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screwed up fasi need help

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concombres

concombres

Rising Star
i extracted some spice w/ limonene & it looks like i added the fasi too fast.
There is a thin, dark yellow layer on the bottom of the jar.
I understand how to clean it up to some extent, but i'm not exactly sure how to proceed.
Should i give it a couple days to sit, separate the limo & base w/ sodium carbonate, then wash with dry ipa or something?
I'd like to turn the oily full spectrum into nice white freebase.
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This extraction is getting sloppy. Had a friend come over & try to help.
His solution was mixing water into the mixture of limo, oily product & fasi.
We're now left with limo & a clouded, yellow water layer.

The dmt should have been converted to fumarate salt already, making it soluble in water correct?
So now what we have should be a mixture of water, dmt fumarate, & isopropyl on the bottom since iso is miscible with water.

In order to save the extraction from further complications nothing else will be touched until we get help from someone more experienced.
 
Why not dissolve some more acid into water, extract into aq. layer, discard limonene, and start fresh?


Also you mentioned already that there was water in the mixture.. As it turns out, acid salts are soluble in water. (How about that) Next time, remove water with MgSO4. And perhaps post in the extraction help thread?

Also pointing out, there is a fasi subforum, why did you post this in A->B chem?
 
So just continue with fasw & cleanup from there?

I had the iso dried with mgsO4 at the start. I still have some sitting in a flask with dry mgsO4.

& i forgot about the fasi/a/w subsection.
Kind of had a brain fart there.
Hopefully a mod will come & move it soon. :lol:
 
I think drying dmk (acetone) would be your best bet. Extract your dmt using water, convert it to freebase, and crash it out using saturated acetone THAT YOU DRIED.

Remember MgSO4 needs to be heated to cleave the water from it. Keep everything anhydrous because your fumarate salts will migrate to the water.
 
So your alkaloids will be in the water now, together with IPA. Dont add base and extract now, because your water will contain some IPA.. So if you mix a base and a non-polar, part of the IPA will stay in the water holding the freebase, and part in the non-polar (which might screw freeze precipitation too etc).

Your best bet now is to separate that water (and do another water wash on the limo and put both pulls together), then evaporate the water completely (boiling/simmering temps are fine). So you will be left with impure fumarates, which you can mix with sodium carb and a bit of water to make a paste, let dry and break into powder, pull with IPA (or acetone) and salt with FASI/FASA, adding it slowly. This time it will probably be much more pure. Wait 3 days for full crystallization (and add more FASI/FASA to see if more cloudying occurs)


Regarding why this happened in the first place, I find it is a factor of three things (not sure which has more weight, if any): IPA/Acetone not being fully dry, adding FASI/FASA too fast, or very impure limonene/extraction

Either way next time be sure to add the FASI/FASA slowly and wait at least 3 days for crystallization of FASI/FASA (even if there's a yellow on the bottom, usually purer crystalls will grow on top of that and on the sides of the container). I've had extractions that were only finished crystallizing after a week.

By the way, this thread is relevant:


The pics link are not working anymore, I'll try to find those pics again and post, they were some very nice cleaned crystals.
 
1ce said:
I think drying dmk (acetone) would be your best bet. Extract your dmt using water, convert it to freebase, and crash it out using saturated acetone THAT YOU DRIED.

Remember MgSO4 needs to be heated to cleave the water from it. Keep everything anhydrous because your fumarate salts will migrate to the water.
Click to expand...

My mgsO4 was heated to remove water & the chunks broken up & added to 91% ipa in a flask with a glass stopper. I used quite a bit (75g before drying) of MgSO4 for ~500ml ipa & then filtered thru a funnel with a cotton plug.
i'm not sure of the dry ipa will absorb moisture from the air during filtration, but even if it does, it can't be much.

The limonene i'm pretty sure was pure as well endlessness. It's supposed to be 98.5% minimum purity & came directly from a large company that specializes in eco friendly terpenes. No hardware store orange oil.

I'll follow what endlessness said & go with acetone over ipa on your reccomendation following what endlessness explained ice.


Thanks for the help guys :)
 
Just to clarify, I mean, impure pulls, not impure limonene.. As in, maybe too warm, or for some reason your plant material had a lot of oils/impurity, or pulls were standing for too long, etc... Just a possibility, maybe not your case.

Let us know how it goes! Dont throw anything away until you are finished.
 
endlessness said:
Just to clarify, I mean, impure pulls, not impure limonene.. As in, maybe too warm, or for some reason your plant material had a lot of oils/impurity, or pulls were standing for too long, etc... Just a possibility, maybe not your case.

Let us know how it goes! Dont throw anything away until you are finished.
Click to expand...

That is more than likely part of the problem. I keep my jars in a heat bath for hours on end @ 150°f.
They get hot but never too hot to handle.
The limo stays declouded & any microscopic water bubbles separate quickly that way.

I have the first water/fumarates/ipa mix evapping in a dish ontop of a crockpot now.
The setting is on medium & with this particular crappy crockpot gets water to ~100°f but the plate sitting ontop & the sides of the pot only get slightly warm to the touch so o figure the heat is low enough not to effect the spice in the solution.
 
endlessness said:
That might be it.

So its a disadvantage in this sense, but on the other hand the heat might help your yield. It may happen what just happened, but now if you clean up it should all be fine :)

Good luck!
Click to expand...

Yeilds don't matter much in this extraction. My normal 2% would be nice.
But even only 100mg i'd be happy with.
This extraction was started as a learning experience to help move toward extracting with safer, less suspicious chemicals.
Ideally i'd like to learn the ins & outs of using limo first & move from there to using a different base.
Lime sounds nice, but i don't like the idea of a dry tek.
 
First pull from the limo yeilded a large amount of impure yellow waxy chunks/ powder weighing 5g

Edit:
Made a paste with the fumarates & 8g sodium carbonate, chopped up chunks, & worked a bit with razor blades to thicken up.
It's drying now.
 

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One other thing with attempting precipitating from limonene is that it seems limonene can hold enough water (possibly as a barely visible microemulsion) to screw things up. A drying step with anhydrous sodium carbonate powder prior to adding the FASwhatever seems to help a bit.

I was thinking to say "of course decant the limo off the carbonate", but as a what if, purely in the interests of science, one could try the FASI/FASA precipitation onto the settled carbonate, do a quick anhydrous solvent rinse after pouring off the limo, then it's ready for basing straight away just by adding water. If it's not worked the goodies will still be in the limonene (you have kept the limonene, havent you?? :D)

I think tinkering is all part of the fun! Good luck...
 
Ideally you would dry the limonene over MgSO4 or even calcium carbonate. One always practices drying EVERYTHING when moisture sensitivity is a concern.
 
Along with MgSO4 these are some other companions:

A dessicator and drierite (CaSO4/CoCl2). It'll change color to let you know the MgSO4 is saturated with water. The dessicator is used to provide an air tright moisture leaching environment for drying/storing.
 

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~60ml fasa added in small increments from a teaspoon over the course of the day.
Crystal clusters are forming nicely already & look to be only faintly discolored.
Some white powder precipped early on. Solvent was murky when initial fasa was added, some sodium carbonate and/or MgSO4 may have made it through the filter.

Crystals formed overnight & an additional 100ml fasa added slowly until no more clouding occured.
 
Crystals grown via fasa were scraped, washed 3x with dry acetone & weighed in @ 3.3g light yellow, dry powder.

A paste was made with sodium carbonate to convert to freebase.

Freebase was washed 3x in cold water thru cotton plug & funnel.
Retrieved with dry isopropyl alcohol & left to evaporate.

Iso yeilded 2g pale yellow powder.

2g redissolved in dry acetone & fasa added slowly
Clouding stopped around 75ml.

Within a couple hours a large cluster of fragile, clear crystals formed on the bottom of the flask surrounded by a crust of many small crystals that seem to be slowly connecting.
Solution will be left to crystallize for 1 week.

Crystals were dried, washed 3x with dry acetone, based with sodium carbonate, water washed 3x, & dry acetone was run through the filter to retrieve dmt.
Upon drying it looks as if some water from the cotton got into the acetone. Crystals formed strange patterns around areas where water remained after acetone evaporated.

Crystals were dried, scraped, & re-dissolved in 100°f naphtha, leaving behind some dark yellow/brown impurities. (minimal amount of naphtha was used. Maybe 30ml)

Warm naphtha was immediately poured into pyrex dish & stuck in the freezer.

Upon removing from freezer naphtha was still slightly cloudy with agitation. Poured into a shotglass & saved.
The resulting crystals formed an extremely fine, sparkling film on the tray weighing out to 0.5g when scraped. Very fine, fluffy, off white powder.

Remaining naphtha was placed back in freezer.

Yeilds were low but for a first run this was a fun process.
Plenty of places throughout where losses can be minimized & more dmt recovered.
Normal 2% yeilds or something close look to be possible.
 
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