the next time. What will the experienced ones say on this matter?)
So. As you can see, thus far all looked well. Now i'll get to the part where the problems beegan.
SWIM decided that he wasn't going to distill the stuff but rather cheat a little (YES! This is the phrase with which all failure reports are usually beegun!)
He thought he'd just dump in some water/baking soda, reflux it till complete convertion to NaGHB (30mins, according to Chromic!), THEN filter (the viscous mixture w/the fine, fine Cu-chromite powder was definitely unfilterable), xtract the unreacted BDO w/some CHCl3 and, - eh - like, voila.
An idiot! Yes. He could've at least 1st dilute the mixtr w/water and THEN filter it.
Anyway. He didn't have any soda in the house so he added K2CO3 instead. And boiled the mixtr for about 2 hours. The smell didn't disappear. The catalyst changed in appearance to brown and its consistency beecame fluffy and very filterable. Definitely reacted. An aliquot was taken and xtracted w/chloroform - upon evaporation it yielded some bitter liquid w/that characteristic unpleasant smell and taste completely unlike that of BDO. The liquid itself was brown and muddy.
WTF! If it was GBL, then it DIDN'T hydrolyze w/K2CO3 in 2 hours!
A sample of the liquid was active in a not-unpleasant way, different from BDO - but of course SWIM wasn't going to use it as is. (Ewwww).
Then it was boiled for yet further 2hrs, xtracted w/chloroform (didn't get rid of the yellow coloration!), most water evap'd, the mess xtracted w/EtOH, alcohol evaporated to leave a brown slurry that was completely inactive.
So. Of course, you're gonna tell me, the best way would bee to distill the mixture and then work-up the distillate. Alright. But still, here are some questions which i would very dearly like to have your opinion about:
- what if SWIM diluted the rxn w/water, filtered and then hydrolysed? Anyone had such an experience?
- HOW LONG does it take for a conc. NaOH solution to quantitatively hydrolyse GBL?
- Can someone describe in detail (yes, i've read all the previous descriptions, but still) how GBL should smell and taste?
Placebo, i am especially interested in your experience with this reaction, you must've had quite a bit of it - and, BTW, i am profusely grateful to you for your work and inspiration! I am truly honoured to at last make acquaitance with you on this board
|As much as I know||Bookmark|
I can't help you with the reaction from BDO -> GBL as I've never pursued it.
>SWIM decided that he wasn't going to distill the stuff
You really should distill. People distill their ethanol...!
>He thought he'd just dump in some water/baking soda
You must use 10 parts water, 1 part NaHCO3, 1 part GBL. Then boil 30 mins. Any less water will slow down the formation of NaGHB. Na2CO3 also works well.
Whatever you do, do not use any grade of NaOH that is not A.C.S. or similar. I've poisoned myself by taking such short cuts, and I shutter to think of the damage I've done to my body. DO NOT DO IT.
If you don't have NaHCO3, K2CO3 should work just as well, just adjust the #s for the base (keep the 1:1 ratio), and keep the same amount of water.
>The smell didn't disappear
The smell should be completely gone to indicate a completed reaction. The solution will also no longer be basic. If there's any BDO it will remain in the water, unaffected, of course.
>it yielded some bitter liquid w/that characteristic unpleasant smell and taste completely
>unlike that of BDO. The liquid itself was brown and muddy.
Without a doubt, that is GBL.
>If it was GBL, then it DIDN'T hydrolyze w/K2CO3 in 2 hours!
I bet you took short cuts on the water. Use 10g water to 1g GBL.
>A sample of the liquid was active in a not-unpleasant way, different from BDO
>but of course SWIM wasn't going to use it as is. (Ewwww).
A big dose of GBL should hit harder and faster than a similar dose of BDO... a big dose you can feel within 5 minutes of taking it... if you weren't tired in the least bit, you'll be floored and unconscious in 15 minutes only to wake up 3.5-4 hours later, and say "what the fuck was that?" I don't recommend you test it this way!!! ... with BDO you'll still be unconscious.
>(didn't get rid of the yellow coloration!)
Yeah, I get that from the GABA -> GBL conversion too. It's odd. I think it's some sort of GBL breakdown product, you will also see it happen if you distill GBL without a vacuum (it's not a significant loss tho).
>So. Of course, you're gonna tell me, the best way would bee to distill the mixture
Yes! If you distill the GBL you will get a liquid (BP ~200C) that has a chemical scent to it, it's not very strong, but it's very memorable. A drop of it will eat a hole in styrofoam and in your varnish. It will also discolor PETE plastic in a couple hours (store in HDPE!). If you dissolve it into water, it will not lose that scent right away, but it will change to the sour nasty smell of GHB. GBL's taste is very mildy bitter, but more so disagreeable. Do not drink it straight as it will peel off a layer of your muscous membranes. It's nasty stuff, and I recommend a minimum dilution of 1ml/30ml aqueous before you ingest it. (preferably more, preferablly add something acidic to turn it into the benign GHB)
>HOW LONG does it take for a conc. NaOH solution to quantitatively hydrolyse GBL?
~5 minutes with mild heating. It's a very exothermic reaction. Dissolve the NaOH in water, then very slowly add GBL.
>how GBL should smell and taste?
I hope that should help? A free GHB/GBL/water solution will smell something like rancid butter. Pure GBL has a very mild scent, which does not change on addition of water (but will with time).
Also, be very careful with GBL/BDO. They're dangerously addictive if used more often than once in a blue moon, and any bee on this board who has played around with them for any significant amount of time will tell you the same story.
First of all that's some good information.
I was wondering what kind of poinsoning did you expirience with industrial grade NaOH?
The poisoning feeling consisted of stomach upset and vomitting before a euphoric dose was reached... my girlfriend puked as well, it was terrible stuff.