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Questions about my second extraction

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mbrown

Rising Star
Hello everyone, this is my first post here. I successfully completed my first extraction a few weeks ago, so thanks to everyone who has contributed to the wealth of information here!

I have, over the past few days, been attempting a second extraction, but using a different method this time. I'm afraid that I had some misconceptions about what is actually occurring in the acid/base extraction, so hopefully someone can correct me. I will describe the process that I followed:

1. 250g shredded Acacia Confusa root bark was placed in a crock pot with approximately 1500ml water. No acid was used. The crock pot was set to low and left overnight.

2. After approximately 8 hours, the liquid was decanted and an additional 1500ml water added to the crock pot, which was set to low and left for a further 8 hours.

3. The two brews were kept separated in mason jars. To each jar, household ammonia was added while stirring until the solution reached a pH of approximately 11 (tested with paper strips). To my surprise, while the first brew produced a thick cloud of precipitate, the second brew produced absolutely nothing.

4. As it was my understanding that the cloud of precipitate contained the desired alkaloids, I discarded the second brew, which produced no precipitate. The remaining solution was left in the fridge overnight.

5. After the precipitate had settled to the bottom of the jar, the liquid was decanted and the remaining sludge poured through a coffee filter. The precipitate was then dried under a fan.

6. The result, to my surprise, was approximately 25g of powder, despite the fact that I was expecting no more than 5g total alkaloids. I assumed that the the powder contained the alkaloids, as well as a large amount of impurities. What other water-soluble compounds present in acacia bark would fall out of solution under basic conditions?

7. The dry precipitate was placed in a jar and 400ml naphtha was added. The jar was heated in a water bath and the solution stirred for approximately 10 minutes. The naphtha was then decanted into a glass tray, covered, and placed in the freezer for 12 hours.

8. Finally, to my surprise yet again, no crystals formed.

Can anyone provide some insight as to why the above method would not work?
 
I think you misunderstood the nature of my post. I've already researched plenty of teks, which is how I successfully completed my first extraction. What I would like to know is why the above method would not work. Thanks to anyone who can provide some insight there!
 
It seems to me you were using harmalas extraction tek and you have discarded all the goods
You're just using the wrong tek and as DmnStr8 said nothing seems right in what you did, anyway what difference method did you use?
 
Yes I was trying to do something similar to the harmala extraction tek. But the question is, why should that not work for DMT as well? Based on my understanding of the theory it should work. The DMT in the bark is in water soluble salt form, so it dissolves into distilled water. When ammonia is added, the DMT is converted to its freebase form and becomes insoluble in water, falling out of solution. So if I filter the solution after adding the base, then the solids collected should contain the freebase DMT, correct? If not, then what is the material that I collected?
 
The material you collected is probably plant material.. well i am not sure of what i'm gonna say but the solution you have is not just water it contains plant material and the ammonia and surely the density of this solution is above 1 and dmt has a density of 1.099 according to Wikipedia so maybe they have close densities and the dmt doesn't just simply sink to the bottom and it is floating in the solution, i never heard of dmt precipitating like that, i am not sure i hope someone comes and and tell us why it is like that :)
 
Well, after some more testing I am only more confused. Turns out that the 25g of precipitate that I filtered from the basic solution did in fact contain the freebase DMT. The problem was simply that it would not dissolve in the the naphtha directly from the dry powder.

I added around 200ml of NaOH solution at a pH of around 12 to the dried precipitate and stirred. It appeared to dissolve completely. I then once again added the naphtha and did a pull as in the usual teks, transferring the naphtha to the freezer yesterday afternoon. This morning a thick layer of crystals had precipitated.

This is very confusing to me. Can anyone with an understanding of chemistry explain why the DMT would not dissolve in the naphtha without a high pH aqueous phase? To me, it seems like it should be easier to dissolve it from a dried powder with no aqueous phase, but my understanding of chemistry is minimal.
 
After some more research, I believe the precipitate that I filtered from the ammonia solution was a clathrate compound, basically a lattice structure of some compound surrounding individual molecules of freebase DMT. This would explain a) why the precipitate sank to the bottom instead of remaining suspended, b) the excess mass of the precipitate beyond the expected yield of alkaloids, c) why the dried precipitate would not dissolve in the naphtha. It seems that exposing the clathrate compound to high-pH NaOH solution breaks down the lattice structure, releasing the DMT which then must migrate to the naphtha in order to escape the polar environment of the aqueous phase.

Searching this forum for "clathrate" shows that the formation of these compounds is generally regarded as a bad thing because it prevents the transfer of DMT from the aqueous phase to the non-polar phase, but I wonder if the properties of the clathrate compound could be exploited for a safer and more efficient extraction process. While the clathrate compound would not dissolve in naphtha, it is possible that it would have dissolved in a stronger solvent which has both polar and non-polar properties, like acetone. In that case, The DMT could then be precipitated in salt form using fumaric acid, or possibly in freebase form by adding water drop-wise to the acetone, lowering the solubility of the DMT to the point where crystals will slowly form. Can anyone comment on the feasibility of this idea?
 
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