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FASA: Slow addition vs. fast addition Options
 
Brennendes Wasser
#1 Posted : 6/19/2023 10:39:25 PM

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When doing any kind of procedure that involves FASA it is always mentioned to add the Fumaric Acid saturated Acetone slowly to avoid creation of Mono-DMT fumarate. Fumaric acid is a di-valent acid so it can bind with 2 carboxylic groups to a respective base, therefore binding 2x DMT with only 1x Acid molecule.

The theory is when FASA is added too fast, it might create a local excess of Fumaric Acid which is prone to only bind 1 DMT molecule and thus may create a salt which has a non-predictable amount of Fumaric acid (= unknown mix of mono- / di-valent ion pairs) and thus potency determination is not easy anymore.

So even though that is quite logical, I think there was never some data to look exactly into what happens if you compare both modes of mixing. It may be that a pretty fast addition will instantly precipitate 1x DMT + 1x Fumaric Acid = Mono-valent salt and thus create the 'unwanted ratio' in high quantities. Then afterwards this might not be able to react anymore with the remaining DMT in solution (like a 2-phase process) which is true for the CIELO TEK where you will only get Monomescaline Citrate instead of forming the theoretical maximum of 3x Mescaline + 1x Citric Acid over time. But still it does not necessarily be the same for all alkaloids, so maybe it might *collect* the remaining DMT in solution over time? Or maybe the crystal formation is rather slow and AFTER the fast addition but BEFORE actual crystal formation the reaction of all available carboxylic acid groups might still complete?


Here is an easy experiment to find out:

1,05 EQ DMT (1 mg / 10 ml Aceton) + 0,5 EQ Fumaric Acid (1 mg / 100 ml Aceton) is prepared.

Case 1: Normal FASA step = always excess DMT

Slow addition of FASA into DMT-Acetone-Mix while stirring


To provoke formation of possible Mono-valent salt I went to the extreme and made

Case 2: Reverse FASA step = always excess Fumaric Acid

Slow addition of DMT-Acetone-Mix into FASA while stirring



Now just by optical judging the first case obviously looked normal, just very fine white powder, not crystals at all but just extreme fine powder. I think with "normal FASA Methods" you can only create true crystalline DMT-Fumarate when recrystallizing in Ethanol.

For case 2 it went different: When clouds started to vanish actual crystals formed. Interestingly they were even yellow and then some pretty white crystals grew on top, but was less than 10 % of total material for sure.


Now a NMR analysis was done and the ratio of the Di-Methyl-Peak was compared to the Fumaric Acid signal.

Case 1:


= The Fumaric Acid Signal is at 0,64

Case 2:


= The Fumaric Acid Signal is at 0,78

The signal increase is roughly 22 %. In theory when comparing a Mono-Valent Salt (1:1) with a Di-Valent salt (1:2) the increase would be at a maximum of 100 %.

Sadly the absolute values retrieved here can not say anything about the actual salt formation, like giving a X:Y number between both. Reason is that only Protons (1H) will give a signal in 1H-NMR and therefore to not eclipse these signals with the obligate solvent it is mandatory to use deuterated solvents with Deuterium (2H). But protons that are highly interchangable can exchange with deterium from the solvent, if they are also interchangable. Both is true for sp2-C-H bonds = double bonds (still not to a high degree) and especially for water (which was used as a solvent here). So to indeed tell if Case 1 was mostly Di-valent salt and then Case 2 was *just 22 % off from the ideal state* I would need to repeat in another solvent, only DMSO would be possible for that.

Maybe will repeat in future, but anyways this shows that just from that raw data the difference is not too strong. But regarding the colour and morphology there is quite a difference, so staying cautious with a slow addition is obviously the best way.
But for people who overshot it, then there is probably no need to repeat the step, as this neutralization seems fast enough to still form mostly Di-valent ion pairs.
 

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Hailstorm
#2 Posted : 6/20/2023 5:50:11 AM

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The usual case against fast crystallization is that crystals are more likely to form "around" impurities, trapping them.

Since "slow" and "fast" are imprecise terms, I now prefer a fast crystallization (with stirring) followed by slow recrystallization of the resulting precipitate. Normally you want to recrystallize your products anyway.
 
famine
#3 Posted : 6/21/2023 9:31:18 AM

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My cat purifies DMT by vacuum distillation, dissolves it in acetone and adds straight fumaric acid until ph <7. I wonder the data of this.
 
Loveall
#4 Posted : 6/21/2023 12:29:42 PM

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famine wrote:
My cat purifies DMT by vacuum distillation, dissolves it in acetone and adds straight fumaric acid until ph <7. I wonder the data of this.


Have you measured the freebase weight and resulting salt weight?

Side note: We have indications that the salt form affects e-juice solubility.
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famine
#5 Posted : 6/21/2023 2:43:03 PM

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Loveall wrote:
famine wrote:
My cat purifies DMT by vacuum distillation, dissolves it in acetone and adds straight fumaric acid until ph <7. I wonder the data of this.


Have you measured the freebase weight and resulting salt weight?

Side note: We have indications that the salt form affects e-juice solubility.

I have ran a conversion this morning to see this. Still drying but at the moment it looks to be more the monosalt. Will update this in a few hours.

Edit: Yes I got around 30% increase. Monosalt
 
 
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