Hey All,
Long time member here but not been around for a long time. Took a hiatus as the kids were growing up.
I just did an extraction on Acuminata bark that I have had for 7 plus years sitting in a box in the shed. I did a few extracts on the same bark a few years ago (same method) and all went well but this time there was just goo. I did a double A/B to get rid of the plant oils and even at the end of that ended up with loads of goo.
I did a shellite (naptha) re-x and the goo slowly dissolved with agitation but the on refreeze just turned back into goo. It is like oil and I think will take weeks to dry out.
Im assuming it has all converted to dmt oxide but there seems to be a bit of conjecture here it seems.
I have just ordered some zinc powder to give it a go but just wondering what the latest tek is on this?
Do I add the zinc in the initial vinegar water boil?
Any advice would be much appreciated.
Cheers.

The DMT oxide thing is/was always a red herring. Thanks to recent research, chiefly by benzyme and Loveall, we're now getting the picture that goo seems to be due to oligomerisation (like polymerisation but with only a few molecules linking together) and polymorphism (where, for whatever reason, part of the DMT molecule decides to sit with a slightly different spatial orientation). There may be some interplay between the two factors, with the different spatial orientation of the side chain nitrogen making an electron transfer more likely, which is a key step in the molecules forming intermolecular bonds in the pyrrole region of the molecule.

Preliminary data indicates that a simple acid/base treatment of the polymeric goo is enough to break it up to back to nice white fluff and this is what happens during a zinc reduction - meaning that the zinc is almost entirely superfluous. Zinc would perhaps be more beneficial if the sample was more extensively oxidised. So you might still be justified in considering a zinc reduction. I would suggest you gather the goo using your usual A/B and subject that to the zinc reduction if doesn't clean up with a simple mini A/B.

Adding zinc to the initial vinegar boil means there's all sorts of other stuff in the bark potentially reacting with the zinc and producing unknown compounds. It's best to avoid this situation - although if you were to run a small batch using that method it would, in the name of science, be interesting to hear of the results.

Here's a thread with information: Minimum Polymer

and Polymorphic properties of DMT

The acid step you are doing may not be enough to breakup the potential oligomers. You can boost the acid step with other acids that seem to do better (citric or vitamin C). Also, adding cations can disrupt indole pi-pi stacking.

What I would do/reccomend:

- 0.3% DMT concentration
- 8% NaCl concentration (or 8% KCl, KCl may be better at breaking up goo). K+ interacts less with water did a better job experimentally before.
- Acidify with vitamin C (pH~4)
- Keep for 4h at 150F
- Cool to ~120F, add a light naphtha. Use a known good lighter fluid (e.g. Ronsonol), avoid the heavier painter's naphtha
- Base while mixing until cloudy and emulsions break

I think that should de-aggregate the DMT and keep it from aggregating during the pulls.

Legends. Thankyou. I will definitely give that a go. I will also try using a different acid from the start instead of Vinegar. It would be great to stop it from happening from the get go. I will report back once I do.
It is funny that now I know what it is called instead of DMT oxide that there was a huge post right underneath it regarding this topic which I didn't see.

Cheers.

@Loveall when you say 8% NaCl or KCl I assume you mean by weight not volume?
Cheers.

Man a lot changes in a short ammount of time

Well, check out Mindlusion's recent post. The goo should form in the solvent, slow cooling and initial concentration may matter a lot.

Thanks Loveall,
I don't pretend to understand half of what's going on in those posts but the half I do understand makes me even more confused. Is the consensus here that it happens in the bark naturally over time or the acid step if the acid is not good enough eg. Vinegar or that it happens in the solvent?
Interestingly one of my last extractions a few years ago I did a double A/B and got very white cloudy solvent. I then put this solvent outside to evaporate in the sun. When I came back an hour later the solvent had turned pink almost and a freeze precip was very oily goo whereas the other half of the extraction was nice crystals. I thought it was the sun that had done something but I wasn't sure what or didn't bother to experiment further. It might be nothing but thought it might be worth mentioning as an anecdotal story.

Yeah, direct sun could have done something.

I think the input from Mindlusion is that if it all goes well and DMT is extracted into the solvent, what determines if an oil forms or xtals form is what happens in the solvent during the final precipitation step. I think Mindlusion explained that to get xtals instead of goo when xtalizing, the solubility, starting concentration, and temperature change profile are the key

- Higher solubility helps form xtals. 1% ethyl acetate may help
- Lower starting concentration helps form xtals. Perhaps better to not evaporate before freeze precipitation. Reuse solvent to not lose yields.
- Slower temperature changes help xtals
- A seed xtal from a previous extraction could also help

As long as there are no non-DMT contaminants the focus should be on the final xtalization step per Mindlusion.

Very interesting. I will try using another acid instead of vinegar anyway but will take on board the other points and somewhat refine my previous lazy technique.
I appreciate your time. Thanks very much.

Loveall, Mindlusion’s post was quite a deep, dense chemistry lesson. I think I followed it to some extent, gleaning the key points you stated above. I guess I missed this point though, that you want low solute concentration. Generally in crystallization you want to boost solute concentration, it’s why lots of people heat (to dissolve more solute and/or evap solvent), to super-saturate, then cool to force crystallization. It sounds like you had some PMs with him where this was perhaps discussed. Could you further explain what’s going on, in this case, regarding “lower starting concentration”? Thanks

Yeah we discussed in chat. Lower concentration makes it more likely to get the slower growth that is more likely to result in xtals as I understood Mindlusion. It is similar to the other principles promoting slow xtaline growth (adding 1%EA and slow temp changes).

Ok, got it…thanks for your quick and clear response.

Could be a useful consideration in cielo goo formation, i am also interested in it wrt to your new dmt work.

Thanks. I think it is mostly important to fight goo during free base precipitation. I think salts should be more robust in general, and as we have seen the fast salting option in CIELO makes tiny xtals (powder like), but still no goo there.

👍🏻