Dry Tek Problem

[Mr. Hoshino]

Hi,
I am hoping someone can help shed some light on this to aid my progress.

It is my first attempt at any type of extraction and I am using the acetone dry tek method on MHRB. I feel confident I have followed all steps correctly.

However when I get to the stage of adding FASA to initiate crystallization I get no precipitation.

Out of curiosity I left one attempt to evaporate. I was left with small whitish lumps. I presume these are just fumaric acid?

So I suppose I am either doing something wrong. Or there is no DMT in my MHRB - I wonder what the chances of that are?

Thanks.

 

[Blazon]

never tried acetone but did try once the Gordo tek
my mistake was the bark wasn't powdered,was shreded and I used ninja blender but still it wasn't powder.

what you had there is the product,fumaric acid would not mix with naptha

 

[Mr. Hoshino]

never tried acetone but did try once the Gordo tek
my mistake was the bark wasn't powdered,was shreded and I used ninja blender but still it wasn't powder.

what you had there is the product,fumaric acid would not mix with naptha

Thanks for your reply.
It was very finely powdered MHRB.

There was no naphtha involved. Just acetone which as you know does disolve Fumaric acid - hence the Fumaric Acid Saturated Acetone to initiate the crystallisation of the (hopefully) DMT saturated acetone from the washes.

Unless of course I have misunderstood something.

 

[Blazon]

acetone and fumaric acid,I see,sorry

what is this Tek called?

 

[downwardsfromzero]

I am using the acetone dry tek method on MHRB

(&@Blazon) Rather than referring to a 'tek' of some kind (especially without providing a reference), it is more helpful simply to describe all the stages of the process.


So, was the bark acidified and put through a couple of freeze/thaw cycles before the base was added?
How long was the base allowed to react before the first pulls were made?

Try adding a bit more water and base to the bark mixture, drying then pulling with fresh acetone. Something may yet show up. Calcium hydroxide can be a bit slow owing to its low solubility, and the low solubility of some of its reaction products with bark components, such as tannins.

 

[endlessness]

IME this won't work. FASAing directly on plant material is problematic, maybe because some other plant compound interferes with solubility/crystallization.

That's why generally FASA is used AFTER you have done an extraction with a non-polar solvent.

You can evap the acetone to yield you DMT fumarate + excess fumaric acid + possibly plant impurities, and proceed to clean up in any number of ways. Do you have any other solvent at your disposal? Are you looking to have the final product as a freebase or you want it as fumarate?

You could for example freebase whatever is left from the evaporation with sodium carb and water, let it dry, pull with acetone and evap, to yield you freebase DMT. It might dry/crystallize (or at least be dryish wax-like) if you insist a bit on scrapping/rescrapping it and letting it air dry for long, or it might stay more oily, in which case you can infuse herbs for example.

You can also try to re-FASA after freebasing, see if the second time around it does end up crashing.

Many ways to skin the cat

 

[Mr. Hoshino]

acetone and fumaric acid,I see,sorry

what is this Tek called?

Here you go:

Dry Technique Extraction - DMT-Nexus Wiki

wiki.dmt-nexus.me

 

[Mr. Hoshino]

I am using the acetone dry tek method on MHRB

(&@Blazon) Rather than referring to a 'tek' of some kind (especially without providing a reference), it is more helpful simply to describe all the stages of the process.


So, was the bark acidified and put through a couple of freeze/thaw cycles before the base was added?
How long was the base allowed to react before the first pulls were made?

Try adding a bit more water and base to the bark mixture, drying then pulling with fresh acetone. Something may yet show up. Calcium hydroxide can be a bit slow owing to its low solubility, and the low solubility of some of its reaction products with bark components, such as tannins.

Hi, thanks for your reply and advice. After the initial attempt as above, here are the steps I used for a second attempt with the results as described.

Here are the steps and materials I used;

Mixed calcium carbonate base with the powdered MHRB at a ratio between 1:2 / 1:1.

Added only enough water to thoroughly moisten the mixture to the consistency of a paste while stirring to ensure the consistency of the mixture.

Left it in the warmth for a few days, stirring occasionally.

Stirred in anhydrous magnesium sulfate until thoroughly dry.

Added an excess of anhydrous acetone and stirred thoroughly, left for a day or so stirring occasionally.

Coffee filtered off acetone and collected.

Repeated with fresh acetone two more times.

Then proceed to add FASA to the collected (hopefully) DMT saturated acetone from the above steps.

Having left or longer than expected I do now see a small amount of residue yellowish in colour and silty in appearance. I now plan to freebase it and see what if anything I have left.

Should I acidify and free thaw in future as you suggest? If so can you point me toward documenting for that process please?

 

[Mr. Hoshino]

IME this won't work. FASAing directly on plant material is problematic, maybe because some other plant compound interferes with solubility/crystallization.

That's why generally FASA is used AFTER you have done an extraction with a non-polar solvent.

You can evap the acetone to yield you DMT fumarate + excess fumaric acid + possibly plant impurities, and proceed to clean up in any number of ways. Do you have any other solvent at your disposal? Are you looking to have the final product as a freebase or you want it as fumarate?

You could for example freebase whatever is left from the evaporation with sodium carb and water, let it dry, pull with acetone and evap, to yield you freebase DMT. It might dry/crystallize (or at least be dryish wax-like) if you insist a bit on scrapping/rescrapping it and letting it air dry for long, or it might stay more oily, in which case you can infuse herbs for example.

You can also try to re-FASA after freebasing, see if the second time around it does end up crashing.

Many ways to skin the cat

Thanks for your reply and help. To save repetition the steps I followed are as in my reply to @downwardsfromzero

I am reticent to use solvents other than acetone for reasons of toxicity / sustainability. And in future intend to switch to the limonene tek.

As you suggest I am intending to freebase via the method you describe. Although I don't remember the method I read mentioning pulling with acetone after the sodium carb and water. But no doubt that's my memory being inefficient.

Just so long as I can avoid being the cat :d

 

[Mr. Hoshino]

So, was the bark acidified and put through a couple of freeze/thaw cycles

@downwardsfromzero would you be able to point me towards some details / instructions for the above please?
Many thanks

 

[downwardsfromzero]

So, was the bark acidified and put through a couple of freeze/thaw cycles

@downwardsfromzero would you be able to point me towards some details / instructions for the above please?
Many thanks

Wet the bark with diluted vinegar (acetic acid), stick it in the freezer for a day, take it out to thaw out and warm up to room temperature for a while. Then put it back in the freezer for another freeze/thaw cycle.

 

[Mr. Hoshino]

Wet the bark with diluted vinegar (acetic acid), stick it in the freezer for a day, take it out to thaw out and warm up to room temperature for a while. Then put it back in the freezer for another freeze/thaw cycle.

]

Thank you.