official extraction help thread

[psilocybin]

Any questions or problems you may run into during an extraction can be asked to get other members input in this thread.

 

[dmt_awehhaea]

Just do two 50mL extractions. That way, you shouldn't lose everything if something goes wrong.

Unfortunately that would mean it takes twice the materials/setup which I don't see any reason to do/buy unless there's no other option.

 

[Tony6Strings]

Is there anything else that should be adjusted such as the lye? Have any of you done the tek with 100g instead of 50g without negatively affecting the yield of 2 seperate extractions?

I did my first Cybs by the book with 50 grams of bark. The second time I used 75 grams bark. I increased lye to 75 grams, and started with 75 ml Naphtha which reduces in volume with each freeze precipitation and pull, I topped up with a little when it got too low. Both extractions went well for me.

The second run, the 75 gram, my 3rd naphtha pull turned dark, you could hardly tell it from the basic solution. First two pulls by the book, white crystals. I freaked out. Freeze precipitated my dark naphtha and got red spice. Did some Nexus reading. Washed my next pull with sodium carbonate for a return to a pretty standard yellow pull. That night I tried the red spice and was blown away. It's perfect how it is, it's incredible, I felt really dumb for freaking out before a bioassay. Did the rest of my pulls without washing, but only got one more pull of the red, whatever it was I pulled it all and by the 6th we were at the end of run yellow oily color. A/B ed the red and the white/yellow, both are great but at this point the red is my fave. Makes me want to try a jungle tek.

Btw Cyb thank you for the tek. Thank you Nexus for empowering me with knowledge. My life is better for having found you. :d :d :d

 

[Elrik]

As with anyone whos done enough extractions, at times I've run into difficult emulsions and I've used the usual tricks commonly mentioned here to greater or lesser success.
I'm finally reading the classic 'Practical Organic Chemistry' by Vogel [I highly recommend it] and in it he mentions 'a few drops' of ethanol being used to break emulsions. He doesn't recommend it, probably because of the slight cosolvent effect it would introduce, but he made it clear that it often works. I looked around and some of the other old-school organic chemists used it as a trick to break emulsions as well and it makes sense as even a small amount of alcohol would alter the surface tension dynamics of an emulsion.
This tactic surprised me, as I've never seen it mentioned here. Has anyone tried using a small amount of ethyl alcohol to break emulsions in based cactus or bark extractions? If so, how effective was it and roughly what volume of ethanol was generally used per 100 ml of extraction mixture?
Thanks

 

[rewindtothestart]

I need some assistance with a FASA extraction. I did a standard A/B with xylene, and pulled the DMT via FASA. I've done successful FASA extractions plenty of times before, and it appeared to be going as planned. Here's a pic of the crystals:



I wanted to clean it up a bit, and I thought that dissolving in H20, filtering, and drying would do the trick. My oven can maintain very low temperatures, so I dried it between 150 and 170 degrees. My understanding is that you should be able to do this with fumarate, because the melting temperature is 152 C (305.6f). When it finished drying, I was surprised to see a goo instead of fumarate crystals. The goo looks very similar in color, and similar viscosity as heated freebase. It has a mild smell like freebase DMT, so I wonder if it somehow converted in this procedure. The tested PH of my water is 8. When I first added the water to the DMT fumarate, it looked like some type of reaction occurred, because very small bubbles appeared throughout the glass.

Here's a pic of the goo:



(The joys of having an animal family - a hair already landed in it. :? )

Do you think the PH of the water was strong enough to convert some or all of the DMT fumarate? If so, would it have completely converted, or could it still have unreacted fumarate salts? I'm okay with leaving it as freebase, but I want to make sure that it's completely converted before I smoalk it.

 

[pete666]

If you had dmt fumarate and dissolved it in ordinary water, I doubt it became freebase.
If you think you could have fumaric acid in the product before, you can remove it easily

The dmt fumarate is a pain in the ass when dissolved in the water. I was trying this path, but the crystallization from the water takes sometimes weeks and leaves bloody hard uncrystallized layer, which is almost impossible to scrape, even with razor. I strongly suggest avoiding that.

The best method imho is the FASA conversion. Leaves nice, easily scrapable crystals.

 

[rewindtothestart]

Thanks Pete. I agree that it shouldn't have freebased with just regular water, but it just looks, smells, and has the texture of freebase DMT. I was really expecting it to harden as you described, and I'm curious what happened. The liquid started crystalizing overnight, and I just scraped it off the dish. It yielded a waxy consistency that should finish crystalizing with time. I'm really half way tempted to just smoalk it as is to truly give it the ultimate test.



I seem to recall running across a post a while back that showed how PH correlates with conversion. It might have been related to harmala extraction. Does this ring a bell to anyone?

 

[pete666]

here

where would you lose the fumaric acid?

 

[rewindtothestart]

Thanks! That's exactly what I was looking for. I guess I'll finish converting it with sodium carbonate.

I'm not sure where it would have lost the fumarate. The fumarate was fairly clean going in - just large crystals with no oils. Assuming that the PH was increased by the water, up to 15% max could have converted, but it sure doesn't look like 15%. My understanding is that heat actually decreases PH, so I don't think it's a factor. The only thing "extra" that I did was placing two drierite jars into the (convection) oven to speed up desiccation. I don't see how this had any effect though.

This was my first time trying this so maybe it's just that. Maybe this is just what DMT fumarate looks like when dried in water. Do you have any photos of when you dissolve the fumarate into water and dried it out? Do you remember if the color was similar? Was the texture pure crystal, or did it also turn out waxy?

 

[rewindtothestart]

Well, the riddle is solved. I just freebased the mixture via sodium carbonate, and I noticed that the waxy DMT immediately dissolved when hot water was added. It looks like fumarate can appear as a wax.

 

[pete666]

I don't have a picture of that, I just remember it was waxy and after few weeks!!! rocky solid. I could see some crystallization, but it was just flat, not real crystals.
I ended up by basifying that and re-extracting by heptane. The color was almost the same, but my was not purified yet before.
I was planning on making fumarate and then purifying, but this is a not a viable way. My final preferred route is STB with toluene, salting with HCl, then basification with NaOH, extraction/re-x with heptane and FASA. Purification of freebase is much easier than purification of fumarate and FASA on freebase is simple and giving very nice results.
It may sound complex, but it is simple STB + mini-A/B with heptane re-x and FASA

 

[rewindtothestart]

Just curious why do you pull with toluene on the first extraction, but heptane on the 2nd? It seems like toluene would pull the "jungle", but heptane would omit it on the A/B. Why HCL instead of vinegar?

 

[pete666]

With toluene I can get all dmt out of the MHRB with just two pulls. It is much better solvent for dmt than naptha.
Than it is salted with HCl, because it is convenient for back-salting/titration. I think another acid could be used as well, but I have tried fumaric acid and there were some problems.
After basification there's cloud of jungle spice in water solution, which is then extracted by hot heptane. Because I know how much dmt is in the solution (because of titration), I know how much heptane to use, so it is saturated to the maximum. Hot heptane can bring the active part of the jungle spice and the temperature while re-x'ing from that heptane is a tool for separation of pure white and orange dmt. The result are these two fractions.

 

[rewindtothestart]

That's beautiful. I'm glad I asked you to elaborate. I haven't heard of titration being used for DMT before. What are the main benefits for doing the extra steps? I always take the PH shotgun approach, but I can respect the precision/control over the process.

 

[pete666]

The titration is very easy in fact. Especially when done with nitrazine.

The main purpose is to have the information about alkaloid content directly after initial extraction. When done properly, its estimate is +-5% from reality. This can help in subsequent heptane re-x and is very good if someone is working on improvements of extraction method as an immediate feedback how it's going.

In fact I would suggest it to the beginners too, because they simply know whether everything goes as it's supposed to and can correct any mistakes as they know when the problem arised.

 

[Atmozic]

Hi All,

Nor sure if I'm wording this right but here goes. I did my first TEK extraction last night:

Cybs' Hybrid ATB 'Salt' Tek - DMT-Nexus Wiki

wiki.dmt-nexus.me

I won't go into TOO many details and bore you so I'll stick with what I believe would be the most crucial facts and see if I'm on the right track or not.

MHRB (Powdered) - 51g (my biggest fear is that somehow the DMT was "extracted" or destroyed in the process of being powdered (is that even possible?)

All other liquid/powdered/granular ingredients kept as per TEK guide.

At Step 3 (Acidifying) - kept to 42mins not 1hr
At Step 5 (Basifying) - Kept to 1.5hrs not 2hrs
At Step 6 (Solvent) - Followed 1 hr first then 45mins after (3 pulls only)

Noted Problems:

- the jar I used did not seal correctly, at the point of adding Base and Acid I lost product solution due to leakage, at the point of adding naphtha I just used a metal spoon to stir

- naphtha separated almost instantly at the point of stirring

- Had a bit of spillage with the pipettes (couldn't get a turkey baster so I used pipettes instead), to clarify I did NOT bring up anything other than naphtha

- After 3 pulls ONLY, no cloudy appearance to the solution, no yellow just straight clear. The only thing I noticed was a yellow substance underneath the naphtha grouping in the centre of the jar.


RESULTS:

So now that the background info is there the results have been - supremely disappointing to say the least, I just pulled the solution out of the freezer, started drying and the tray looks to be pretty much empty or with oily droplets (still waiting for it to completely dry before saying NOTHING is there).

So based on what I've listed; I never expected anything truly fantastic as far as results, but a complete lack of DMT it seems is more what I'm worried about. So is there anything about what I've listed above that is incredibly worrying? Could it have been a bad batch? Should I have held out on certain aspects or in the product that spilled would 90% of the DMT been in there?

Really appreciating everyone taking the time to look at this.

 

[pete666]

I don't see any significant error. It seems to be bad bark.

MHRB (Powdered) - 51g (my biggest fear is that somehow the DMT was "extracted" or destroyed in the process of being powdered (is that even possible?)

Hardly

- the jar I used did not seal correctly, at the point of adding Base and Acid I lost product solution due to leakage, at the point of adding naphtha I just used a metal spoon to stir

How much have you lost?

- naphtha separated almost instantly at the point of stirring

How well have you mixed it? Mixed or just stirred? For how long?

- Had a bit of spillage with the pipettes (couldn't get a turkey baster so I used pipettes instead), to clarify I did NOT bring up anything other than naphtha

Pipettes are way much better than turkey baster. What volume is your pipette?

 

[Atmozic]

I don't see any significant error. It seems to be bad bark.

MHRB (Powdered) - 51g (my biggest fear is that somehow the DMT was "extracted" or destroyed in the process of being powdered (is that even possible?)

Hardly

- the jar I used did not seal correctly, at the point of adding Base and Acid I lost product solution due to leakage, at the point of adding naphtha I just used a metal spoon to stir

How much have you lost?

- naphtha separated almost instantly at the point of stirring

How well have you mixed it? Mixed or just stirred? For how long?

- Had a bit of spillage with the pipettes (couldn't get a turkey baster so I used pipettes instead), to clarify I did NOT bring up anything other than naphtha

Pipettes are way much better than turkey baster. What volume is your pipette?

Thank you so much for replying, it's doing my head in trying to figure out what went wrong. I'll answer/reply to your points in order:

- Could be bad bark, will be trying again tonight to see if any results change

- Hard to say how much product I lost, when I saw it leaking I used a towel to contain the spillage at both points (firstly as a cleanup, secondly as a preventative measure), the volume decrease relative to the original amount was not significant, but as to exact mL I can't say.

- Stirring for 10-20 seconds in 15min intervals

- Pipettes are 3mL capacity and yes, there was a lot more control to be had with them

**UPDATE**

I managed to stumble across this post (#7):

DMT slime? - STB - Welcome to the DMT-Nexus

After checking out the lid to my glass tray, it's not broken but it is bent out of shape and such, and I could smell naphtha in the freezer (suggesting some level of venting), after touching the residue on the tray, it was slimy/lightly oily but then went "sticky" (to better explain, if you've ever used a motorcycle chain lube, where when first spraying it's a light and slick substance but after exposure to atmosphere becomes "gluey")

Some thoughts for my next attempt:

1) Use cling film on the tray before putting the lid on

2) Add a fraction more lye

3) Using a different mixing container that actually seals properly so I can properly shake it

I think it was yourself that said heat wasn't required, for reference I did use a bath (warm) in this attempt, after adding the lye though it hardly seemed necessary so I want to try without.

Thank you again so much for the reply.

 

[pete666]

- Stirring for 10-20 seconds in 15min intervals

This is possibly a problem, stirring may be not enough, you should shake as much as possible, about a minute or two. Then let separate. And then shake again and separate. Do that cycle 3 times per first pull, increase count in subsequent pulls.

- Pipettes are 3mL capacity and yes, there was a lot more control to be had with them

You need 50ml pipette

3) Using a different mixing container that actually seals properly so I can properly shake it

This is essential

 

[Atmozic]

- Stirring for 10-20 seconds in 15min intervals

This is possibly a problem, stirring may be not enough, you should shake as much as possible, about a minute or two. Then let separate. And then shake again and separate. Do that cycle 3 times per first pull, increase count in subsequent pulls.

- Pipettes are 3mL capacity and yes, there was a lot more control to be had with them

You need 50ml pipette

3) Using a different mixing container that actually seals properly so I can properly shake it

This is essential

I had a feeling that stirring might not be enough, so today I went straight out and bought a container that will definitely seal it. I figured it would be affected somewhat but to the extent where I got nothing, that was a huge problem for me.

For reference why do you say 50mL pipette? is it just for capacity or is there another reason?

Armed with this I'll be having another go tonight can't wait to share the results.

 

[pete666]

What's the material of this container? Is it compatible with chemicals you use?

The volume of the pipette is just practical, you can do it with 3ml, it's just annoying.