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Two FASx Questions Prior to My First Extraction Options
 
mikeAtHome
#1 Posted : 8/7/2017 6:19:27 PM

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Hi everyone. I’m planning my first extraction (in the DMT world) using MHRB and have been reading threads, searching our Wiki and slugging through a ton of research done on plant-based extractions in general as well as those targeting alkaloids. I’ve done a number of extractions before but on compounds very different from DMT. For one thing, the end product extraction (as opposed to intermediate extractions for isolating impurities etc.) always used NaOH/HCL. Nice strong conjugates. Additionally, my end product was a salt. So: no need for smelly solvent evaps or multiple precips, stable, easily washed (cold acetone) and Xtalised (boiling IPA). I really want to go the FASx way. My questions are:

1. If I’m reading things correctly. DMT-f is VS in H2O (1g/ml). My previous extractions were usually pulling 1 to 2 grams of honey with identical solubility. But I used about 75ml in the aqueous layer and usually had very little come out on the 3rd pull. It really didn’t matter what the volume of basified solvent was. Other folks going after an oz. of product would report 14g from their first 100ml pull! Can someone explain how DMT is different? I read in one thread someone saying that DMT was stubborn about coming out of water but that was in reference to the extraction from bark. And I could swear I'm heard other members say it wasn't that water soluble at all (I know the acid sure isn't). Is it really that stubborn in a titration or am I using incorrect solubility data?

2. I would also like some advice on which of 2 ways I should go when it comes to obtaining the salt. One way is to follow FASx extraction guidelines and go right to the DMT Fumarate. Another way would be to follow some other tek – I like STB and Jorkest’s tek looks like it got good yields. That tek uses NaOH which is not compatible with FASx. Not a problem. I could use HCL to obtain the salt. Maybe give it a wash and then basify with Ca(OH)2 and salt out using fumaric acid, wash w. cold acetone and Xtalize w. boiling IPA (soluble at 1g/200ml). Will this work or is it just plain crazy?

This is a much different world than I am used to and I’m obviously no chemist so please don’t take this as a challenge to tek being used in FASx and A/B but… A lot of the tek is more volume-oriented than it is ph-oriented when it comes to hitting certain targets. Maybe I’m just paranoid but I’d always check ph prior to water washing a basified solvent and after every water pull to make sure I was on target (ph=6.5) . You’re using different A/B combos here and I know each pairing can have its own rules about the ease or lack thereof in changing ph. And I really don't completely understand all of the ionic influences in play. It would be nice to not feel so anal about ph if there’s no call. It’s a PITA and I go through a shit-ton of ph paper.

Probably took too long to ask a couple questions; will attempt more brevity from here on… Thanks.
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endlessness
#2 Posted : 8/7/2017 9:12:20 PM

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Does it really matter the exact solubility of DMT fumarate? If you are salting out with FASW, do 3 pulls, the first one or two will have most product, the last one will have less product, but you dont want to waste anything, so why avoid the third pull since its so simple?

I dont know what posts you are referencing to saying "DMT is stubborn coming out of water". Without more context its hard to know.. Are we talking about dissolving DMT from whole bark into acidified water? Are we talking about salting out DMT from a non-polar solvent? Are we talking about using DMT Fumarate as is your case, or something else? I think you are worrying too much here.. Just do 3x FASW pulls or add FASI/FASA to your non-polar till it stops cloudying, and there you have it.

Regarding what you said about NaOH not being compatible with FASx, I dont know where you got that idea from? Read BLAB tek for example... Also, how does the base matter for fumarate salting, if the fumaric acid will never come close to the base, since you are first using a non-polar and only after separating that you will use the fumaric acid to salt out the non-polar.

Lastly, it is completely unnecessary to measure the PH, and you dont have to understand the ionic influences at play, it wont increase your yield or make your product purer. The products from these teks, for example BLAB, have been tested with GC/LC-MS and have shown to be very pure (90+%) without any need of special measurements.

The only common extraction where measuring the pH is important is for mescaline extraction when salting with HCl.. Other than that, totally unnecessary.

Hope that helps
 
mikeAtHome
#3 Posted : 8/8/2017 1:28:34 AM

The only God I can imagine is a God that I can't possibly imagine


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Thanks for such a quick reply, endlessness. A lot of what you said eases my mind.
But to clarify:
endlessness wrote:
Does it really matter the exact solubility of DMT fumarate? If you are salting out with FASW, do 3 pulls, the first one or two will have most product, the last one will have less product, but you dont want to waste anything, so why avoid the third pull since its so simple?

Yes, I am planning on 3 pulls. It's just a question of how much water really needs to be there. And I see now that the FASW you wrote calls for very little water needed in the pulls. I must have been tripping. I could have sworn a larger volume was suggested. I've been reading through so many teks and it seems most folks like winding up with the freebase. That's just my impression. Some of the extractions can go for 6 pulls or so (of solvent). The FASW tek is where I want to finish but I did like some of Cyb's STB thinking on the extractions. Didn't know if there was some incompatibility or not.
endlessness wrote:

I dont know what posts you are referencing to saying "DMT is stubborn coming out of water". Without more context its hard to know.. Are we talking about dissolving DMT from whole bark into acidified water? Are we talking about salting out DMT from a non-polar solvent? Are we talking about using DMT Fumarate as is your case, or something else? I think you are worrying too much here.. Just do 3x FASW pulls or add FASI/FASA to your non-polar till it stops cloudying, and there you have it.

Okay, on this one I wasn't tripping. I spent some time trying to find it again but the Forums and Wiki are extensive so I couldn't find it. The context was: person wanted to know if they did not need to defat, could they just skip basification entirely and get the extract by evaporating the acid alc/water soak (whatever it was). The answer was no, followed by some phrase about DMT, water and being stubborn. Maybe it wasn't "coming out" but the "going into" water that got mentioned. Just thought maybe there might be something different about titration of DMT salt. Glad to hear there isn't.
endlessness wrote:

Regarding what you said about NaOH not being compatible with FASx, I dont know where you got that idea from? Read BLAB tek for example... Also, how does the base matter for fumarate salting, if the fumaric acid will never come close to the base, since you are first using a non-polar and only after separating that you will use the fumaric acid to salt out the non-polar.


Yeah, there's a thread, fairly recently posted 1)why can't you use lye 2) does NP solvent... and you clear that up right away. Plus I must be mis-remembering other instances of remonstrances to the effect of, "no, you can't substitute using NaOH..." I have no idea why I shouldn't be able to salt out with fumaric/NaOH. I just don't recall seeing that combo and have read some organic chem stuff about needing to do your due diligence when not using conjugates. And you have to admit, fumaric acid is just a little weird. Not very soluble, 2 pKa's, weak... Thanks for the BLAB mention. Good stuff.

endlessness wrote:

Lastly, it is completely unnecessary to measure the PH, and you dont have to understand the ionic influences at play, it wont increase your yield or make your product purer. The products from these teks, for example BLAB, have been tested with GC/LC-MS and have shown to be very pure (90+%) without any need of special measurements.

Again, good to hear. Doesn't seem to be a lot of worry about that here. You just hear things here and there like ph too hi/lo damages the alkaloid or pull at too low a ph and you start getting garbage, pull too high and you leave product behind etc. But it seems DMT pulls are tolerant and that's nice. Thank you very much. And if you have never been to the CyberLipid Center it's a great place. It's kind of clunky but has a huge amount of information on all alkaloids and plant extraction methods. The clunkiness is actually part of the appeal...
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endlessness
#4 Posted : 8/8/2017 4:37:33 PM

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mikeAtHome wrote:
Some of the extractions can go for 6 pulls or so (of solvent). The FASW tek is where I want to finish but I did like some of Cyb's STB thinking on the extractions. Didn't know if there was some incompatibility or not.


6 pulls of moderately selective solvent (like naphtha) is different than salting 6 times because DMT in salt form like fumarate is way more soluble in water than freebase DMT is in
naphtha. You can do CYB's extraction fine and after you have your freebase you can convert it to FASW by just making FASW and dissolving your freebase and evaporating (and then doing any of the clean ups to remove excess fumaric acid for example the one I linked in the other fumaric acid thread). Or even before you get to your freebase, when you have your DMT in your non-polar solvent, you can already salt it with FASW

mikeAtHome wrote:


Yeah, there's a thread, fairly recently posted 1)why can't you use lye 2) does NP solvent...


In that thread its a dry tek, where you only add minimal amount of water and you make a sludge with your plant material. I dont know why they said its not possible, I cant see any chemical reason behind it, it should work (but do note I haven't tried using NaOH in a dry tek myself so Im takling theoretically). Other cases where NaOH might not be appropriate is when using a cooking oil as a non-polar, since the NaOH will make it saponify. Either way this has nothing to do with the FASx part, which comes after you separate your non-polar from the basified material, so whatever base you used should be irrelevant in that sense.

Quote:

Again, good to hear. Doesn't seem to be a lot of worry about that here. You just hear things here and there like ph too hi/lo damages the alkaloid or pull at too low a ph and you start getting garbage, pull too high and you leave product behind etc. But it seems DMT pulls are tolerant and that's nice. Thank you very much. And if you have never been to the CyberLipid Center it's a great place. It's kind of clunky but has a huge amount of information on all alkaloids and plant extraction methods. The clunkiness is actually part of the appeal...


Yeah, DMT extractions are extremely forgiving. Just remember to not throw anything away before you are completely finished, that way if something goes unexpected, you can always come to the Nexus for help and tips and the DMT will be recovered from wherever it is Smile

Good luck!
 
mikeAtHome
#5 Posted : 8/11/2017 1:49:05 PM

The only God I can imagine is a God that I can't possibly imagine


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Thanks again endlessness,

No need to answer on this. I just wanted to post in case someone else came along and read this short thread....

I followed an "illuminated" link to an older thread in this thread's parent: nteresting discovery when salting with vinegar . Tt's not fumarate to acidify but the same principal applies. Any salt form looks to be very water soluble (Very Soluble implies a min of 1g/ml). Don't know if I mentioned earlier but meth salt is also VS and documented experience there shows 14gr can easily "fit" into 100ml on the first pull. This was with a 15 minute wait and where that 14g was 50% of the final yield. People who were doing water pulls on that substance (as opposed to those who used and acid gas into the solvent to force precipitation) came to realize a few important points:

1. The spice starts moving into the aqueous layer way in advance of the target ph where (the one where 99%+ solute eventually resides). No big surprise since that's what pKa is all about. But the more seasoned users would do their first pull a couple ph above their target and keep individual pulls separate during evap. In every case that first provided much cleaner product than the last pull (which was usually targeted at 1 ph below the pKa). Don't really know if that applies to DMT but plan to find out.

2. A clean water wash was done by everyone prior to addition of acid for the first pull. Hard shaking for 2 minute and waiting at least 10 minutes before separating and pitching the dirty water. The always made sure the ph of the wash water was high enough to insure it contained no solute. Your feeling is that's not really required for us. And I've only had a couple times where I felt I should increase ph just a tad before washing. Even then, I doubt it had more that 1% effect on final weight. The important thing was the wash. It did make a difference in removing any chemicals that had been added to the solvent (whatever was left of the base plus a small portion of undesired compounds that have been riding along with the targeted solute from the start). It may or may not help in our tek as well but it's really no bother so why not?

3. Pulls involved 2-3 minutes of shaking as hard as possible followed by a 10 to 15 minute wait prior to separation. Some folks shook, waiting a couple minute, shook again and then waited the 10-15 minutes. I don't know how much it helps but it can't hurt and doesn't require much effort.
So again, why not? Visually, the separation happens right away which makes it tempting to just go ahead with seperation. But what you can't see are the tiny amount of solvent compounds still fighting their way out of the aqueous layer. Nor can you see the few slowpoke solute compounds struggling to make that shift into the aqueous layer. This does probably make a difference and is why I included the above link. The overnight rest after lowering the ph lead to nearly 100% of the DMT coming across in that first pull. I'm not recommending an over night wait; just saying a wait between pulls is justified. A few would wait overnight prior to the 3rd and last pull. They did get a bit but never anything to brag about. If I recall correctly, the extractor who was expecting a full ounce overall, got just a little under 1g. And he may have been doing that last pull as the 4th not 3rd. The moral holds: most everything comes out on #1 and #2. Those of us going after roughly 1g probably won't see much on that 3rd, especially if the first 2 involved aggressive shaking and a reasonable wait before separation.

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