No yield q21q21 Tek 1

[Woolmer]

I recently attempted my first extraction using q21q21's tek that involves limonene but after evaporating the vinegar in the last step, I got next to nothing on the spoon except a few traces of some goo which would not vaporize (it only burned when put into a yocan magneto with very hot coils). I believe all the materials I used should have worked as expected. My lime was bought at an industrial chemical supplier, my limonene at an art store but I verified with the store that it only contains limonene, and my white vinegar just at a grocery store. I know my vinegar is only 4% but I figured I should still be able to reach the right PH. Here are the details of my attempt:

50 g powdered MHRB bark used
4% white vinegar added to form clumps and then near boiling water to reach right consistency
More than 40 g lime was added and a bit of water to reach oatmeal-like consistency, bark turned grey with a brown layer forming on top if left to sit.
Bark was left to sit for 24 hours

75 ml limonene was added and periodically stirred for 25 minutes before poured off into separate container (The limonene clouded a bit but q21q21 states that it should stay clear, will attach image of limonene below).

I slightly messed up in the next step but I don't think it is the cause of my issue: I poured a shot of vinegar into the container with the limonene, agitated for a few minutes, then added warm water (Whereas the tek says to agitate vinegar, take out vinegar, add water to limonene, agitate, take out and combine with vinegar). My vinegar was quite clear initially and only turned slightly darker once evaporated to about 30 ml if that helps at all

The vinegar was then put on a low flame in a tiny pan to evaporate while I attempted a second pull with the same solvent + a bit more since the bark absorbed some in the first pull.
The steps were followed correctly this time for the acid wash and then new batch of vinegar was added to the gently simmering pan

Evaporated it down to about 20-30 ml and then attempted to evaporate further with spoon over low flame. I have read several times that freebasing the acetate by heat is not considered the best manner as of late but I have never been able to find a thread which states why it is not recommended anymore.

There are 4 things which I could think of could be wrong:
1) Bark is bunk
2) Vinegar not strong enough (also contains sodium metabisulfite but this is in most vinegar?)
3) Limonene not correct (Specifically was dipentene which is racemic limonene but this is basically the same thing and should have been no hindrance?)
4) Heated evap does not work at all?

I am quite confused as to what went wrong, but knowing myself it is probably some very obvious silly mistake that I am missing so it would be kind if someone could point it out for me

 

[downwardsfromzero]

The most likely problem is bunk or weak bark, but if you add a bit more lime to the bark paste and adjust the consistency with distilled water so it's like bread dough you could try a few more limonene pulls. It can take a while for the bark to break down and release all the goods.

The limonene itself, even listed as dipentene, is - as you infer - almost certainly fine. The clouding most likely is from lime particulates which inevitably get picked up from the lime slurry. Getting the consistency right can help with this, as well as having a bit of patience so the cloudiness settles out. The limonene can then be decanted off the sediment before washing with the vinegar water. This way you avoid getting so much calcium acetate in your pulls, which otherwise would skew your yield calculations and produce an inconvenient jelly if you tried purifying with ethanol or isopropanol.

The problem with having sodium metabisulfite in the vinegar is that it is not (completely) volatile. This will skew your yield measurement. A sensible approach here would be reconverting to freebase and pulling with another solvent. Did you weigh your acetate goo? Because it appears you did get a small but nonzero yield. Have another try, you might get something yet.

 

[Woolmer]

The problem with having sodium metabisulfite in the vinegar is that it is not (completely) volatile. This will skew your yield measurement. Did you weigh your acetate goo? Because it appears you did get a small but nonzero yield. Have another try, you might get something yet.

Ok, so I attempted another pull today with the same batch of limonene. I threw it into my basified bark and mixed for 10 or so minutes, poured it out, poured vinegar into limonene and agitated (more vigorously than last time as I thought maybe it was not grabbing all of the FB), poured water and agitated, and then went on to evaporate with same procedure as yesterday.

Got a slightly higher yield, in total I have "pulled" around 200 mg (0.4%). The goo that remained on the pin and knife which I used to scrape was burned with a lighter to see if it would act similarly as yesterdays. Some bits vaporized off immediately but others turned to flames in 1-2 sec and burned for 1-2 sec. The goo smells very citrusy.

I put a drop of limonene onto another pin and tried to light it and it acted similarly to the pin with the goo. From what I have heard, limonene does not evaporate very easily but is quite flammable and so most of my yield might be made up of limonene and vinegar?

A sensible approach here would be reconverting to freebase and pulling with another solvent.

To do this I would take my goo (DMT-acetate), mix it with sodium carbonate (or lime? I see on an older thread that you recommended someone use lime), dissolve into IPA/Acetone and evap?

The most likely problem is bunk or weak bark, but if you add a bit more lime to the bark paste and adjust the consistency with distilled water so it's like bread dough you could try a few more limonene pulls. It can take a while for the bark to break down and release all the goods.

Ok, I have done this and will attempt another pull tomorrow.

Also, thanks for all the help you have given me so far, I have learned a lot just from your responses

 

[Woolmer]

I did another pull today with extra lime added from the previous day and also left my limonene for about 1.5 hours. Yielded 300 mg of something, 230 mg of which seems to look more like a DMT-acetate goo. When I evaporated, what was left on my mini pan was a large flat section of dry grey/white type powdery substance and a smaller but denser section with brown goo. I am going to try and convert to FB with sodium carbonate and an acetone pull but was wondering if it was worth it to combine all 3 of my yields or should I try each one separately since they all have different consistencies and I'm not sure if the grey/white substance is DMT.

 

[downwardsfromzero]

The goo smells very citrusy.

With that, and from the looks of your extracts, they'd benefit from a clean-up of some kind. Boiling with distilled water would get rid of the limonene residue.

Your plan to basify and pull with acetone seems like a sensible way to proceed. It would be far less fiddly to combine all the material for that. The grey powdery material is probably calcium acetate.

It would be a good idea to recrystallise the final yield with naphtha or heptane if you have it.


Another possible approach would be to dissolve the acetate in distilled water - maybe filter it if there are particulates - then add sodium carbonate solution, and allow the freebase to precipitate in the refrigerator.

thanks

You're very welcome!

 

[Woolmer]

Another possible approach would be to dissolve the acetate in distilled water - maybe filter it if there are particulates - then add sodium carbonate solution, and allow the freebase to precipitate in the refrigerator.

Are you sure this is correct? It may be freebase then but I do not see how it is going to precipitate with all the water. Am I supposed to evaporate the water off first?

 

[downwardsfromzero]

A respected member has reported positive results with this recently - in the past week, IIRC - and it's a theme that's been discussed over the years. If you are into experimenting with naphtha-free methods I thought it might be worth a try.

Maybe to optimise you would use a concentrated solution of DMT.HCl and concentrated SC (no excess of HCl though - foaming!) The NaCl which also forms will help push the DMT freebase out of solution.

 

[Woolmer]

A respected member has reported positive results with this recently - in the past week, IIRC - and it's a theme that's been discussed over the years. If you are into experimenting with naphtha-free methods I thought it might be worth a try.

Maybe to optimize you would use a concentrated solution of DMT.HCl and concentrated SC (no excess of HCl though - foaming!) The NaCl which also forms will help push the DMT freebase out of solution.

I'd like to read up on this a bit more as I don't really understand how this works. Could you link me to a thread or give me some guidelines? If you make a solution with HCI and SC the water will not be able to freeze anymore and dmt can precipitate out?

I did actually attempt a solution with sodium carbonate and DMT-acetate. I know very little about chemistry and extracting DMT so I kind of just chucked in a fair amount of sodium carbonate and probably way too much water not really expecting to get any results. The solution just ended up freezing and was very clouded with sodium carbonate that did not dissolve into the water.

Anyway, I filtered a few times in-between all this and finally dissolved into acetate to evap and it seems like I have finally yielded some decently clean jimjam. I also picked up some naphtha yesterday and am in the process of a pull. My naphtha also clouded up quite a bit which I assume is from the lime (why does the lime get pulled so easily? I changed my consistency to be more dough-like but it seemed to make no difference).

Edit: Nevermind, it seems like the sodium carbonate has just further messed up my pull and now I have 1.4 g of some white powdery crystally substance that only seems to burn (does not melt or vaporize).

 

[downwardsfromzero]

Yeah, you have to know how to think about what you're doing. Understanding how the basic calculations for chemical reaction equations work is actually pretty useful.

The other thing is, there's a reason - simplicity - why beginners are recommended to freeze precipitate from naphtha.


Maybe you've recovered sodium acetate?

If you haven't thrown anything away there's still a chance of getting a reasonable product.


I've had a brief, unsuccessful look for the recent mention of recovering freebase without using NPS. It's something that really ought to be noted somewhere easy to find - not that it necessarily is. Now, how would one choose the best search term to find it?

 

[Woolmer]

I stumbled across an old tek the other day which claimed to be "water only" but it was debunked and concluded that it does not actually work.

What could I do to reduce the sodium acetate? A few pulls with acetone would work right as the sodium carbonate would not carry into the acetone?

 

[downwardsfromzero]

OK, that 'tek' was attempting to produce crystalline DMT from plant material, water and lye. The crude plant material is far too messy for that to succeed. It's bugging me now that I can't find the reference, but using already relatively pure DMT acetate (or maybe was it fumarate?), dissolved in a little distilled water, plus the requisite amount of sodium carbonate solution when mixed and placed in the refrigerator (not freezer) should (it is claimed) produce recoverable DMT freebase.

Otherwise, a drytek with sodium carbonate and acetone will do the trick. The SC/acetate mix must be dried out completely and the acetone must be dried with a suitable drying agent; if not, sodium salts will come along with the DMT. Don't be too surprised if your freebase still smells of oranges after this, though.

 

[spanda]

I've had very good results with the q21q21 Tek 2 using naptha to pull the alkaloids and putting it in a freezer as described. Got close to 1.5% on last effort. Very potent material.