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pH one million? (miscalculations)

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syntroniks

Rising Star
So instead of a reasonable amount of water (860mL I beleive), I read it as 460mL.

Basically (pun intended), I have twice the amount of lye I should have, or half the water. I am using 56 grams of MHRB not powdered, but hand shredded and broken into little chunks. All of the MHRB is covered, and the solution is BLACK. Not exactly black, but a very very very very dark alkaloid color. You know what I mean, you all have seen it.

So I suppose my question is: Do I dilute this to proper strength before the naphta pulls, or will it not matter.


I also want to get one thing straight. Since I have basic (pH13+) polar solvent in there now (water), where is the basic nonpolar alkaloid? Surely it couldn't be dissolved in the solution!


Also, the MHRB has been soaking for a bit over 12 hours now, and will until probably tonight when I find a container to do the extracts from. Also, syringe as a seperatory funnel + agitation. I can add naphta to the bottom and have it bubble up through the soup.
 
syntroniks said:
So instead of a reasonable amount of water (860mL I beleive), I read it as 460mL.

Basically (pun intended), I have twice the amount of lye I should have, or half the water. I am using 56 grams of MHRB not powdered, but hand shredded and broken into little chunks. All of the MHRB is covered, and the solution is BLACK. Not exactly black, but a very very very very dark alkaloid color. You know what I mean, you all have seen it.

So I suppose my question is: Do I dilute this to proper strength before the naphta pulls, or will it not matter.


I also want to get one thing straight. Since I have basic (pH13+) polar solvent in there now (water), where is the basic nonpolar alkaloid? Surely it couldn't be dissolved in the solution!


Also, the MHRB has been soaking for a bit over 12 hours now, and will until probably tonight when I find a container to do the extracts from. Also, syringe as a seperatory funnel + agitation. I can add naphta to the bottom and have it bubble up through the soup.


In my amateur opinion: I dont think diluting it with more water will help you too much anymore, but I also dont think diluting it more will be bad in any way.

Some people are against the excessive use of lye saying it ´burns the molecule´, but I honestly have never seen any trustable information regarding this (and if this was so, I guess it would be too late now). Also what people say against excessive lye is that you would need more care, since it would be more chance of residual lye in your final product. This can be properly ´fixed´ with a simple ph 8,5 sodium carbonate wash of the separated naphta.

As for where is the alkaloid.. Well, I dont know, maybe trying to ´hide´ somewhere still in the mimosa, haha.. what matters, though, is that its very very ready jump to the nonpolar solvent :)


as for the naphta ´bubbling up through the soup´, sounds nice but I guess just once would not be enough so there would need some sort of stiring/agitation after that

good luck :)
 
"I also want to get one thing straight. Since I have basic (pH13+) polar solvent in there now (water), where is the basic nonpolar alkaloid? Surely it couldn't be dissolved in the solution!"


Yes, I also pity the dmt molecule when it's being abused ! Think grasshopper .. >! keep thinking ! this may lead you to reconsider the way the dmt molecule is really needing to be handled !

The stb-tek, especially when you heat the lye-stew, replicates the chemical process used in pulp mills. YOur hand-shredded bark is getting 'pulped' (ie digested - releasing all goodies)) but the dmt is clumping up with other insolubles (at pH > 13) -it's clumping up in the black goo, hiding with like, insoluble alkaloids and molecules.

In A-B separation you use only enough lye to basify so that the dmt becomes momentarily insoluble in water, but luckily there's NP solvent for it to 'run' to.
 
What El Ka Bong says is true. But fortunately nonpolar solvents are up to the task of coaxing the DMT from these clathrate-enclosed insolubles.

The only thing to be wary of is that having such a supersaturated hydroxide solution may allow a slight bit of lye to migrate into your nonpolar phase, particularly if the extraction is heated. This problem can be fixed by doing a sodium carbonate wash on the nonpolar extraction.
 
hmmmm, so if I were to dilute the solution closer to 13-12 PH, it wouldn't give me all that much benefit be cause the DMT has already "clumped" up with other insolubles?

I'd be better off extracting and washing the extract w/soda ash then I suppose. Instead of soda ash, how about some good 'ol ammonia? I've heard that that would be BAD!

Any basic (8-10pH) polar wash should leave the DMT alone while taking any lye away...


I'm going to read responses/ thoughts before proceeding. Thank you all for being so supportive !


---Edit

Is DMT broken down/ destroyed in a very basic environment?!?
 
Well, I dont know how much is left in the soup, but there definitely was some dmt and it did come out. A but oily though. I didn't wait to fully evaporate I suppose. Either way, I got a peek into hyperspace. Maybe next time I'll do things right for a change
 
Practice makes perfect ! And stay away from "supersaturated" lye solutions ..!

All my opinions about this chemistry have an experiential basis for them - I go on because there are facts of chemistry to appreciate - like this concise statement:

"The only thing to be wary of is that having such a supersaturated hydroxide solution may allow a slight bit of lye to migrate into your nonpolar phase, particularly if the extraction is heated..."

When basifying an acid extract, you also risk lye contamination, and this might only be to a pH of 11 or 12. When people talk about a pH of 14, it's ludicrous, and totally off-scale - this is 1000 times more concentrated in [OH] than a pH of 11 - why do you need to go beyond a pH of 12 ..? (ans - because some believe in 'pulp-milling' the MHRB, which might be a way to go if you can't grind the bark, and insist on doing a washing step.)

But re washing - I have to clarify, by asking:

The ammonia wash is done on solid crystals, right ? This is when you pour liquid ammonia solution (3% NH4 in H2O) over your crystals that were scraped up after evaporating ?

But what is a bicarbonate wash ? Is that a step you do by mixing liquid bicarbonate solution with the liquid NP solvent (that has been used to pull dmt from basified extract). YOu mix them up a bit and then you re-separate the liquids..? Does this lead to less loss of dmt - if you mix two liquids at pH > 8.73 ?

If I understand it correctly ammonia washes work like this - the ammonia (NH4+) grabs the lye's (OH-) making ammonium hydroxide, which is itself polar so it stays dissolved and moves with the water through the filter. Dmt is not going to dissolve in the ammonia because it is an alkaline solution (> pH 8.73 = pKa of dmt). The Na+ from lye also stays dissolved, and washes out through the filter, leaving cleaned dmt in the filter. What else is washed out - the answer depends on NP solvent used, I'd guess ?

Still you lose some dmt when washing - can someone give the explanantion for this ? It's because of pH right ?! (If the pH is too close to pH 8.73, there is some dmt-freebase reverting to dmt-salt, is this why ?)


Oh ! And then I found a definition of 'clathrate'


So I am left pondering - how does the creation of 'clathrates' promote the clean, highest yeilding extraction possible of pure dmt from MHRB ? Anyone have any ideas .!? Do clathrates help isolate dmt, and can they actually protect the molecule before it finds it's way into the naphtha ? This could be, but I wonder what else comes along for the clathrate-clumpy ride ?

Instead of creating a clathrate crust or 'cage', it would seem so much easier to get dmt out of a soft "Hydration shell" of protective water molecules - resulting from leaving the pulverized MHRB in pH 2.0 water.

Imagine dmt is the green, positvely-charged moelcule in this diagram of a hydration shell -


Or for an animated of hydration shells, look here -




EDIT !

Copy and paste these links - I can't get it to work in this post -



Or here, the background section describes it -


Imagine pure dmt encased in concentric layers of 'hyrdation shells', floating happily, invisibly, totally soluble and safe in water. A happy, dmt solution.

Then imagine 'clathrate' encapsulated dmt, clumped with gunk, that you are trying to get onto a naphtha layer - does that sound like an 'easier' way to get the dmt out of MHRB?

In contrast - imagine dmt just popping it's watery hydration shells as the pH jumps from 2.0 to 11.5 ! A screaming crowd of 'naked' spice molecules looking for a home !

Although it works, to a yeild that satisfys most people, this sounds like an unfiltered, dmt-dungeon, from which you will have to wash the dmt you do 'rescue' from pHell !
 
El Ka Bong said:
Still you lose some dmt when washing - can someone give the explanantion for this ? It's because of pH right ?! (If the pH is too close to pH 8.73, there is some dmt-freebase reverting to dmt-salt, is this why ?)
is it a fact that you lose dmt when cleaning it? Or is it just the weight of the impurities you are washing away? Thus turning your 3 grams of spice into 2.8 grams of spice for example.
 
XENONSION said:
El Ka Bong said:
Still you lose some dmt when washing - can someone give the explanantion for this ? It's because of pH right ?! (If the pH is too close to pH 8.73, there is some dmt-freebase reverting to dmt-salt, is this why ?)
is it a fact that you lose dmt when cleaning it? Or is it just the weight of the impurities you are washing away? Thus turning your 3 grams of spice into 2.8 grams of spice for example.


I would guess it depends on what you are washing with, at what pH. How do you minimize dmt loss ?

100% purity, can it ever be achieved - what amount of washing is needed? We hear of 1.4 and 2.0% yeild sometimes, around here, which sounds full of something that is water soluble, or not (clathrate- buddies with dmt could be other desireable alkaloids too).
 
El Ka Bong said:
XENONSION said:
El Ka Bong said:
Still you lose some dmt when washing - can someone give the explanantion for this ? It's because of pH right ?! (If the pH is too close to pH 8.73, there is some dmt-freebase reverting to dmt-salt, is this why ?)
is it a fact that you lose dmt when cleaning it? Or is it just the weight of the impurities you are washing away? Thus turning your 3 grams of spice into 2.8 grams of spice for example.


I would guess it depends on what you are washing with, at what pH. How do you minimize dmt loss ?

100% purity, can it ever be achieved - what amount of washing is needed? We hear of 1.4 and 2.0% yeild sometimes, around here, which sounds full of something that is water soluble, or not (clathrate- buddies with dmt could be other desireable alkaloids too).
I dunno, that's why i was asking, lol.

Doesn't make much sense that the washing would remove any dmt. Any weight loss, one would assume would be from the impurities being washed away.

How you can figure how much dmt, if any at all, is lost during the wash process?
 
Why lye may supersaturate: The more you add, the hotter it gets...

How Ammonia wash may work: It takes the polar lye which happened to get into the Nonpolar solvent


or it may react... Nice post Ka Bong, lots of info there!
 
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