hCiLdOdUeDn (Hive Addict)
05-25-03 21:40
No 435534
      DMT extraction problems  Bookmark   


God, I especially need your help.

SWIM attempted to extract DMT from 118.0g of Mimosa Hostilis root bark using the standard A/B extraction method. This is what swim did.

1) Ground up 118g rootbark until it was a mostly fine powder and some stringy plant material.

2) Added the rootbark to the jar and added 500mL of 5% HCl solution and let it soak for 48hrs.

3) Filtered via buchner funnel and returned the rootbark for further extraction

4) Extracted 2x more with 500mL 5% HCl by heating the jar to 50C for 1hour each, and filtered on the buchner.

5) Left swim with 2L of dark brown/red solution.

6) Defatted with 3 x 100mL naptha. Discarded Naptha layer via separatory funnel. (emulsion took several hours to clear)

7) Basified to pH 11 using Lab Grade KOH. (well the solution turned a dark grey color when swim stopped), while under strong magnetic stirring, 2 drops at a time.

8) Attempted to extract the DMT using 3 x 150mL Naptha. Stirred 2L of the basified solution with 150mL naptha 3x using a magnetic stir bar, and poured into a seperatory funnel, seperated the Naptha/emulsion layer and kept in a jar overnight until the emulsion layer phased into the bottom liquid layer.

9) Poured the Naptha combined extracts (about 450mL worth) onto a large pyrex dish and it fully evaporated with a fan in 8 hours.

 There were no crystals, but about 10mg or less of a thin yellow film which wouldnt crystalize. Swim was confused big time and also very dissapointed.

What went wrong? Swim think he didnt basify strongly enough or extract with warm enough naptha(naptha used was room temp). Is that important to do?

Swim saved all solutions and rootbark. He reduced the basified solution to about 800mL and made the pH to about 2 again. He further extracted the rootbark with 1500mL of 5% HCl solution on the hotplate at 75C overnight to extract more goodies?

He plans to combine the extracts and earlier solution and reduce the volume to about 1000mL and extract with xylene. Will xylene work as well for the goodies? I know it works well to extract MDMA base, a bee would think its a better choice than naptha.

I really dont know what went wrong. My extraction procedures are usually really good, I have good technique and never throw out a liquid/solid until the extraction worked out.

 Please help swim on why he didnt extract any DMT freebase the first time. Also, swim had about 50mL of an emulsion layer in a beaker and left the beaker to sit during the whole process (5 days) and when he looked in the beaker it all evaporated and there were some crystals about the size of salt grains, diamond shaped and flat. He suspected this might have been DMT, but why in the water solution? This was also water soluble. So did swim create DMT.HCl and not basified it strong enough? 

So, so confusing, SWIM really wanted to try DMT. crazy
05-26-03 03:42
No 435585
      Hcl concentration  Bookmark   

Your Hcl concentration is much,much to high!
instead of 5% use 1% or 1N Hcl.
Hcl and oxygen oxidizes your DMT to noting.
and you don't have to heat it,let time do the job.
(Hive Bee)
05-26-03 06:43
No 435613
      hope this helps...  Bookmark   

It sounds like you didn't basify enough. The solution should go from clear red to chalky gray, then finally to inky black when basification is complete. As reported by others, I have stopped testing pH at this stage, just look for that inky black to replace the chalky gray streaks. I do all phases of extraction in a beaker under gentle magnetic stirring, then transfer to sep funnel.
     I'd have to agree that 5% HCl is way too strong, but I'm sure there are other opinions about that. Some say the acid cannot be too strong to rip up the desired molecule, but I've always used pH 1.0-2.0 distilled H2O with perfectly satisfactory results.
     Heating your non-polar solvent will speed things up but shouldn't be required. I'd be careful not to overheat, I always keep all phases of mhrb extractions at 50* C or lower.
     Xylene will work for extraction, I'm sure I tried it once but I used more than one solvent in that particular extraction. I think toluene is a better choice since the bp is lower and you're more likely to get it evapped without leaving it's aroma behind.
     Those crystals you saw in dried emulsion were not DMT HCl! They were whatever caustic you used (KOH?).
     Hope this helps, don't give up!
(Hive Addict)
05-26-03 08:09
No 435624
      Well if i used too much HCl and it did damage...  Bookmark   

Well if i used too much HCl and it did damage the DMT molecule then that explains a whole lot. Im going to do another extraction and basify till black, and extract with xylene then ill report back to you.

So does too strong HCl really damage DMT? I hope not...
(Hive Addict)
05-26-03 08:53
No 435631
      There were no crystals, but about 10mg or less  Bookmark   

There were no crystals, but about 10mg or less of a thin yellow film which wouldnt crystalize. Swim was confused big time and also very dissapointed.

Sounds like the goods right there...
some things swim would have done differently(basically piggybacking on what both calcium and freakyD said):

-he wouldnt have used heat (this causes it to oxidise much faster lowering yeilds)
-he MAY have used slightly less acidic DH20 (swim always just added pH2 H3O+, enough to cover, plus some...) -swim never noticed too great a loss in yeilds from over acidifying- but he suspects that IN COMBO w/heat is a large source of swiys loss
-he too adds NaOH until the solution stops changeing color- itll bee a dark grey- dark dark- with a soapy texture to the liquid- dont worry too much about over basifying (just make sure to do a few quick backwashes at the end!)
-he would use only naphta (strictly because that is all he had ever used, and it worked great!)
-did swiy take some time when he pulled the freebase?  Or did he just let it settle, and separate?  Although swim wasnt a chemist bee- all he knows is what worked for him- he'd let the final pulls sit for at least 4-6 hours a peice, usually overnight!  Just to make sure the good stuff migrated.  Once again, just an uneducated bee's experience!

If everything was saved- remember, swiy gets about 3 pulls from the basified solution...also, if the final product was oily, that means the defat wasnt up to par- either more filtering, and/or more care with the defat (swim'd take a full 24 hours to do 3 defats).  Also, swim suspects that adding heat during the h3o+ soaks is more apt to pull oils into the mix- making defatting that much more of a nesessity.

patience grasshopper..., its right around the corner!wink

shit...I found out it was all just one big manic episode!
(I'm Yust a Typo)
05-26-03 10:58
No 435653
      you shouldn't let it 'sit' for 4-6 hours, you...  Bookmark   

you shouldn't let it 'sit' for 4-6 hours, you should shake it. Unless that gives you the bastard emulsion from hell.
(Hive Bee)
05-26-03 12:38
No 435673
      why not break the emulsion  Bookmark   

Instead of waiting out on the emulsion to clear naturally, break the emulsion free by filtering through celite?

Just work it baby!
(Hive Addict)
05-26-03 12:41
No 435674
      it'd most definatly form nasty emulsions...  Bookmark   

it'd (shaking) most definatly form nasty emulsions...

edit: oh yeah, warming the naphta before use is always a good thing, just make sure it isnt warmed in the container it came in (specially if it came in a yellow plastic container- it'll pull some super-yellow shit over into the final product...although dont worry if its pale-yellow, thats somewhat normal due to a little oxidation)

shit...I found out it was all just one big manic episode!
05-26-03 13:20
No 435691
      tartaric acid instead of Hcl  Bookmark   

you could also use tartaric acid instead of Hcl,this can easely obtained because it is also used in home brewing of wine/beer you can buy it from online homebrewing companies.
(Hive Addict)
05-26-03 13:35
No 435693
      the rootbark could also possibly bee a/the...  Bookmark   

the rootbark could also possibly bee a/the source of low yeild.

Swim had heard of one 'reputable' vendor who was selling straight up bark as root-bark -but this was a little over a year ago.

shit...I found out it was all just one big manic episode!
(Hive Bee)
05-26-03 14:13
No 435702
      Something tells me...  Bookmark   

...that this whole thread belongs in the newbee forum!

Anyway, try it again, and be patient. Every DMT extraction that has worked well for me has done so because I wasn't in a big hurry. Everytime I've gotten fancy ideas about finishing up in a hurry I've fucked my yields.
     Heating the initial acid extraction of the rootbark is a tricky thing. I've found that keeping the temp at or below 50 works great, but higher temps turn the bark pulp into a gooey mess that doesn't drain well and picks up all kinds of unwanted crap you have to get rid of later.
     For extracting the basified aqueous sol'n, I like to stick it on the hotplate stirrer, warm it to 50 C and gently stir with a big stirbar. An hour or two later I drop it all into a sep funnel and have very little emulsion trouble. I've found pet ether of some sort works better than DCM due to the fact that DCM rips other stuff along with the alkoloids, making clean up a nightmare. I follow the initial extraction with another a/b which I then extract with DCM, because it evaps sooo clean.
     That's my two cents worth on mimosa hostilis rootbark extraction.
(Hive Addict)
05-26-03 15:19
No 435712
      Thankyou everyone  Bookmark   

Thanks, im gunna try this now, nice and slow. Ill report the yields back...
05-26-03 17:30
No 435736
      Shouldn't this be in tryptamine chem?  Bookmark   

Shouldn't this be in tryptamine chem?
(Hive Addict)
05-26-03 17:40
No 435739
      Same Problem  Bookmark   

I"ve blown a lot of hostilis by this point.. I REALLY don't like that extraction, and while a gentle naptha soak for a week might work, i feel like I haven't got the scientific method if it doesn't work right.. and I really want it to work right..

  What I discovered was that the emulsions had a lot of saponions in them.. ( i got to wash out the sep funnel w/ MHRB "SOAP" after the basification failure.

  I believe that a sodium carbonate treatment prior to the Acidification will cause the carboxl saponin precursors to precipitate out.  I would do a cellite or cellulose packed buchner vacuum filtration after acidification and 1st defat wash.  Then defat 2x more.   Then proceed to the base/org extraction.  I haven't tried this yet, but it is where i ended up as the next thing to do after my recent failures.

Infinite Radiant Light - THKRA
(Chief Bee)
05-26-03 17:58
No 435742
      Shrooms @ The Shroomery, Xtraction in this forum  Bookmark   

Extraction of chemicals or drugs from plants or OTC products always belongs in "Chemicals & Equipment", unless it is specifically intended for the manufacture of meth, in which case it goes in the Stimulants forum.

If you read the sticky post in the Tryptamine Forum ( Post 412519 (Lilienthal: "Tryptamine forum improvements", Tryptamine Chemistry) ), you'll see that extractions and shroom growing are depreceated in that forum, as it was originally created for the discussion of the synthesis of tryptamines and lysergide derivatives.

Extraction of alkaloids is most definitely something classified as "Basic Chemistry & Techniques" rather than "Drug Related Chemistry", if you look at the broad categories on the front page.