Decided to start a thread due to invading someone else.

Issues: dmt lost? suspended in a solution.

A little perplexed with this one. A friend watched a couple of 100g extractions out of interest. The first yielded 2.24g which was the best yield ever observed. The pulls were very very saturated. However it had a little bit of base in it after 24 hours in the freezer so It got re dissolved in fresh naphtha. It should have just been re-xed from that point, but It was decided to include it in the mini a/b of the second extraction.

The second extraction was with the same amount of material (ACRB), again pulled highly saturated NPS from the aqueous solution in line with the first extraction. There should have been a combined total of around 3-4g between the two.

It was decided that a mini a/b would be a good idea to get super clean spice. The acidified solution (HCl - 500ml De-ionized water) was mixed in with the dmt saturated naphtha from the first extraction and second extraction - around 400ml nps total. Mixed gently, it looked nice in the sense that it had separated a lot of plant fats out and left a dirty layer. The NPS was decanted and saved in a flask in the event that something were to go wrong. The solution was then re based.

It went a very cloudy white and there were pretty large crystals forming between the aqueous and NPS layers. Approximate 50-60mg chunks of what looked to be pure white spice.

4 pulls were taken off the mini A/B expecting the pulls to be very cloudy and saturation however they pulled clear with the exception of the first. The first pull was 'ok' and it just about crystallized entirely without putting it in the freezer. However looks to be about 500mg or less. Super fine crystals forming in scratches of the glass surface.

The naphtha didn't seem to want to take up any of the DMT from the solution. So there is at least 2-3 grams of dmt 'somewhere'. A second look at the plant fat solvent from the cleanup smells more like dmt than solvent. Nothing was discarded on the basis that it's probably in the A/B cleanup?

What would theoretically be the best way to go about resolving this?

Combine everything back (current vessel + cleanup vessel) into a 2lt vessel, acidify it 2-3ph, add NaCl then basify out to 12ph and try and pull again with clean solvent? The soup at the moment apparently looks like a snow globe. Clear, milky liquid with lots of fine white specs throughout. The A/B solution looks dirty with a little bit of aqueous on the bottom, maybe its in there? around 30ml.

Combine everything back? If that means what I think it means then why would you reacidify your already based solution? I probably would combine everything in a jug and warm it up and do warm pulls. Another idea would be to run more acidic solution through your solvent. I usually run about 900 ml of acid through it. I run 300 ml 3 seperate times. And I shake the hell out of it( probably overkill)

You could have kept it on the same thread if you want, it sounds like the same problem.

Does your friend have any other solvents (xylene, heptane) that could be used to try to recover DMT from the base solution instead of naphtha? I'm very curious about whether or not it really is DMT trapped in there. I'd test it myself but I no longer have the bsse solution.

I'll add to this that it was using Earthwalkers thread, which I've seen used a few times in the past with very successful results. Albeit without the A/B cleanup using MHRB and ACRB.

There is xylene available, you can't freeze precipitate with xylene though? Evaporate it off for a week might be the only option there? It's so slow to evaporate.

It has to be DMT in there. The pulls that were been taken from the powdered ACRB came out so thick and white you couldn't see through the syringe. Or an entire 3 x 50ml beaker for that matter you couldn't see through in the slightest. The 4th 50ml pull showed a little let up. Blowing on any of those saturated mix looked like mixing cloudy ammonia. Saturated!

When the syringe hit the solvent even its lower temperature caused DMT to crash. And the fact that over 2g was put into the mix that was crystalline (well redissolved) means the spice actually has to be somewhere there. There just can't be over 2 grams of impurities.

One of the first things observed when it was crystallizing between the aqueous and nps layer was an additional 100ml of water and NaOH added to make the solution more basic. Then placed in a 60 degree heat bath for 30 minutes to warm the mix. This broke the crystalline formations floating on top of the mix but then dispersed it within the basic solution to what looks like a snow globe.

An observation was made this morning. It appears that the basic solution is eaten all of the white specks up. It is basically a clear aqueous solution. Naphtha still doesn't hold any alkaloid.

At the moment, the aqueous solution has been based a little more. The cleanup solvent has had 300ml of highly acidic mix added to the flash. It may be time to turn the attention back to the cleanup solvent after a warm xylene pull to satisfy all curiosities. Will add a photo or two shortly.

The first image was the a/b solvent which had 300ml of acidified mix added to it - mixed separated.

The second image is the same flask with the solvent decanted. There wasn't enough NaOH left over to bring the Ph to the correct value so its flouting around 8-9. There is reason to believe that this contains goods. Are the floaters a good sign? Anyone?

The last image is the original A/B aqueous solution with a layer of NPS sitting on the top.

I'm wondering if it may have mostly been out of the initial A/B in one 70-100ml pull.
That pull crashed out pretty much instantly at room temp with the rest from an overnight freeze precipitation. Might have been too little hasty with eyeballing the yield. It looks very fine, not even slightly sticky, no oils.

The crystallizing dish is about 20cm across and holds about 2lt. Probably the cleanest spice a little space donkey has ever seen. Maybe it is about right? There is about 2.46g of extremely white spice with no hint of any coloring. The dish hasn't been fully scraped out, might be another 300mg or so. So almost 3g from 200-220g?

So if I'm following this right, the remaining DMT stayed n the "dirty" solvent and you were able to recover it by mixing with a strong acid solution, converting this to a base and then doing a large naphtha pull on that?

No, sorry it's a bit convoluted. I'll try and explain it a little better.

So, It turns out, that the first 'slightly' saturated pull from the original A/B using approximately say 100ml of hot naphtha contained a majority of what crystallized in the freeze precipitation probably around 2grams in 100ml of naphtha. That comprises the final yield you see.

Originally it was suspected to be a poor yield due to the lack of 'clouding' or apparent saturation. A second pull around 70ml was also taken but it looked like it was not holding anything as it pulled pretty much clear. Same with the subsequent two pulls. This actually precipitated a 'little' bit.

It can only be hypothesized? that the reason it doesn't cloud up like the original pulls from your bark mix before the A/B is that its significantly cleaner. Totally open to ideas on that.

So everything up until this point has just been poor perception rather than a 'real' loss.

As for those crystals that precipitated between the layers. They were broken up by using more NaOH and a heat bath at 60deg to a snow globe effect that ran clear given +12-16 hours. To be sure there is nothing left worth the time in the basic a/b (initial) a pull was taken with xylene which is now evaporating.

Couldn't say what that actually is other than some by product? However it can't be DMT as it doesn't pull into a solvent at all, well at least not naphtha. I might suggest he try and filter that solution with a coffee filter and evaporate just to see what it is.

Now, there still is only about 2.75g from 200-220g of powdered ACRB. Which gives the assumption that there 'may' still be say 500+mg stuck in the expended solvent from the A/B.

That was acidified with a strong solution and mixed around 15 times and let to settle, the NPS has been removed and only slightly based as there was no more NaOH to use.

It clouded up pretty nicely again so the assumption is there that it contains some more alkaloids. A little more NaOH is needed to really drive the Ph past 12 so that a fresh pull of NPS can extract anything that is left - if there is anything.

So the flask holding the expended solvent from the initial mini a/b, is now itself a mini A/B. Nothing has been pulled from this yet but that will get based further with a clean pull in the next day or so.

Will hopefully have some results on that soon.

The remainder of the A/B was completely based and a clean NPS pull was taken. It yielded approximately 160+mg. Probably wasn't worth the effort but it was good to find out for sure.

The xylene pull returned nothing except a nasty smelling dish.

One would assume that a bit of it gets trapped in the plant oils and fats like EarthWalker suggested in his method.

Potentially a little to vigorous in the mixing process although I wouldn't have thought so. Overall it was a decent enough yield for some personal work with the final results very pure white spice.

Encouraging to see the improvement in efficiency in extracting as you get better at it.

I looked at the previous extractions and compared (3) side by side and its night and day improvement. The colors vary from crude extract with a sandy appearance to some pretty nice, but slightly pale yellow crystals to super pure white fluff.

Probably not something your parents would be proud of but a little fist pump is in order.

Hey,

Don't be fooled by clear pulls ! There could well be a lot of spice in there...

Earthwalker's tek states that pulls from the mini A/B will be clear !

Good job anyway that's some nice fluffy white spice !

Tryptallmine - I'm glad it worked out well for you. Thanks for posting all this. It's really useful information. It sure looks like DMT trapped in that mini A/B, but I guess it really is just the fats or maybe just a pretty small amount of spice.

pulls from the mini ab should clod, the origina ab itself is mostly clear with a tinge of yellow