FASE + FASW -> failed. please help.

[Kalitechnik]

So i tried my first FASing experiments. I had around 250ml of xylene from my extraction of 50g of MHRB powdered bark.
And i wanted to make fumarates. After reading many threads, i found some post where @Samvidbuho secribed how acetone is not the best for salting fumarates, and using ethanol (FASE) together with water (FASW) is way better.
Here is the post:

Solubility Studies 1: Salts & Salting Out - Guide to Enhanced Techniques

Hi All, I've started working on a series of solubility studies aimed at perfecting the art of crystallization. This part is based on a solubility study I did on fumaric acid, in solutions of water, acetone (undried and dried) and ethanol. I found that the solubility of fumaric acid in even...

forum.dmt-nexus.me

I tried to follow some of his description and mixed ethanol (25ml) with around 700mg of FA. I was adding very carefully at the begining with few drops after the drop, and it was looking like those small droplets where salting out, but later i add a little more and mre a bit faster and when i finished 20ml, i seen barely nothing (in the description of his method Samvidbuho, was writing that the whole process took him around 5 minutes).

later i tried to add FASW as he suggested. so i had prepared a 50-80 ml of water with around 2g of acid, and i started to add it a bit faster than before.
when the water finish and i did not see any precipitated crystals at the bettom i gave it a shake few times.
And still nothing falls on the bottom.

One thing i have noticed, that the xylene which was piss yellow, becoe quite watery, and the water became yellowish.

And now i am stucked, and i have no idea what i did wrong, and what should i do better, and how shall i proceed, and what can i do to recover my deems if possible.

Can you please help and explain, as i just lost my faith in FASing dmt fumarates from xylene, which was so promising.
Did anyone tried ethanol and water as it is described in the linked article?

 

[Kalitechnik]

So with my limited understanding i tried to backsalt it to recover my dmt. I added some hot water with citric acid and mixed thoroughly.
The xylene got quite clean i pipete it out, and now placed the flask in heatbath to let the rest of of xylene to evaporate.

And now comes a question, did i did good? I mean if a xylene can be backsalted? So now i will add lye solution and do the pet ether pulls?

 

[Varallo]

So you added ethanol, water, fumaric acid mixture to your xylene? Then after shaking it should form a watery layer with the dmt fumarate and excess fumaric acid.

You could dry this to get a, if you’re lucky, crystalline product that will be a mix of fumaric acid and dmt fumarate depending upon the respective quantities.

Now you have added more water to the xylene and citric acid, so now you have a mix of water ethanol acids and dmt salts. I think when you would extract this mix after basing the ethanol could cause problems.

 

[Kalitechnik]

So you added ethanol, water, fumaric acid mixture to your xylene? Then after shaking it should form a watery layer with the dmt fumarate and excess fumaric acid.

You could dry this to get a, if you’re lucky, crystalline product that will be a mix of fumaric acid and dmt fumarate depending upon the respective quantities.

Now you have added more water to the xylene and citric acid, so now you have a mix of water ethanol acids and dmt salts. I think when you would extract this mix after basing the ethanol could cause problems.

thats why i try to warm it to evaporate the rest of the solvents... and i think that ethanol layer was very thin and above the xylene.
i just want to get my freebase out of it.

my first try on precipitating fumarates failed... i dont knwo what i did wrong, but i got a bit scared of this...

can you advice on how to make a proper precipitation?

or maybe actually its better to just convert freebase to fumarate once we have our extraction done.

 

[Varallo]

first try on precipitating fumarates failed... i dont knwo what i did wrong, but i got a bit scared of this..

It failed because there’s water in the mix so there will be no precipitation

can you advice on how to make a proper precipitation?

Use the FASI or FASA method and make sure to dry all ingredients thoroughly before using them, so also your liquids

or maybe actually its better to just convert freebase to fumarate once we have our extraction done.

Sure just calculate the amount of fumaric acid and mix in some water ipa or acetone and dry. If an excess of acid was used clean the resulting powder with dry acetone.

 

[Kalitechnik]

It failed because there’s water in the mix so there will be no precipitation

i got confused a lot after reading the document mentioned at the begining. It is stated there that ethanol and water can be used, and actually no need for the drying acetone. have you read that document?

 

[Varallo]

No it’s not that it’s possible to form dmt fumarate with water in the mix but it just won’t be precipitating out. It will be in solution in the water, like you mentioned as salting out with your citric acid solution, it’s the same thing.

 

[Kalitechnik]

No it’s not that it’s possible to form dmt fumarate with water in the mix but it just won’t be precipitating out. It will be in solution in the water, like you mentioned as salting out with your citric acid solution, it’s the same thing.

how the hell this guy is doing it?
after reading his document i got so excited

have you ever tried FASE as in this document?
i wish the author would be around and give some explenations.

 

[Varallo]

how the hell this guy is doing it?
after reading his document i got so excited

have you ever tried FASE as in this document?
i wish the author would be around and give some explenations.
View attachment 99043

The key is in the description of the picture, “settling into aqueous layer”

Precipitation is used wrongly in this article, precipitation is commonly seen as the formation of crystalline material in a liquid, the description of the article is not correct.

 

[Transform]

The document has now been reformatted into a pdf, maybe this will at least make viewing easier for some people:

https://forum.dmt-nexus.me/attachments/a-comprehensive-guide-to-salting-salting-techniques-optimization-through-alternative-ap-pdf.99048/

Precipitation is used wrongly in this article, precipitation is commonly seen as the formation of crystalline material in a liquid, the description of the article is not correct.

I get the impression that after an initial addition of FASW, the FASE does lead to precipitation of solid material from the xylene, but this material is promptly dissolved by the previously-added aqueous phase for ease of collection via pipetting or with a separatory funnel. All the crystal pics are, presumably, the result of evaporating the resulting aquo-ethanolic solution of DMT fumarate. Presumably, the use of FASE as a second step in precipitating fumarate from xylene still allows a reasonable degree of titration to minimise the excess of fumaric acid in the product.

 

[Kalitechnik]

It would be very nice to see someone taking the process from the article and showing result with more explanations. I got lost after reading it. Seemed so promising and easy, but looks like i did not understood it.

1. I have also soething else on my mind. As i was reading FASAing our fumarates right from xylene pulls will be a bit dificult to collect, also it would rather need cleaning.

2. I wanted to use FASAing from xylene to skip the evaporation stage of xylene.

3. But if i can backsalt my xylene pulls, i might be skipping the evaporation stage too, as well making a first step into cleaning my spice.

4. When later pulled with pet-ether i can freeze precip, and get a freebase easilly.

5. Saving xylene and saving pet-ether for the next pulls will be possible.

6. And if i want to make fumarate (which mainly i would like to do for oral consumption) i can do the conversion tek, which should be rather easier.

Is my thinking correct?

 

[Varallo]

It would be very nice to see someone taking the process from the article and showing result with more explanations.

Might that person be you?

Seemed so promising and easy, but looks like i did not understood it.

You’re almost there.

Read the comments here and in your other thread carefully and you should be able to answer your questions, because your thinking IS correct.

 

[Kalitechnik]

Might that person be you?

I tried. And failed, or maybe not failed actually but succeded with gaining some knowledge and experience.

You’re almost there.

I do hope so. I have a feeling that i am starting to understand a bit...

Read the comments here and in your other thread carefully and you should be able to answer your questions, because your thinking IS correct.

I re-read comments few times. English is not my best language especially with technical knowledge but hopefully i got it.
Let me conclude if i understood it correctly.

My experiment fith FASE and FASW "failed" because i was expecting to see the precipitated crystals in the aquatious layer, but that is not rather possible since fumarates are soluble in water. So possibly i got my freebase from xylene converted to fumarates, but to get the crystals, i should collect the aquacious layer and evaporate it?

 

[Varallo]

My experiment fith FASE and FASW "failed" because i was expecting to see the precipitated crystals in the aquatious layer, but that is not rather possible since fumarates are soluble in water. So possibly i got my freebase from xylene converted to fumarates, but to get the crystals, i should collect the aquacious layer and evaporate it?

Spot on !

Great to see this!

 

[Transform]

English is not my best language especially with technical knowledge but hopefully i got it.

Hey, you're doing pretty well - I'd struggle with following technical instructions in Polish for sure, but least there are plenty of internet tools for helping understand foreign languages nowadays. I also suspect that having a good grounding in technical subjects in your native tongue would help a lot. If I wanted to learn car mechanics I probably wouldn't pick up a book written in Korean, for example, so I'd definitely recommend looking for additional educational materials in your principal language.

 

[Kalitechnik]

Ok. So to sum it up. At this moment my understanding is like this.
1. If i want to get fumarates i will do the simple conversion from freebase to fumarates.
2. Salting out fumarates from xylene, at this moment i can skip, since i can easilly do backsalting with other acids, as a way of skipping evaporation of xylene. As this was actually my main reason to do fase + fasw.

Thanx for guidance guys.

At the end i got 750mg from backsalting , basifying and pulling with pet-ether.