I have just undertaken an A/B extraction on some Acacia Floribunda bark and its currently at the freeze precipitation stage.

Four pulls were done using warm shellite and each pull took on a very clear yellow colour in the separatory funnel. Once transferred into a beaker I blew across the top of it and noticed white precipitation followed by the whole lot clouding over into a yellow/green(?) colour.

This was put into the freezer for around 24 hours and the last picture below is what remained in the beaker after the shellite was decanted off. Not long after it looked as if it were starting to melt.

In hindsight, I probably should have just left it to dry as I'm sure it would have recrystalised and been ok, but I ended up re-adding the shellite and putting it back in the freezer for a couple of reasons.

The first reason was, I noticed that when I blew across the top of the shellite it clouded with precipitate again so it appeared that it still needed longer.

The second reason was that I assumed the freezer was set to its coldest setting, which it wasn't...you know what they say about making assumptions. so that has now been rectified.

Anyway, with a slightly colder freezer I'm hoping the results will improve by this time tomorrow but if my freezer isn't cold enough I might attempt freeze precipitation with dry ice.

Does anyone recommend using dry ice or would it be better just to let it evaporate?

Hi mate,

Interested to see your final results with floribunda.
As you may know the net seems to contain many hit and miss anecdotes.

Why do you want to use dry ice?

I would just go through the usual steps, decant Shellite, then allow to dry out for a while (possibly days).
Remember that you may end up with a liquid (goo), as if the dmt is impure, the melting point of the mixture will be lower than that of dmt, thereby not being a solid at room temp. If there is some nmt accompanying the dmt, then you may not get a room temp solid, no matter how long you dry it out for.

Is that a kugelrohr in the background?

Hi there

Yeah from what I have read there seemed to be mixed results with this species, but those same people also mentioned that the variety they were extracting from had yellow coloured flowers, where as the trees I harvested from had cream/white flowers when I first came across them, which I believe is the desirable strain.

I'll be sure to post my final results once I've finished with it all. I plan on attempting some more pulls on the base mix next week as it seemed like I could have got a little more out of it. I'm not holding my breath but we will see.

I also kept the AF bark sludge and have it soaking in some acidic water with the intent of coming back to it if this first experiment failed. I'll try and extract from it again just out of curiosity... if I get something from it great, if not no harm done.

The reason I thought of using dry ice was in case my freezer wasn't getting cold enough. At least with a dry ice/acetone bath I could a achieve a much colder temperature and it would also reduce the time needed for freeze precipitation. It was just a thought and was wondering if anyone would recommend that approach instead of evaporation.

I appreciate your input, so I'll do as you suggest and keep going ahead with the usual steps.

PS, no it's not a kugelrohr it's actually a rotary tumbler. Used for cleaning/polishing brass, jewelery, metals etc.

Thanks mate

Your freezer is cold enough to get the job done.
Make sure you keep your vessel sealed during the cooling process to avoid water condensation.

The main reason not to use acetone dry ice is that it cools to -78c.
Once you get to aliphatic hydrocarbons larger than heptane, they freeze above -78c.
Shellite will definitely contain aliphatic hydrocarbons larger than heptane.
Therefore there is a chance that some of your solvent mixture is going to freeze at -78.
You would also go through a fair bit of dry ice and have to be around to keep topping it up.
Freezer is easy.

Ok so it appears that a slightly colder freezer made a bit of difference going by these pictures.

The green looking pic is the result of using a flash and it certainly doesn't look like that in real life, I just thought it was interesting.

This is now being left to dry in the beaker and while that's happening I'll attempt some more pulls and see what comes of it.

These 4 combined pictures are shots taken over different backgrounds which each give a different appearance of what is left in the beaker.

To the naked eye it looks like there are tiny looking crystals/solids within a somewhat very thin translucent film that is sticky to touch is the best way I can describe it. It definitely looked more promising when it first came out of the freezer.

Should I let it dry further as is or should I scrape it together, transfer it to a shallow bowl and try and dissolve it in warm shellite/naptha and see if it forms into something more manageable?

The second picture is a side by side shot of the second round of pulls next to the first/used round after it had finished being in the freezer (decanted into another beaker).

The beaker on the left is the second round which looks as if there was still more to be gained. I am letting this batch evaporate as a comparison to the freeze precipitation method.

I scraped what I could out of the beaker and put it into a shallow dish/watch glass and hopefully it dries out. It currently has the look and consistency of honey, maybe even a little thicker.

There is still quite a bit stuck inside the beaker and almost impossible scrape it out...I guess I can try and dissolve it in warm naptha and transfer it to another dish?

Do you know what mass you have roughly?

You have a few choices now;

Leave the honey substance uncovered to dry and work it with a blade occasionally, in hope that it becomes more solid.
Or
Recrystallise the honey substance with hot shellite.
Or
convert your honey into enhanced leaf.

Be aware that you might not end up with a solid, regardless of what you do. Especially if this is a mixture of alkaloids, rather than just dmt.

If you have a significant amount of this stuff, I would find out what's in it. There are at least 2 ways to have it analysed via this website. Or with a little effort and know how, you can do thin layer chromatography yourself. I say this, because you are going down the path less travelled, ie. not using mhrb or acrb.

As you discovered, choose a wide vessel for precipitation, as its easier to scrape up the product.

Good luck, keep us in the loop.

Hard to say.... I had planned on weighing it on the watch glass but my scales aren't working properly (you get what you pay for) so I have to get some more. I honestly couldn't even guestimate the weight due to its wet/sticky consistency, but its possibly heavier than it looks due to that fact.

At this point I think I will give it some more time, perhaps a week(?), and see if it dries out. If that fails, I'll visit those other two options when the time comes.

I'd definitely be interested in getting it analysed so I'll look into that too. Thanks.

In case your interested, the first attached picture is the second round of shellite pulls after I let it evaporate in a wide tray. Much easier to work with. Lesson learnt.

The second picture are side by side extract results of the two separate pulls. Right first, left second.

Well you got something.

If you get into extracting different acacias, then it's worth getting the bits and pieces required for tlc. Or buy a kit ready to go.
If you think this is a one off, and you won't extract many times and you have a large amount of product, then send off a sample for testing.

If I'm interpreting this right, your second set of extractions seem to have produced as much as the first?
That means there is more to come.

Yeah I got something.... I'm sure there is DMT in there but I'm interested to know what else is in it.

I'll have a look into TLC and see if it is something I want to do down the track. I've got some phyllodes from this tree that I want to extract from too and I also plan on trying some other acacias such as a.pycnantha at some stage as it grows everywhere around here.

Yes you are correct, the second round of pulls produced approximately the same amount as the first. I quit once the pulls stopped clouding over. That said, I'm currently reducing the acid water I had the used/left over bark sludge soaking in while I was busy with the extraction, so I'll be interested to see if I can get anything else out of it.

Looks like you should keep extracting your basic solution.

There are plenty of examples on this site of people still getting some product after 5,6, or 7 extractions with heptane or naphtha.
Obviously this is due to the limited solubility of dmt in these solvents.

A less tedious approach would be as follows;
Do three extractions of your base solution with shellite, then freeze precipitate, in hope of obtaining fairly pure dmt..
Then do three extractions with toluene or xylene, for the purpose of removing any remaining alkaloids, especially nmt.
Your base solution will be pretty much spent after that. Evaporate down your toluene or xylene to leave behind your mixture of remaining alkaloids, as an oil or goo.

I'm saying this because you are using a source material that is perhaps not going to be just dmt. Nmt, the next most likely compound, will not be easily extracted with Shellite.

TLC is really useful in these situations.

TLC is also great because you can screen a plant for alkaloids with just one to two square cm of phyllode or a bit of bark. No need to do a full on extraction.

Definitely active goo.

Result of bioassay here https://www.dmt-nexus.me...osts&m=929458#929458