DMT a/b WTF?

[homobrassinolide]

So I tried a DMT a/b extraction and I didn't pull squat with my naptha after making basic. Right now I'm using a hot water bath with my aqueous (basic water) and naptha fraction and it seems like it's doing the trick. Before I tried doing it lukewarm and it didn't do squat.

For some reason I feel like I'm losing too much goods with my defatting steps in all my a/b extractions. I think I'm gonna say the hell with defatting from now on.

My reagents...

Botanical: MHRB

reagent grade: HCl, NaOH, d.d. H2O

hardware store grade: Naphtha

I started with a hot extraction with pH 4 d.d. H2O and then of course strained with a coffee filter. I then cold precipitated any lipids that had gotten through by placing my fraction in the refrigerator for an hour and filtering again. I then turned the solution basic with 0.5M NaOH to a pH of 12. Can someone tell me why all the TEKs take the pH well below and above the pKa of the particular functional group in question? I don't get it... Anyway, I tried pulling off the DMT with cold naptha but didn't do a darn thing so I'm using heat now. Let you know how it turns out.

[kcmoxtractor]

Maybe where you cold precipitated your lipids you could have lost some yield? The rest of it sounds perfect and just like any other tek I have ever seen. Are you going to do a sodium carbonate wash at the end before freeze precipitating?

How much naphtha did you use?

Naphtha seems to have a very big change in solubility with temperature with the DMT fb. Why the freeze precipitation works so well. Always do your naphtha pulls in a hot water bath.

I would say the reason for overcompensation is because most don't really have a clue what is going on. Also HCl loses potency when it has been opened, lye can absorb water from the air, etc. The pH changes with the pulls also, so check between each.

[homobrassinolide]

Originally Posted by kcmoxtractor

I would say the reason for overcompensation is because most don't really have a clue what is going on. Also HCl loses potency when it has been opened, lye can absorb water from the air, etc. The pH changes with the pulls also, so check between each.

Not gonna really belabor this one cause I really don't care so much (I'd be lying if I put a lot of effort into responding) but forgive me if I am wrong but the logic behind acid/base extractions is charging/de-charging, by way of protonation/deprotonation, a particular functional group on a molecule. If that's not correct I'll go back to school.

I'll try your extraction kcmo to the letter and let you know how it turns out.

[kcmoxtractor]

I'm kinda confused now... did I say something wrong? Yeah, the DMT changes charge with the different steps to the extraction, I'm sorry if my vocabulary is a little off on the subject its been several years since I had a proper chem class. (Can't wait until next semester!)

[bbd2]

Originally Posted by homobrassinolide

I then turned the solution basic with 0.5M NaOH to a pH of 12. Can someone tell me why all the TEKs take the pH well below and above the pKa of the particular functional group in question? I don't get it...

beyond "high pH (13+) works experimentally"
dont really know

but sometimes i think its an artifact of the naphtha

something about dmt solubilty in naphtha changing as pH changes
maybe its a linear relationship, as pH goes up, dmt solubility increases

not so much that the dmt needs to be turned to freebase
but that naphtha just doesnt dissolve dmt very well at ph 12
it does so better at pH 13+

[homobrassinolide]

sorry kcmoxtractor, "communication breakdown."

From your words

I would say the reason for overcompensation is because most don't really have a clue what is going on.

My bad dude, I'm a schizophrenic apparently. I saw "you" where you have "most." Typical for me. Ashamed. My sincerest apologies, it happens all the freaking time.

[homobrassinolide]

Originally Posted by bbd2

beyond "high pH (13+) works experimentally"
dont really know

but sometimes i think its an artifact of the naphtha

something about dmt solubilty in naphtha changing as pH changes
maybe its a linear relationship, as pH goes up, dmt solubility increases

not so much that the dmt needs to be turned to freebase
but that naphtha just doesnt dissolve dmt very well at ph 12
it does so better at pH 13+

Thanks. It seems a digital pH meter is an essential as paper is just really getting on my nerves.

[Thre365ive]

Originally Posted by homobrassinolide

Thanks. It seems a digital pH meter is an essential as paper is just really getting on my nerves.

Papers are damn near useless with MHRB. So much color from the solution comes out on them that it's almost impossible to read. For the basic step, though, you really don't need one. Just making sure that you have an excess of NaOH should do it.

[dimension traveler]

yep from what you said the only thing that makes since is maybe a higher ph. I always do 13 to be safe over basification is'nt as much of a problem as under lol, when working with mhrb it can be done without a ph meter although I reccomend a meter if you have one. you can tell by the color difference, make sure your basified solution gets black and then maybe put just a little more into be safe. And warmer naptha, I don't like it to hot tho as it seems to pick up more impurities. And yea I dont see a need for defat's it wastes alot of np, as long as you hit all the right ratios and temps in each step you can get white to translucent white thats not waxy without the defat. And of course if u mess up there's always heptane and imo that's a better route to go if needed cause you would use way less heptane than you would naptha doing defats. anyways helps this help best up luck.

[homobrassinolide]

. It looks like some salts are forming at the interface of the naptha and aqueous phase. Fuck yeah!

Yes, indeed, "the blacker the berry, the sweeter the juice," or so the saying goes.

[Norman]

Originally Posted by homobrassinolide

I started with a hot extraction with pH 4 d.d. H2O and then of course strained with a coffee filter. I then cold precipitated any lipids that had gotten through by placing my fraction in the refrigerator for an hour and filtering again. I then turned the solution basic with 0.5M NaOH to a pH of 12. Can someone tell me why all the TEKs take the pH well below and above the pKa of the particular functional group in question? I don't get it... Anyway, I tried pulling off the DMT with cold naptha but didn't do a darn thing so I'm using heat now. Let you know how it turns out.

One has found that filtering the acid solution at all results in a massive loss of goods. Strain it, put it in the fridge and pour the clear solution off of the sludge on the bottom and reduce from there. You can do another cold crash after that, but don't ever filter the solution through anything finer than a tea strainer.
One has also found that a pH of 12 is the minimum required to be able to perform a decent agitation without an emulsion that could be spread with a butterknife, but it still leaves a lot of goods in the aqueous and that taking the pH up past 13 more than doubles the yield.
Here's to hoping you haven't thrown anything away.

[Thre365ive]

Originally Posted by Norman

One has found that filtering the acid solution at all results in a massive loss of goods.

You must be doing something wrong, then. If everything goes properly during the acidic stage, then all your salted alkaloids should be dissolved in the water. Maybe cooking the acidic phase for longer or powdering the bark more would help.

[Jawn]

I'm surprised nobody has said this yet but...

why are you defatting at all? You don't need to defat with MHRB, you only really need to with greenery. Root bark doesn't have the tannins that leaves and grass have, so the step is unnecessary.

And yes, your cold naptha is absolutely a problem. Cold naptha is a step closer to freeze precipitation. Warm solvents can always be more heavily saturated than cold ones, and increasing the temperature of the extraction will give you much better yields.

[Myketos]

Originally Posted by Jawn

I'm surprised nobody has said this yet but...

why are you defatting at all? You don't need to defat with MHRB, you only really need to with greenery. Root bark doesn't have the tannins that leaves and grass have, so the step is unnecessary.

And yes, your cold naptha is absolutely a problem. Cold naptha is a step closer to freeze precipitation. Warm solvents can always be more heavily saturated than cold ones, and increasing the temperature of the extraction will give you much better yields.

With mhrb its all tannins , with greens its lipids!
True no need to defat mhrb , just put your mhrb acid solution in the fridge or let sit 24hrs , pour off leaving sludge behind , you can do this step over and over till nothing settles . Swim has seen the cleanest after doing this for 5-8(times) days until acid solution (mhrb tea) has no residue on the bottom at all. Then goes to the base step to 13.5-14 (can't really go higher) then add your nap<etc naptha at or close to 100%f while jars are in a hot water bath as well , stir with stir rod, pour into sep. funnels wait/drain collect CLEAR nap. freeze etc.....If naptha is piss yellow color as well as your crystals , the acid solution was not clean enough. This will never be seen if you pour off your acid solution leaving sludge behind MORE THAN ONCE or twice, you don't want to see ANY powder residue on the bottom NOTHING .So just allow your mhrb tea (acid) to settle 24hrs room temp or in fridge (cold-defat) , do this over and over until CLEAN bottom (as many times needed until no residue.Crystal Clear spice EVERYTIME!!!!!

[kcmoxtractor]

Originally Posted by Jawn

I'm surprised nobody has said this yet but...

why are you defatting at all? You don't need to defat with MHRB, you only really need to with greenery. Root bark doesn't have the tannins that leaves and grass have, so the step is unnecessary.

And yes, your cold naptha is absolutely a problem. Cold naptha is a step closer to freeze precipitation. Warm solvents can always be more heavily saturated than cold ones, and increasing the temperature of the extraction will give you much better yields.

The reason MHRB is sold is because of its tannins. It is used in leather tanning.

[homobrassinolide]

First DMT experience....

Houston, we are a go for lift off. Let you know how the "business man's trip" is. I'm so pumped. Thank god I won't be tripping all day.

[whatchamacallit]

In SWIM's experience, the a/b comes out cleaner, but the yield comes out much better with an STB, even after recrystallizing, to get it white/clear. It also takes much less work and time, doing an stb instead of an a/b because all the heating, cooling and filtering is a major PITA, and still doesn't give the yield, even with excessive amounts of water that need to be cooked down to a manageable amount. SWIM would have to agree with Norman on this issue.

[Norman]

Originally Posted by Thre365ive

You must be doing something wrong, then. If everything goes properly during the acidic stage, then all your salted alkaloids should be dissolved in the water. Maybe cooking the acidic phase for longer or powdering the bark more would help.

Yeah, I know "should", but I tested it by filtering half a batch and the unfiltered half yielded normally and the filtered half yielded shit.

[Jawn]

With MHRB its all tannins , with greens its lipids!

The reason MHRB is sold is because of its tannins. It is used in leather tanning.

Thanks for correcting! I wrote that backwards, haha.

I love a knowledgeable community.