Hybrid tek hypothesis

[dooby]

Hello,

What I am about to propose is not so much a new thing as it is a combination of existing methods and I am reasonably confident that what I am about to propose is already being done by some people but I have yet to find a write-up of this method...

I will include one step that I think is new, although it is merely doing things in a different order...

This method uses mhrb, vinegar, salt, sodium hydroxide and naphtha...

1 freeze/thaw cycle
2 acidify with vinegar
3 add salt
4 add sodium hydroxide
5 pull with naphtha - warm or cold doesn't matter, excessive amounts of naphtha shouldn't be a problem either...
6 salt naphtha with vinegar
7 allow to separate
8 decant most but not all of the naphtha
9 add salt
10 add sodium hydroxide
11 mix
12 let separate
13 decant naphtha
14 slow evap

The "trick" lies in using as little vinegar as possible to salt out the alkaloids from the naphtha so it's as close as possible to saturation, then letting enough naphtha sit in the jar for the expected amount of alkaloids but still as little as possible... when the sodium hydroxide is added, precipitation of the alks will be very visible and the heat created will heat the naphtha, mix this hard and fast, let separate, your pull should be very saturated...if the solution isn't clear/transparent after this step, pull again with fresh warm/hot naphtha then combine pulls (repeat until solution is clear)

If anyone is interested I'll provide some more detailed answers...

I'll be happy to answer any questions or comments...

PLUR

 

[DreaMTripper]

The theory is good more quick reduction methods are needed but the problem I see with excess naptha is the physical space the vinegar has to cover to salt out the alkaloids.
Ive read 1ml dissolves 150mg which is great however contact has to be made with the vinegar and dmt in the first place. It doesnt get pulled to the vinegar so you may need to use equal amount of solution with no reduction having happened and the freebasing to do again..
I could be wrong I dont have full knowledge of the science behind salting out.

 

[dooby]

You probably have a point there...

What I meant was that if you do it cold, the extra amount of solvent you need compared to doing warm/hot pulls should be no problem...

One way around this would be to salt the first pull, decant the naphtha then salt the second pull in the same vinegar...

Also, adequate mixing...

 

[DreaMTripper]

Yeah that could work. Back salting usually loses a portion of spice somehow so as long as you dont mind that then its well worth an experiment.
Using a test tube would increase the chances of success I think back salting bit by bit using the same vinegar to pull salt each time.

 

[dooby]

What is the mechanism or principle that causes loss of spice in a back-salting situation?

Is there an indication to be found anywhere as to the amount/percentage of yield that is lost in this way? Is it high enough to warrant the purchase of a freezer?

 

[cyb]

is it high enough to warrant the purchase of a freezer?

You would save yourself a whole lot of agro if you managed to get a freezer...
20 bucks at a garage sale or charity shop...or a trip to the city dump for a free one.
It doesn't have to be a full size unit.

 

[dooby]

Back salting usually loses a portion of spice somehow

I have been thinking about this and I can see only two possible explanations:

- Not all freebase molecules are converted into their salt form
- The salt form of the molecule is partially soluble in the nps...

Maybe I'll evap some vinegar-salted naphtha in the near future to check if it leaves behind either freebase or acetate molecules...

Or can anyone answer the question without me having to experiment?

 

[DreaMTripper]

Im not sure why, a freezer is definitely ideal and safer. If its cold enough there and np is saturated enough outside over night may precipitate then you can filter through micro filters and fan evap the rest
What yeild are you expecting?

 

[downwardsfromzero]

Your "tek" starts: "1 freeze/thaw cycle". Surely you'd need a freezer to do that?

 

[dooby]

Your "tek" starts: "1 freeze/thaw cycle". Surely you'd need a freezer to do that?

I'm using somebody else's freezer for this, but I can't use it for precipitation purposes...

Still wondering about this though...

- Not all freebase molecules are converted into their salt form
- The salt form of the molecule is partially soluble in the nps...

 

[DreaMTripper]

Your "tek" starts: "1 freeze/thaw cycle". Surely you'd need a freezer to do that?

I'm using somebody else's freezer for this, but I can't use it for precipitation purposes...

Still wondering about this though...

- Not all freebase molecules are converted into their salt form
- The salt form of the molecule is partially soluble in the nps...

Yes I'd say both. I would guess that some is also decomposed during the process.

 

[Infundibulum]

Your "tek" starts: "1 freeze/thaw cycle". Surely you'd need a freezer to do that?

I'm using somebody else's freezer for this, but I can't use it for precipitation purposes...

Still wondering about this though...

- Not all freebase molecules are converted into their salt form
- The salt form of the molecule is partially soluble in the nps...

Yes I'd say both. I would guess that some is also decomposed during the process.

I doubt either;

Practically all frebases are converted to their salt form during salting (or something along the 99.9999% line...) And practically none of the salt forms (or at least no more than 0.0001%) is soluble in the NPS. I have heard rumors that dmt acetate is somewhat soluble in halogenated solvents (like chloroform or DCM) but then again I do not know if the person who said as such did it with dmt acetate or with dmt acetate dissolved in water (which is two different things).

Dooby, I do not understand what is the catch with this hybrid tek, or why it is called hybrid to begin with; because of the backsalting? This is an old enough technique. Because of teh minimum vinegar? The minimum amount of vinegar isn't really going to get you good salting of the NPS - it is better to use more than less and ensure good mixing, i.e. at least 10% the volume of the NPS you want to salt and salt 3 times.

A In a good extraction one ideally salts the NPS pull 3 times, then uses the very same NPS (now devoid or holding a minimum of non-recovered alkaloids) to pull freebases from the basic soup, then proceed to salt again and so forth. This way you use the minimum amount of NPS overall and ensures no loss of actives; your final NPS pull will have traces of freeabses only and when you salt it you will practically get everything out of it.

Also, contrary to what the others say, a freezer is absolutely not necessary. It is very useful though if you want to crystallise and re-crystallise, but personally I wouldn't care less. On the other hand, a separatory funnel (or a contraption that does a similar job like a glass gravy separator) is really a saver for salting the NPS.

 

[Randomness]

At the start of your tek you do a freeze thaw and then add vinegar and soak. I have had real good success with soaking the powdered bark in vinegar covering and microwaving for 30 seconds at a time until the bark goes like Thai current paste. If you did that first or even just added vinegar then froze then the water crystals will help rip the bark to bits and push the acid further into the cells.

Just doing the microwave part and leaving as a paste for a few days I got a deep blood red liquid as soon as I added my water for the extraction.

 

[Randomness]

BTW I managed to salt 0.6 g of spice into 20ml vinegar from limonene after this point it started forming emulsions and would not retrieve any more (this could work better with naphtha as it is less polar). Upon addition of 2g sodium hydroxide spice was able to be retrieved by heating and shaking solution as in Ice House's freebase conversion tek. Everything stuck to the side of the jar and was retrieved and cleaned with acetone to leave two large honey coloured crystals upon evaporation. Second time trying this resulted in an oil rather than crystals.

You could just make a simple soxhlet extractor for a few pounds (real easy to do) to reduce your initial pulls to the point where they were supersaturated and just evaporate from there. Would save all the extra steps and not waste any excess solvent.

 

[DreaMTripper]

Good to know thanks for clearing that up infundibulum.

 

[dooby]

@Infundibulum: I thought of this because I don't have a freezer and wanted to keep the amount of solvent to be evaporated to a minimum... Also, for those who do own a freezer, it would reduce the need for pre-evaporation of less saturated pulls before freeze-precip...

I am trying to use a little solvent as possible and use it as many times as possible.
I a grateful for your explanation regarding amounts, ratios and the fact that I should salt three times (with fresh vinegar?)

@Randomness: Thank you for sharing your experience and insight... The microwave might be very helpful indeed... I haven't freeze/thawed with vinegar yet but I will the next time...

 

[Infundibulum]

@dooby: Yes, repeated saltings are done with fresh vinegar each time. Think of it washing clothes; the more soak in water + discard water cycles you do, the cleaner it will be and that a single soak with a lot of water will not make the clothes as clean.

Mind you, depending on your technique and the scale of the extraction, in the end you will be left with a fair amount of vinegar that will need volume reduction - this can be quite smelly. Maybe you could consider using an alternative acid, like citric acid? This is easily obtainable, food grade with applications in home wine making, is not volatile and does not stink the house. DMT citrate is also one of the dmt salts that is thought to be particularly (i.e. on par with acetates) soluble in water.

 

[dooby]

Thanks... Citric acid will be given a try in the near future...

I assumed, incorrectly so it seems, that using a minimum amount of vinegar and shaking thoroughly over extended periods of time would result in higher saturation of the vinegar with dmt-acetate thus reducing the need for evaporation...

Now that I know this assumption is wrong, I am inclined to abandon vinegar experiments mainly because of its impurities (that show up under basic conditions - floats on water, insoluble in hot naphtha)(when pulling from a clear liquid this gives the false impression that alkaloids are in there when there aren't)

I'm also getting some toluene and fumaric acid from a friend "for Christams"

PLUR