0% yield with Cybs Max ION Tek

[lowski]

Dear Nexanians,

--- tldr;

i know it might be a rude first post and certainly not the right section. But since im not promoted yet, i don't know where else to turn.

I had about 500g of MHRB and i did a few 100g and 50g extractions, using different tek everytime. I thought this would be the smart thing to do, getting to know the different methods and find the one that works best for me.

In retroperspective i think its much better to stick to one tek and really get the hang of it than the other way around.

Anyway. So much for my skill level. For the last 100g bark i chose to follow "Cyb's Max ION" Tek. Obviously not the most basic and beginner friendly tek but i really liked the guide. The explanation and reasoning behind each step and for the most part cyb

So i followed the guide as you will see, however after the 2x 3 pulls i yielded absolutely nothing. And with nothing i mean there are 2 small flakes at the bottom of my jar, that sits in the freezer right now. (maybe 10mg)

Today i was about to throw the soup out but then i thought of the saying "if its not in the collection jar, its still in the soup" something along those lines. I tried to figure it out

----

I followed the instructions closely but did a few things differently


1. Im not sure it i have bought the wrong vinegar but it ph4 by itself. not sure how it would be possible to get it lower than that after adding water and bark. This is why i used citric acid (food grade) A couple of spoons until the final mix for the acid bath was somewhere between ph 2 - 3.

2. it kept this mix between 40 - 50 degrees Celsius using heat baths for about 8 - 9 hours. after that i added around 80g of salt and topped up with dest. water for a total of around 800ml litres (my flaks only holds ca. 1200ml)

the last 200ml were used to mix in 100g of lye (NaOh - Natrium Hydroxide) i mixed the base with the rest of the mix and gave it another hour in the heat bath. then waited a couple of hours for the mix to get back to room temp and made 3 x 40ml pulls with warm or hot naphtha.

let a bit of the Naptha evap, freeze over night... but the next day.. nothing. just clear naphtha in my freezing jars. i collected the Naptha for re use and let the soup sit for a weekend. then i tried another pull with the same measures as last time. how ever i found the ph to be 10 at best. i added the rest of my lye (probably 100 - 150g for a total of 2000) after that i ended up at ph11 maybe.. which is not high with this amount of lye i would have expected at least 12 maybe 13.

anyway i made the pulls ( heated Naptha to 50 and / or 70 degrees, added it to the mix, rolled the flask for 5 minutes, then let it separate and got it out. ) and again. there is absolutely nothing in my freezer.

so where did i go wrong? is it because of the citric acid or the wrong amount of salt? The obvious would be the basification, maybe the NaOh i bought is shitty and the ph just not high enough. can i increase it somehow without buying new lye? maybe by adding a few pinches of sodium carbonate?


It would be really nice if somebody could shed some light on this or just try to.


thanks

david

 

[downwardsfromzero]

It could be that you used too much citric acid and not enough base. Seeing as you apparently used the same batch of bark with which you'd had success before, it shouldn't be a bark issue - although you haven't explicitly stated that your previous extractions were successful.

Another thing to be aware of is that you might as well keep the base soup warm because adding a bit of warm naphtha to it when it's at room temperature just cools the naphtha down. The heat capacity of water is way higher than that of naphtha.

So, I'd suggest adding another dose of (decent) lye and extracting from the warm solution - the standard warning applies: no naked flames, use a hot water bath!

 

[Hyper Turtle]

I had about 500g of MHRB and i did a few 100g and 50g extractions, using different tek everytime. I thought this would be the smart thing to do, getting to know the different methods and find the one that works best for me.

In retroperspective i think its much better to stick to one tek and really get the hang of it than the other way around.

I think both are good approaches. I feel that by trying many teks, i learned something different each time and got a bit more of an understanding what is really going on. But sticking with one and perfecting it sounds like a good idea too

I'm really not sure why you have (almost) no yield. I suspect that part of the problem was that you added a lot of acid, then had to add a lot of base, and the resulting buffer system trapped part of your alkaloids. Ime the soup can get quite thick/viscous when there's a lot of lye in it, which might not help either.

If it was my extraction, next thing i'd try would be to add some more salt water and do more pulls, this time heating both the soup and naphtha. I'm not sure that it'll help but i think it's worth a try.

 

[downwardsfromzero]

Yep, too much citrate will produce a PITA buffer system as well - and can also contribute to emulsions (some have claimed) due to its emulsifying properties.

 

[mud1]

FWIW I did the max ION tek the first time too, I think the main recommendation I could make would be to test the PH of the soup before you do your first pull, but since you tested later on it doesn't seem like that's the issue.

is it because of the citric acid or the wrong amount of salt?

I used a mix of citric and acetic and it worked fine, I think I might have used more salt than you. Personally I think the salt amount shouldn't matter since if you dissolve too much, worst case is that it just won't dissolve further.

Yep, too much citrate will produce a PITA buffer system as well - and can also contribute to emulsions (some have claimed) due to its emulsifying properties.

Wasn't aware of this issue, but fwiw my pulls separated waaaay to fast with citric/acetic mix. I did use a hot water bath at 140 F though. The naphtha would separate almost immediately.

The obvious would be the basification, maybe the NaOh i bought is shitty and the ph just not high enough. can i increase it somehow without buying new lye? maybe by adding a few pinches of sodium carbonate?

Also doubt this was an issue, as long as the lye brings your pH up, it should be acceptable lye. The whole point of the extraction teks are to bring the pH above a certain threshold.

I suspect that part of the problem was that you added a lot of acid, then had to add a lot of base, and the resulting buffer system trapped part of your alkaloids

Would you mind explaining a little more about how a buffer system can trap the alks? I thought the main thing that mattered was the the pH being above 12?


Overall, if the wrong acid/too much base may hurt your yield, maybe lowski you can try doing a STB extraction, you that would reduce the chances of both issues.

 

[downwardsfromzero]

A buffer system will interfere with pH changes, slowing them down and spreading them out.

Buffer solution - Wikipedia

en.wikipedia.org

 

[Hyper Turtle]

Would you mind explaining a little more about how a buffer system can trap the alks? I thought the main thing that mattered was the the pH being above 12?

I'd love to, but i'm afraid i don't understand it well enough. If i understood it correctly when it was explained to me, it's an equilibrium thing. Like, overall pH will convert the alkaloid to freebase, but some of it keeps getting converted back to salt due to the presence of the acid.

 

[downwardsfromzero]

This graph sums it up:

File:Buffer titration graph.svg - Wikipedia

en.wikipedia.org

"Citric acid is a useful component of a buffer mixture because it has three pKa values, separated by less than two."

 

[acacian]

Hey Lowski

.. Personally I don't have experience extracting from mimosa hostilis but do have extensive experience working with various acacias and feel like the issues I'll point out could potentially cross over into other species.. and with some acacia species prolonged exposure to high acidy seems to break down the alkaloids - reducing final yields... obviously nn-DMT as a compound does pretty well in low ph solutions but I think that in some plants the acidity can cause undesireable reactions between other compounds in the solution which may have a knock on effect on the alkaloids. Prolonged exposure to high heat can also have this effect with some acacia species.

I thought of this when I saw that you had your soup sitting at a ph of 2-3 for 8 hours.. otherwise my impression was that mimosa hostilis copes iwth high acidity quite well. Although I think you would be safer working between ph 4-5.

How old was your bark? Had it sat for long periods of time between trying the various teks? How'd you store it?

I think its good you are trying differen't teks.. realistically you don't want to be relying on teks too much to do extractions though.. or at least understanding the chemistry behind the tek you are doing goes a long way .. so that come any problems you can work your way out of situations the tek might not address

Lastly, did you evap your naptha in the end?

 

[acacian]

Just food for thought.. I think its useful to know some of the basic principles behind DMT extraction (maybe you do already but i'll post this anyways).. better if some of the more versed chemists chime in here but this is my basic take..

Firstly that DMT occurs as a salt in plants.. the salt is water soluble from neutral down to the acidic spectrum (so ph 7 and under, but too low will degrade it... and the plant itself will often bring the ph down anyways) however a more acidic solution helps speed up this process as the dmt will bond to the acid that is added. Since DMT as a salt is so soluble in acidic water, the best way to isolate it from the solution is to make the solution basic so that it becomes insoluble in the solution. This way you leave behind a lot of unwanted compounds that will stay dissolved in the water despite the ph change

DMT becomes a freebase when its holding solution is made alkaline.. the freebase is not soluble in water and will as a result precipitate from the solution. The next step is to use a solvent that is not miscible with water and that DMT freebase will readily dissolve in..

The floating freebase crystals will dissolve in the solvent as they come into contact and the solvent then needs to be drawn off of the solution and either evaporated or depending on the solvent cooled down to precpitate DMT which is insoluble in some solvents at cool temps

 

[lowski]

Thanks for your replies

So, I'd suggest adding another dose of (decent) lye and extracting from the warm solution - the standard warning applies: no naked flames, use a hot water bath!

If it was my extraction, next thing i'd try would be to add some more salt water and do more pulls, this time heating both the soup and naphtha. I'm not sure that it'll help but i think it's worth a try.

Im hitting a few constrains. My Flask only holds a little above 1l and i don't have anymore lye lying around. ^^
So this might be the point where i take a second flask, split the soup and top up both bottles to 1l again using salt water.

It the problem was and still is that the ph is not high enough, i really don't know what to do. Testing with litmus paper while you have even the tiniest layer of naphtha floating on top is hardly possible, if at all. Also me and the color chart comparison that's a story in itself... i should have gone digital.

I have however sodium carbonate at hand. I got it to wash the yellowish naphtha that was collected during all prior extractions. Now i don't even now if its basic enough to get the soups ph up at this point and from what i read its really not suggested at all.


So at this point, the soup has been sitting with the additional lye for almost 3 days. So the next thing ill do is another pull as is.. but with warm soup (30-40) and hot naptha (60-75). Ill make the split into the second bottle afterwards and the following pulls in the next couple of days
.
Meanwhile things start to show up after freezing but in amounts that - if one would try to scrape them - would end up with next to nothing probably. So i collect the naphtha and fan dry as usual. If i spot some low hanging fruits of contamination, ill try to get it out but otherwise i just add the naphtha from the new pull and freeze again.

 

[acacian]

You could always just extract the spice out of the cold soup with a solvent like xylene, toluene .. they don't require being heated - the difference is that you need to evap these instead of the precipitation method. You can then do further steps to crystalize your extract with naptha.. but you can be sure if the solution is ph 12 or above and you use any of those solvents i mentioned, that will pretty reliably pull it out (and you should need no more than say 75 to 100ml).. no need to mess around with heat

 

[mud1]

Firstly that DMT occurs as a salt in plants.. the salt is water soluble from neutral down to the acidic spectrum (so ph 7 and under, but too low will degrade it... and the plant itself will often bring the ph down anyways) however a more acidic solution helps speed up this process as the dmt will bond to the acid that is added. Since DMT as a salt is so soluble in acidic water, the best way to isolate it from the solution is to make the solution basic so that it becomes insoluble in the solution. This way you leave behind a lot of unwanted compounds that will stay dissolved in the water despite the ph change

Thanks, this clears up some info for me, I always wondered why we added acid to AB extractions, but all previous explanations weren't great. But this leaves me with a few questions you could hopefully help me answer:

1. If the DMT is in salt form in the plant, why bother add more acid? Salt form DMT isn't going to bond to the acid. (you mentioned salt DMT is more soluble in acid water, so is that another main reason?) Is the acid to capture any lingering freebase DMT so that it becomes water soluble?

Someone once told me the acid step was to break down the plant matter but that doesn't sound accurate since the lye would also break down the plant matter.

2. How long is too long for DMT to degrade? The tek I used had me put a 2 pH DMT acid soup in a 60C bath for 8 hours. I still ended up with 1% yield. I do wonder if that was too long, too hot, or too acidic.

3. Will DMT break down if you leave it in too basic a solution for too long? I have heard of people using NaOH or KOH and leaving that base soup for a week before starting to extract.

It the problem was and still is that the ph is not high enough, i really don't know what to do. Testing with litmus paper while you have even the tiniest layer of naphtha floating on top is hardly possible, if at all. Also me and the color chart comparison that's a story in itself... i should have gone digital.

Since you probably have a turkey baster or pipette, you can just use that to extract a drop below the naphtha and drop it on your ph paper.

 

[acacian]

DMT occurs as a tannate.. which is water soluble.. however other DMT salts such as acetate and citrate are more readily soluble in water. DMT tannate is perfectly soluble in water still.. it just quickens the process changing it to some other salts

I'm not really sure how long it takes DMT to degrade in boiling water.. its likely that the length of time could vary from plant to plant depending on whether there are compounds present that might cause undesireable reactions when exposed to prolonged acid or heat.. nen888 is quite knowledgeable on this and might be worth messaging.. he is the guy who started the trying to improve acacia info thread (link is in my signature)