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Freebase solubility in h20? Options
 
Oncewas
#21 Posted : 1/30/2010 6:09:03 PM
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Nevermind the extraction failed completely. Fucking a. Well, hopefully someone can learn from swims mistakes. Too broke to do any more extractions so um, it's been fun.
 

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narmz
#22 Posted : 1/30/2010 9:46:46 PM

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Did you already flush it all down the drain or do you still have your solution? Maybe it can still be salvaged, if you had spice in there to begin with, it should still be there... Personally, I'd evap it all, pull it with heptane, and go for a freeze precip, assuming it's freebase.
Everything I post is made up fiction. SWIM represents a character who is not based in or on reality.
 
Infundibulum
#23 Posted : 1/30/2010 10:19:12 PM

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mydriasis wrote:
Nevermind the extraction failed completely. Fucking a. Well, hopefully someone can learn from swims mistakes. Too broke to do any more extractions so um, it's been fun.

What exactly happened? how can others learn from SWIY's mistakes if he doesn't describe the mistakes?

Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
amor_fati
#24 Posted : 1/30/2010 10:40:28 PM

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Is SWIM correct in assuming that SWIY had extracted with xylene, salted with vinegar, and potentially had product in 200mL of vinegar solution? Then the fact that SWIY couldn't get it to precipitate out and couldn't extract it with xylene back out of the solution led him to believe the extraction had simply failed and there likely wasn't even any product in the solution at all? More detail would help, as the product can always be salvaged one way or the other.
 
Oncewas
#25 Posted : 1/30/2010 11:03:12 PM
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Amor that's pretty much what happened.

Well swim tried pulling with xylene. Had an emulsion. Waited a few hours in a hot-water bath. Put 10 more grams of naoh in it. It all dissolved. Still an emulsion. Tried pulling the top part of the emulsion just to get whatever swim could and the xylene soaked up some paint from a tool swim was using. That's when swim just said fuck this.

Nuetralized the ph with vinegar. Dumped it into the garden.

What the problem was, I have no idea. Probably more than likely the error of the extractor.

I really don't think adding base to a vinegar solution saturated with alkaloids is a good idea. If it does precipitate it must be magic. Thanks for the help though it was appreciated.

Taking a break from extracting, chemical exposure(and inhalation), naoh welts(even while wearing gloves), cost, illegality, just not worth it right now. Maybe aya is more for swim.
 
amor_fati
#26 Posted : 1/31/2010 6:16:55 AM

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That's rough, sorry to hear.

Well, whenever SWIY gets the inkling and resources to give it another go, consult the handbook a bit before deciding how to go about it. It's not yet complete, but it's already fairly comprehensive in terms of the ins and outs of extraction and will at least point SWIY in the right direction. Use a good reliable tek as a starting point and explore from there. It's a learning process, even SWIM made his fair share of mistakes in the early days.

Take it from SWIM though, toss the toxics, and invest in a few simple, wholesome items: d-Limonene, pickling lime, vinegar, fumaric acid, baking soda, and a food dehydrator. SWIY will be set for mescaline and DMT and the food dehydrator is infinitely useful for the entheogenic hobbyist (evaps and drying botanicals).

mydriasis wrote:
I really don't think adding base to a vinegar solution saturated with alkaloids is a good idea. If it does precipitate it must be magic. Thanks for the help though it was appreciated.


Well, it's never been properly tested. Such processes would generally call for little to no excess of acid. It would also have to be known that there is in fact product to precipitate (a simple evap of the vinegar would determine that). This absolutely could not have been the reason for failure (especially considering all the other problems apparent) if xylene wouldn't even pull the actives (how did SWIY even determine whether they were in there? Such details would be important for the community to help SWIY).
 
Oncewas
#27 Posted : 1/31/2010 3:45:49 PM
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Well swIm assumed there actives where there UNLESS xylene and vinegar react. The reason why is swim shook the xylene and vinegar(when salting from the xylene) and the solution turned cloudy white. That's when swim smiled and said okay this is done. It could have been a reaction but I highly doubt xylene would react without a catalyst(unless the aluminum in the lid + acetic acid provided this).

The tek was pretty much figured out but swIm had this brilliant idea to try this out instead of evapping the vinegar. swim was writing what swIm thought was his own tek for chaliponga without defats but infundibilum corrected swim and everything he thought of had already been done(so swim couldn't have been too far off).

swim will get back on the horse and try this again once they can afford to do so, unfortunately swim can't in the near future.
 
Infundibulum
#28 Posted : 1/31/2010 5:37:27 PM

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mydriasis wrote:
...swim shook the xylene and vinegar(when salting from the xylene) and the solution turned cloudy white. That's when swim smiled and said okay this is done.

Well, if one shakes xylene and water together both solvents get cloudy as they separate but become clear again upon total separation. The fact that the vinegar remained cloudy does not mean that all of the alkaloids migrated to the vinegar.

Ideally, one needs to salt a xylene pull 2-3 times to get everything out.

The think SWIM does not understand is what happened when the vinegar was based. OK the alkaloids did not crash out, but some naphtha would have picked the spice up. Why did SWIY use xylene after the (re)basind step of the vinegar and what was he trying to do? dmt cannot be precipitated out of xylene and xylene takes approx 1 million years to evaporate.

Anyway, it was a bad thing that SWIY chucked everything out. Usually everything can be salvaged to a great extent and people with horror scenarios have managed to get a decent yield after asking for troubleshooting! Even added contaminations (e.g. melted plastic spoons in the solvent) can be salvaged. Just remember that an extraction per se is an attempt to "salvage" the spice that is trapped inside the plant material!

The worst thing is to get disappointed and say aw, fuck it and chuck everything out!


Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
Oncewas
#29 Posted : 1/31/2010 5:46:26 PM
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Well if you can find a way to pull 5meo oxide or nndmt oxide with naptha let us know. As far as I have been told it is impossible(says 69ron). Unless your swiy has other experience?

The reason why swim did this was so he didn't have to evaporate the xylene but if that's going to fail then swim figured screw it, pull with a NPS. If 10 grams of naoh(in an already naoh saturated solution) + hot water bath for a few hours wasn't enough to cure the emulsion than it's pretty doomed imo.

So after shaking xylene and vinegar and wait 4 hours and the solution was still highly cloudy is not a good indicator that something migrated into the water solution(no emulsion and layers completely seperated)? What was that then? Why else would vinegar turn milky after being shaking with xylene and allowed to seperate?

Thanks for the suggestions though.

Yea it just wasn't worth the hassle honestly. Cuz then swim would have had to nps->acid->base->nps->acid. Just got to be a little overwhelming so swim said screw this it's not even worth the supplies the risk or the time.
 
Infundibulum
#30 Posted : 1/31/2010 7:00:25 PM

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Metta wrote:
Well if you can find a way to pull 5meo oxide or nndmt oxide with naptha let us know. As far as I have been told it is impossible(says 69ron). Unless your swiy has other experience?

Amazing logic!

For once, why did SWIY assume that 5meo is necessarily present? SWIM has extracted chaliponga that had no 5meo present at all, this he knows by bioassay though.

Secondly, why assume that nndmt (and 5meo) are in their oxide forms? In all seriousness, SWIM's last chali extraction (A/B with xylene then FASA) yielded the whitest spice he has ever seen. There were marginally any oxides.

It is basically an assumption that the dmt in leaves is in oxide form.

But anyway, the easy way to get the oxides as well as the standard freebases is to evaporate the vinegar solution down. This helps because one gets the crude acetate salts, but also one sees that he's got something to work with. Then make an acetates/sodium carbonate (or other base)/water paste, let it dry and pull with acetone, IPA or ethanol.


Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
Oncewas
#31 Posted : 1/31/2010 7:08:15 PM
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Ahhh it appears the assumptions are what always bite swim in the ass, lol. No 5meo though? That is interesting. DMT must be active sublingually than, hence the tea-bag quid tek.

that makes more sense, it's kind of like a dry tek. Good advice thanks infund. perhaps another time Smile
 
Infundibulum
#32 Posted : 1/31/2010 7:11:59 PM

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Metta wrote:
Ahhh it appears the assumptions are what always bite swim in the ass, lol. No 5meo though? That is interesting. DMT must be active sublingually than, hence the tea-bag quid tek.

that makes more sense, it's kind of like a dry tek. Good advice thanks infund. perhaps another time Smile

5meo yes, but not always! it may be too little or just enough (e.g. for a quid). Wink

Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
amor_fati
#33 Posted : 1/31/2010 7:44:42 PM

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Infundibulum wrote:
But anyway, the easy way to get the oxides as well as the standard freebases is to evaporate the vinegar solution down. This helps because one gets the crude acetate salts, but also one sees that he's got something to work with. Then make an acetates/sodium carbonate (or other base)/water paste, let it dry and pull with acetone, IPA or ethanol.


Evaporating the vinegar is what SWIM would always suggest for such a situation. Otherwise it's largely left to chance whether there are actives and whether they can be retrieved.
 
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