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Cleaning up dirty fumarates

Migrated topic.
Anyone have the general consensus on this technique?

Of course one person may not represent the general, but I have yet to see much update on this.

Seems like one person did this very successfully...
 
I have done a lot of experimenting recently with cleaning fumarates. The standard freebase cleaning procedure of cleaning by dissolving in warm naphtha didn't work too good for me, and I can't get heptane. However, the novel technique discovered by olderROM using cotton balls looks promising, gotta try this sometime. Novel reX procedure?

So I tried both methods described in this tread and these are my thoughts:

Method 1 by endlessness: rebasify in sodium carbonate paste, then dry and pull with acetone

- This cleanup didn’t work well for me because I had to dry the carbonate/DMT paste for more than a week (I didn’t apply heat). This caused more my DMT to come out more yellow after the cleanup than before, due to oxidation in the basified paste.
- In my experience it works better to dissolve the fumarates in water, add base, pull with naphtha and precipitate the freebase in the freezer. Then dissolve the freebase in acetone/IPA and add fumaric acid. So a re-A/B. This way the freebase DMT is not exposed to base and oxygen for a long time.

Method 2 by Narmz: dissolve DMT fumarate in boiling IPA, then put in freezer to precipitate

- Narmz’ IPA cleanup works good. However, it had to be performed multiple times to get a white product and uses up quite some IPA. I used 100 ml of boiling IPA per 3 grams of DMT, 3,5g would not completely dissolve so solubility is somewhere in between.
- Something interesting I noticed was that my fumarates came out whiter if I put the hot IPA in the freezer right away. When I first let it cool to room temperature the crystals that formed were bigger, but more impure.
- No DMT gets lost with this method. It is in the stable fumarate form the whole time. Also, when I evapped my leftover IPA after precipitation no crystals formed, only a tiny bit of yellow stuff remained.

Method 3: fast precip from IPA

- A good method for purifying is to dissolve freebase in IPA, add straight fumaric acid (no FASI!), and stir good. This causes an instant precipitation of small but pure DMT fumarate crystals. The DMT fumarate formed is contaminated with fumaric acid but this can easily be removed by dissolving the DMT fumarate in water.
- This method didn't work with acetone. With acetone bigger, impure fumarate crystals formed really fast. Maybe this is because my acetone wasn't anhydrous, this needs to be checked.

I dissolved some pretty yellow DMT and look at the result after employing this method:



If you want to purify DMT, it seems you should always shoot for small crystals. Either by cooling a solution down rapidly or by adding fumaric acid fast. Big crystals trap more impurities.

This is all based on just a few experiments, I would love for someone else to try this out and report his/her findings!
Also, why isn't there a reX subforum? The topics about this are numerous and scattered. There is of course the wiki, but since there is no consensus on what the best method is a subforum would be in place in my opinion. I believe I've heard this issue addressed before, but I forgot what the reason against it was.
 
hey..

i tried it this way.. had a 7 gramm of pretty dirty fumarates from d-limo pull.
used 13 gr of sodium carbonate, made a mix an watered it till it got wet enough to drip from one side to the other…
dried that, till completely dry, and permantently used a morser to break any chunks, so had some nice powder.. put in glass and added twice as much of aceton than i had material..
Settlement of Carbonate went pretty good in first pull. 8see pic, right is first pull..
then i filled again same amount of Aceton to the powdery-mixture which wnet white, left pic, and is not settling anymore.. been like this for about 10 hours now… tried heatbath and tried fridge.. bith without any sufficient outcome…:
 

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Forgive me if this is a stupid question but; did you remember to freebase the second pull as you did first?😁
 
Luuk said;"If you want to purify DMT, it seems you should always shoot for small crystals. Either by cooling a solution down rapidly or by adding fumaric acid fast. Big crystals trap more impurities."

This seems true and it bugs me because I reason that bigger crystals equal larger concentrations of pure spice with less surface area. Instead it seems that solvent gets trapped in the matrix of the crystal.

But not all crytals are created equal!

Here are two examples of recrystalization
1rgd.jpg
zkuy.jpg

in the first one we see reX from Naphtha in a wide open baking dish over a slow period of time. They are very pure!

in the second image we have reX from anhydrous acetone in a small bowl. this evaporated rather quickly and formed crystals with in thirty hours.
Close inspection reveils contamination in the matrix of these crystals.
mt4z.jpg
u5q5.jpg
wyyg.jpg

Or so I'm told by the person who did this and sent me these pictures:grin:
 
YTXian said:
Forgive me if this is a stupid question but; did you remember to freebase the second pull as you did first?😁
Click to expand...
As he used the Paste-Conversion from Fumarate mixed with sodium Carb, he had a freebased dried out paste in the end.. so then he wanted to pull with Aceton, so he filled the mixed fumarate high as line indicates on pic, and then filled it up with an amount twice as much as mixture… then let settle, and decatnted 1st pull, which is the right one.. all in all it tool 2 hrs incl settlement, and seperation,,
He then filled fresh Aceton to the leftovers of the fumarate sodium powder to fill that up again for a 2nd pull, mixed that, and what you see on photo is the situation after 12 hrs.. so he decided to use just Pull 1 for the FASA and started doing it, but very slowly.. just few drops every now and then he passes along… now after 30 hrs also the second pull has settled somehow, although still bit milky, but much more difference to the one yesterday.. he decanted that as well, and started in a different bowl a FASA for 2nd Pull,, which alos works quite good.. but really only dropwise and half hour later next 5-6 drops, etc…. 1st pull is full of chrystals already, but permanently still clouding out using some drops FASA.. so still adding ,,,
Pull 2 also builds up chrystals pretty fast-- and the same willbe done with Pull 3 in 2 dayys then… just to make sure i have everything out of the product…

but still not understand what you mean to freebase pull 2???
pix follow soon..

cheers
 
thats right… but as product gas been freebased in paste technique, i see no advantage of using more base in 1st container, as i am trying to wash the fumarate alkaloids out of the solution..
or do you rebase after every pull you do? no sense IMO….
 
Uh, no and nevermind. Sounds like your problem resolved itself anyway. Good work man! cheers!
 
Hupecat said:
YTXian said:
Forgive me if this is a stupid question but; did you remember to freebase the second pull as you did first?😁
Click to expand...
As he used the Paste-Conversion from Fumarate mixed with sodium Carb, he had a freebased dried out paste in the end.. so then he wanted to pull with Aceton, so he filled the mixed fumarate high as line indicates on pic, and then filled it up with an amount twice as much as mixture… then let settle, and decatnted 1st pull, which is the right one.. all in all it tool 2 hrs incl settlement, and seperation,,
He then filled fresh Aceton to the leftovers of the fumarate sodium powder to fill that up again for a 2nd pull, mixed that, and what you see on photo is the situation after 12 hrs.. so he decided to use just Pull 1 for the FASA and started doing it, but very slowly.. just few drops every now and then he passes along… now after 30 hrs also the second pull has settled somehow, although still bit milky, but much more difference to the one yesterday.. he decanted that as well, and started in a different bowl a FASA for 2nd Pull,, which alos works quite good.. but really only dropwise and half hour later next 5-6 drops, etc…. 1st pull is full of chrystals already, but permanently still clouding out using some drops FASA.. so still adding ,,,
Pull 2 also builds up chrystals pretty fast-- and the same willbe done with Pull 3 in 2 dayys then… just to make sure i have everything out of the product…

but still not understand what you mean to freebase pull 2???
pix follow soon..

cheers
Click to expand...

so here are, even when little unsharp due to crap camera some Photos of the 3 Pulls SWIM did.
 

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Endlessness's sodium carb dry tek didn't work for me and I used 3 times as much soda ash as recomended.

I poured in over a gram of dmt-fumarate in to sodium carb solution and watched it fizzle away, dried it overnight and pulled 4 times with acetone, evapped the acetone and was left with not much but a little bit of goo.

I placed all the remaining still dried sodium carb/dmt-fumarate into a container with a little lye and naphtha became cloudy when extracted.

I am voting for IPA methods for time and effort.
 
Narmz's boiling IPA wash didn't work for me either...

I used 100ml of 100% IPA, and boiled it and then dissolved over 1 gram of dmt-fumarate, it picked up most of the brown/tan oils and about 500mg of spice. It was then freezed overnight at -14c. I poured it on a plate and only half had semi-precipitated, then other half was evapped and scraped.
 
From now on I will only do naphtha recrystalizations before converting to fumarate. If I have to convert some goo to fumarate, I will then re-basify with lye and pull with naphtha and re-convert.
 
Hi everybody.... i searched in the forum but i did not find any answer unless "chop it to release any traces of solvent"

i have some light yellow fumarates that i would like to convert into fb for smoalking.
i collected them, dryed on a plate then chopped and dried more in the oven at 60 celsius for 4 hours then chopped again for half an hour or so and 4 more hours of 60 degrees in oven again.
then i left them under a black pot in the sun for 4 days but if i get them and chop again i can still smell some xylene-acetone smell and i have some concerns about converting them into fb due to fb solubility in nps.

i assume that to be completely sure that no NPS will remain in the spice a vacuum evaporation should be performed but i can't pay for that.

what can be a possible way to go ahead? thaaanks!!

P.S i have no access to clean IPA or EtOH and i just run out of fumaric acid.
 
U gO said:
Hi everybody.... i searched in the forum but i did not find any answer unless "chop it to release any traces of solvent"

i have some light yellow fumarates that i would like to convert into fb for smoalking.
i collected them, dryed on a plate then chopped and dried more in the oven at 60 celsius for 4 hours then chopped again for half an hour or so and 4 more hours of 60 degrees in oven again.
then i left them under a black pot in the sun for 4 days but if i get them and chop again i can still smell some xylene-acetone smell and i have some concerns about converting them into fb due to fb solubility in nps.

i assume that to be completely sure that no NPS will remain in the spice a vacuum evaporation should be performed but i can't pay for that.

what can be a possible way to go ahead? thaaanks!!

P.S i have no access to clean IPA or EtOH and i just run out of fumaric acid.
Click to expand...

Do you have mortar and pestle? You can powder your product and leave in oven on low setting.

Maybe storing the powder in a sealed box with some dessicant will also help removing traces of solvent.

Vacuum drying is necessary when you need to avoid heating the product, but DMT fumarate is stable enough to withstand that, so vacuum is not necessary. I would still go for a closed box with dessicant to avoid getting moisture to your fumarate after baking.

I store my DMT fumarate in a Petri dish sealed with parafilm and with a small silica gel packet inside.
 
the problem is when i want to convert to freebase that even the littlest NPS trace will come out as it happened when i converted a small part of this fumarates that they don't smell solvent anymore but when redissolved in water and based with sodium carbonate solution the NPS cames out.
 
I recently had some fumarate that refused to stay solid and kept turning into a sticky goo...even the freebase was still an oil after trying the sodium carbonate saturated water technique. I hit it directly with some room temp. FASI and it clouded upon contact. I added excess and stirred it up real well and then stuck it in the freezer. After some hours I retrieved it with a snowy precipitate at the bottom. I let it warm up to room temp and then filtered with regular paper (from my printer) since the particulate was so fine, washing it at the end with 100mL or so of room temp dry IPA. From ~1g of freebase oil (1.75g jim jam fumarate goo to start with), I was left with ~600mg of fine fumarate powder that smells mildly of only DMT...no oranges or IPA at all.
 

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