mini A/B without NP step at the end

[m4estr0]

I wonder if one cannot simply collect DMT freebase from sodium carbonate-basified water, by decanting + drying. Very few people seem to be doing this.

Is this because...

1) It doesn't work very well? (poor yield?)
2) Having traces of sodium carbonate in final product is undesirable/harmful?

 

[downwardsfromzero]

This procedure has been described before. It seems people prefer to collect the alkaloid in a solvent somehow, to ensure a reasonable yield and to avoid contamination with sodium salts. Uncontaminated product makes for more accurate weighing of doses.

 

[m4estr0]

Another reason that I think of myself now is that if the DMT freebase precipitate from basic water solution is decanted and dried, the remaining sodium carbonate in the drops of water covering the DMT freebase is hygroscopic and will be very difficult to dry.

 

[doubledog]

Yes, you can easily obtain dmt fb this way. Just suck out the basic water with syringe through small cotton ball, add very small amount of clean water for washing of fb and suck this water out again. Check pH of this washing water, if it is too high, repeat washing.
No issues with yeild with this method.

 

[m4estr0]

Yes, you can easily obtain dmt fb this way. Just suck out the basic water with syringe through small cotton ball, add very small amount of clean water for washing of fb and suck this water out again. Check pH of this washing water, if it is too high, repeat washing.
No issues with yeild with this method.

What would be the 'too high pH'? >10 ? DMT freebase itself is also slightly soluble in neutral water as it is a very weak base. See PKa - DMT-Nexus Wiki

 

[doubledog]

Washing water should have pH 8, as its purpose is to dissolve remaining base. Washing have to be quick to minimize losses due to solubility of dmt, but in practice, this losses are minimal.

 

[m4estr0]

Yep, and my guess is it also helps if you have big DMT crystals in order not to lose much during the wash.

With freeze precipitation, it is advised to lower the temperature slowly (heat bath -> room temp -> fridge -> freezer) to get big crystals.
I wonder if one can follow a similar "slow" trajectory when basifying a salt solution of DMT, when the pH comes close to 7, every hour or so adding drops of a very weak sodium carbonate solution such that DMT slowly precips out.

 

[Jees]

...I wonder if one can ... basifying a salt solution of DMT...

This was a thread fiddling with the ideas:
Backsalted liquid crashing out. No pull needed.

This was a once off experiment and I would not make conclusions on that, it just shows 'something' might be possible. More experiments are needed especially why the sodcarb did lesser well than ammonia, maybe I just didn't use enough? I left that route and continued with freeze precip in naphtha. But it would be really cool to see people turning it in a very practical format.

 

[doubledog]

I use KOH as a base for precipitation of dmt fb from acidic (vinegar) backsaltings from toluene pulls.
Formation of dmt crystals is almost immediate, but I always wait a few hours for better separation. I separate crystals from basic water, and wash it with clean water. Once I weighed products from each step (including before and after water wash) and was not able to find any losses.

 

[m4estr0]

This was a thread fiddling with the ideas:
Backsalted liquid crashing out. No pull needed.

Wow, cool! I wonder why sodcarb did worse. Also why did milk not form until pH 10 with sodcarb... Something going on there...

Interesting that you bring up ammonia. I think it's also better than sodcarb for washing because it completely evaps.

I use KOH as a base for precipitation of dmt fb from acidic (vinegar) backsaltings from toluene pulls.

Any specific reason for using KOH?

 

[Jees]

I use KOH as a base for precipitation of dmt fb from acidic (vinegar) backsaltings from toluene pulls.
Formation of dmt crystals is almost immediate, but I always wait a few hours for better separation. I separate crystals from basic water, and wash it with clean water. Once I weighed products from each step (including before and after water wash) and was not able to find any losses.

Interesting.
Do you have a number on yields please? Is it on par with pulling + freeze precipitations? You say 'no losses' so I suspect it's quite comparable?

 

[doubledog]

I use KOH as a base for precipitation of dmt fb from acidic (vinegar) backsaltings from toluene pulls.

Any specific reason for using KOH?[/quote]

Not really, maybe that it's a strong base and it's easy to work with.

Yeilds from Mhrb consistently 1.6-1.9% of yellow spice. I never did freeze precip with naphta, so I can not compare.

 

[Jees]

...Yeilds from Mhrb consistently 1.6-1.9% of yellow spice. I never did freeze precip with naphta, so I can not compare.

With the recent bark I get 1.5% with freeze precips. Best bark was max 2% so far.
Your yield is quite okay with that method :thumb_up:

 

[fathomlessness]

It's called the Dry-tek. No one has mentioned using acetone to pull from dried sodium-carb which can then be combined with fumaric to drop out dmt-fumarate (eadible and stable salt of dmt).

 

[Jees]

Since we keep working with a heavily water based method here we can hardly call it a dry-tek

...No one has mentioned using acetone to pull from dried sodium-carb which can then be combined with fumaric to drop out dmt-fumarate (eadible and stable salt of dmt).

With this thread we're closing in on an approach that uses no pull at all onto the backwash liquid, to endeavour if that's possible in practical terms, huray to doubledog for obtaining regular yield numbers. Yes there are more ways to skin a cat but this here is particularly about not pulling with anything and relying on other phenomena to get the job done.

Related: Alternative to Recrystallization: No NP Solvent Needed
What I found interesting in that link is that sodcarb could lead to lesser crystallization effects, somewhat I also discovered in my trials.

 

[m4estr0]

Related: Alternative to Recrystallization: No NP Solvent Needed
What I found interesting in that link is that sodcarb could lead to lesser crystallization effects, somewhat I also discovered in my trials.

There's really something there...
Will definitely use ammonia then.

 

[doubledog]

I am describing how to precipitate dmt fb from acidic water after backsalting toluene, so use of NPS and also water is necessary.

To clarify:
I use normal STB approach to extract dmt fb.

(80g of shredded Mhrb, 40g of KOH, 40 g of NaCl, 550 ml of water.
Mix, wait 3 days, add 60ml of toluene, mix, let separate, wash toluene with acidic water, return toluene to the mix and repeat 5x.
Collect acidic water washes)

Then:
1. Add KOH, low amount, 1g or so, aiming to pH 12, you will see transparent white crystals precipitate very quickly.
2. Cool it.
3. Separate water from crystals - I simply use funnel with cotton ball in it. Wash it with water while still in the funnel - I use 10ml of neutral water without any base. Using sodcarb or even sodbicarb water would be probably better.
After dissolving in IPA and drying, it surprisingly change colour to light brown and consistency to slightly waxy.

 

[Jees]

I am describing how to precipitate dmt fb from acidic water after backsalting toluene, so use of NPS and also water is necessary...

Yes, to obtain the bachwash liquid there were pulls on the bark water. To avoid potential confusion it is good to point out that this thread actually starts from already having your backwash liquid at hand and how to proceed from there with no second pulling strategy in mind.
:thumb_up:

 

[fathomlessness]

Since we keep working with a heavily water based method here we can hardly call it a dry-tek

...No one has mentioned using acetone to pull from dried sodium-carb which can then be combined with fumaric to drop out dmt-fumarate (eadible and stable salt of dmt).

With this thread we're closing in on an approach that uses no pull at all onto the backwash liquid, to endeavour if that's possible in practical terms, huray to doubledog for obtaining regular yield numbers. Yes there are more ways to skin a cat but this here is particularly about not pulling with anything and relying on other phenomena to get the job done.

Related: Alternative to Recrystallization: No NP Solvent Needed
What I found interesting in that link is that sodcarb could lead to lesser crystallization effects, somewhat I also discovered in my trials.

It is to my understanding what the OP explained was called a dry-tek "collect DMT freebase from sodium carbonate-basified water, by decanting + drying".

With respect to "Alternative to Recrystallization: No NP Solvent Needed" thread: it is a thread about recrystalisation where as this thread was originally about a mini A/B which could essentially be both an extraction method or recrystralisation method. I now see you are trying to hone in on that but it wasn't clear whether the OP intended it to be about recrystalisation or extraction.

At any rate, Precipitating alkaloids from a black basified solution full of tannins would be like trying to drink the ocean with a fork, so it is of no use to me. I am just trying to find a method to extract that doesn't involve acid cooks, boiling/reducing, STB or solvent pulls on a basified solution and which is different to the FASA extraction. So far Gibrans tek thread and Benzymes tek look problematic for my purposes for aforementioned reasons in the threads.

 

[Jees]

...It is to my understanding what the OP explained was called a dry-tek "collect DMT freebase from sodium carbonate-basified water, by decanting + drying".

The 'drying' in OP is pointing to evaporating moisture on the obtained crystals at the end. This is unlike a dry-tek which is an extraction technique that occurs with a non watery solvent onto a non watery {substrate that contain freebased alkaloids}. Indeed both have the word 'dry' embedded but refer to different actions altogether.

...At any rate, Precipitating alkaloids from a black basified solution full of tannins would be like...

The suggested precipitation therefore occurs in, as the thread title indicates, a backwash liquid (mini A/B style) which holds no tannins and is white. What precipitates there are clear white crystals, ready to wash and dry (there you have that word again )