Proprer ph during basification?

[rienflake]

Firstly, swim embarked on the journey to extract dmt from mhrb , fortunately everything was going great until the basification stage.

So you can get an idea, the dmt was extracted from the 114g of MHRB into dmt-Hcl with water, this was done several times, he then proceeded to combining the extractions and boiling them down to half their volume, making it a total of 225mL, then made a basic solution with 225mL of water and an unknown amount of NaOH, the problem was that swim was relying on his digital pH meter to tell him when he had reached a reasonable pH of 13.5, but the pH meter never reached that, it always showed 12.8 - 13 but never higher, in total less than 50g of NaOH was probably added, but it seemed like alot, so he stoped and decided to use ph papper, and darn, im not sure what ph Black is but swim thinks its more than 13,

unsure of what to do he added the basified water mixture to the acidic mixture, as soon as it was pored a gray crusty layer appeared and then dissipated just a quickly, the entire solution went from a dark dark red to a brownish black, and smelled strange,

swim was considering adding some HCl to lower the ph a little but wasn't sure if excess NaOH would be a problem so he added 100mL of toluene, he shook vigorously and the layers separated within the minute, and now he waits, wondering if anything else should be done before extracting the toluene and evap/ freeze precipitation

 

[DMTripper]

This is all normal. It's fine to take the pH very high, the DMT can take it. And it helps eliminating emulsions. Your pH is probably very high that's why the layers separated very fast.

You're good to go now. I pull 3 times.
Good luck.

 

[rienflake]

Thank you for the quick reply its much appreciated, SWIM has just recently heard that toluene will not freeze percip apparently because it has too strong of a bond with the DMT and was just wondering if this is true...

 

[Trickster]

This is all normal. It's fine to take the pH very high, the DMT can take it.

Very high pH may lead to extraction of some inactive alkaloids. Taking pH very high may be necessary to break cell walls, but it could be avoided by doing a few freeze/thaw cycles on soaked mhrb powder before the extraction.

Also, IME, very high pH is the cause of red/brown coloration of NP pulls that leads to red/brown goo in the product.

And it helps eliminating emulsions. Your pH is probably very high that's why the layers separated very fast.

That's right. With lower pH the solution to emulsion problem is not to create it in the first instance, i.e. careful handling, no shaking. IME, magnetic stirrer on low is the best.

I pull 3 times

Yeah, 3 is the magic number, although I prefer 5 smaller pulls.

, SWIM has just recently heard that toluene will not freeze percip apparently because it has too strong of a bond with the DMT and was just wondering if this is true...

If you do not get decent yield with freeze-precip from toluene, evaporate it completely. You may use your spice "as is" or redissolve it in heptane/hexane and then freeze-precip if you prefer to clean it.

For evaporating any significant amount of solvents consider a simple distillation setup. Toluene seems to be quite toxic.

 

[endlessness]

Very high pH may lead to extraction of some inactive alkaloids.

Such as? (and source for claim please)

Also, IME, very high pH is the cause of red/brown coloration of NP pulls that leads to red/brown goo in the product.

Not IME.. Never had that problem in my life even extracting with very high pH. It seems there are more factors involved.. would be interesting to try to pinpoint the variables related to why people get that issue.

, SWIM has just recently heard that toluene will not freeze percip apparently because it has too strong of a bond with the DMT and was just wondering if this is true...

If you do not get decent yield with freeze-precip from toluene, evaporate it completely. You may use your spice "as is" or redissolve it in heptane/hexane and then freeze-precip if you prefer to clean it.

For evaporating any significant amount of solvents consider a simple distillation setup. Toluene seems to be quite toxic.

Toluene will not freeze precipitate, and its because dmt is too soluble in it even in freeze temperatures. Its not that youre not gonna get decent yield as Trickster said, its that youre not gonna get any yield. Yes you can evaporate it all but thats nasty as hell in terms of smell, in terms of efficiency/wasting products, in terms of ecological sustainability. Instead, salt out your product. Im not sure how FASA or FASI work with toluene, maybe someone else knows.. but you could definitely salt out with FASW or vinegar (just do 3x acidic pulls on the toluene), evaporate the combined water layers. FASW should result in a solid/waxy product, vinegar will probably be a goo. Both can be consumed orally. Otherwise for smokable product, just convert that to freebase. Check the BLAB tek (scroll down wiki front page) for instructions on that conversion

 

[ubu]

Taking pH very high may be necessary to break cell walls, but it could be avoided by doing a few freeze/thaw cycles on soaked mhrb powder before the extraction.

Hello Trickster, that's new info for me. Could you explain a little better this freeze/thaw procedure and what are the advantages/disvantages besides requiring a not so high pH? Thanks a lot!

 

[Trickster]

Very high pH may lead to extraction of some inactive alkaloids.

Such as? (and source for claim please)

Working on this. I hope to write more rigorous reasoning sometime later.

It has been mentioned on the forum. Also this is my experience (personal and limited).

Recently I did many small-scale (20-50g) test extractions changing different variables. I pre-processed mhrb so that cell walls were completely broken and most alkaloid content was emptied into the acidic solution (3 freeze/thaw cycles followed by ethanol extraction in a Soxlet) and then proceeded with a standard A/B extraction followed by freeze-precipitation in hexane.

My yields varied significantly with the pH range I had applied during A/B extraction. Couple of times I changed pH between 2.5 and 13. Average yields were ~1.8%. The product looked like white crystalline powder that does not need any cleaning, but bioassay has shown that it was rather weak.

In 2 latest extractions I narrowed the pH range to 5 - 11 and collected 0.8% of pure white crystalls. Out of curiosity I raised the pH to 12.5 and pulled again. This was done on the same, processed earlier, basic mhrb solution. I collected another 0.5% of fine white crystalline powder. Then I pushed pH to 13.2 and got another 0.5% of the same fine powder. Judging by the results of bioassay these last two extractions yielded progressively weaker product.

Here is my layman reasoning. There are many substances in mhrb with different pKa. In freebase form some of these substances are soluble in NP solvents. If pH of the aqueous solution is well above a substance pKa, most of it is in its freebase form. Also some of these freebases may be only marginally soluble in NP solvents used for pulling DMT. Therefore they may crash out during freeze-precipitation and contaminate the spice. To avoid this it would be andvantageous to keep pH during A/B cycle at pKa +-2 of DMT freebase, i.e. 6.68 - 10.68. Benzyme suggested that this range is too narrow and should be increased to 5-11, which I did.

I would appreciate your comments on the above.

Also, IME, very high pH is the cause of red/brown coloration of NP pulls that leads to red/brown goo in the product.

Not IME.. Never had that problem in my life even extracting with very high pH. It seems there are more factors involved.. would be interesting to try to pinpoint the variables related to why people get that issue.

This has happened to me twice during PanoraMIX extractions. Nevertheless, you're right, the reason could be different.

 

[Trickster]

Taking pH very high may be necessary to break cell walls, but it could be avoided by doing a few freeze/thaw cycles on soaked mhrb powder before the extraction.

Hello Trickster, that's new info for me. Could you explain a little better this freeze/thaw procedure and what are the advantages/disvantages besides requiring a not so high pH? Thanks a lot!

I do the following:
1. Mix and soak mhrb thoroughly in alcohol.
2. Freeze it in a freezer for several hours.
3. Warm it to room temp.
4. Do steps 2 and 3 2 more times.

Sometimes, instead of warming the solution to room temp, I heat it in a microwave and then freeze again. It saves time and microwaves disrupt plant cells as well.

Advantages: more thorough extraction in less time.
Disadvantages: hassle.

 

[DMTripper]

I do the following:
1. Mix and soak mhrb thoroughly in alcohol.
2. Freeze it in a freezer for several hours.
3. Warm it to room temp.
4. Do steps 2 and 3 2 more times.

Sometimes, instead of warming the solution to room temp, I heat it in a microwave and then freeze again. It saves time and microwaves disrupt plant cells as well.

Advantages: more thorough extraction in less time.
Disadvantages: hassle.

Why soak in alcohol? It doesn't even freeze.

Why not water?

 

[Trickster]

Why soak in alcohol? It doesn't even freeze.

Why not water?

I used to do that with water, but now I am experimenting with alcohols for preliminary Soxhlet extraction. All my findings relate only to a specific procedure ( preliminary Soxhlet or CSLE extraction followed by an A/B extraction).

It is probably useless with alcohols. In practice I noticed only slight speeding up of Soxhlet extraction after alcohol freeze/thaw cycles.

With water the idea is simple. Wster expands when freezing and its tiny crystals disrupt cells walls. That's why deep freeze suspended animation is so difficult to achieve.

Theoretically a few water freeze/thaw cycles would be helpful for Herbal Percolator tek and traditional A/B teks, requiring acidic cooks.