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Cleaning up dirty fumarates Options
 
endlessness
#1 Posted : 12/30/2011 9:32:58 PM

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So I've been doing some fumarate clean up tests. Here are the pictures:

Before (hard yellow chunks from FASI):


After:





So the pictures above show how well it cleans, with very little yield loss (I think from around 4.4g of yellow stuff I ended with 3.7g white/transparent crystals). The process is simple sodium carb paste and FASA. Here's the detailed instructions:

1- have the dry fumarates and mix them with sodium carb. I added excess sodium carb, maybe twice as much as fumarates, overboard but its better too much than too little.

2- Add some warm water to make a paste, and mix well. It can be a bit more water than paste, like runny, but no need to be a solution.

3- Dry the paste. I used a hair drier to make it faster. Remember its freebase, so use heat less than 100 degrees celcius. Once it's getting drier, it forms some chunks, break them up to finish drying.

4- Put the dried paste/powder in a glass and pull 3 times with acetone. I added around twice the volume of the dried paste in acetone for each pull (last pull a bit less).

5- Make a FASA solution (just add excess fumaric acid to acetone, shake shake, filter)

6- Add FASA to the dissolved DMT freebases from the 3 paste pulls. I added around the same volume of FASA than there was of acetone with DMT, but probably less is necessary. Too much is not a problem since excess fumaric acid does not precipitate.

7- Wait a few hours, decant/filter/let your fumarates air dry.


This could potentially also be done with IPA, maybe even with ethanol, instead of acetone, but Im not sure how the other solvents will affect crystallization (might be less pure, or more, or different crystal shapes, or same same...)
 

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joedirt
#2 Posted : 12/30/2011 9:52:38 PM

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Nice! Very nice!

Next time I find myself thinking of extracting I'm going the fumurate route. I've discovered I much prefer oral to vapor.

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endlessness
#3 Posted : 12/30/2011 11:11:55 PM

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Cool joe! Indeed check it out! I would like to try this again with some very dirty fumarates from FASW or similar (last time I had to re-a/b because washes or acetone re-x werent effective, but I had not tried this paste and FASA method).

And yeah the oral route has a lot of advantages.. I usually go for it too.
 
oldtripper
#4 Posted : 1/3/2012 4:55:17 AM
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beautiful endlessness! I must say I am confused as to the middle steps and the "pulling". if you have a solid chunk of spice and acetone or FASA, i guess i am lost as to what you are doing by "pulling" as there wouldnt be 2 layers correct? Are you dousing the acetone then sucking it up in something then transfering to new glass leaving any soda on the botton of first glass? That is such a work of art I really want to understand what you are doingWink
 
endlessness
#5 Posted : 1/3/2012 8:56:51 AM

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By pulling, I meant when you make a paste with the sodium carbonate.. You will have a solid chunk of spice+sodium carbonate, and this is where you want to add a quantity of acetone to it and separate, or "pull", because the acetone doesnt dissolve the sodium carbonate excess (or the sodium fumarate salts which are formed from the reaction of fumaric acid ions and sodium carbonate), so it will only dissolve the freebase spice.

Does this make sense?
 
oldtripper
#6 Posted : 1/3/2012 10:33:46 AM
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Yes that clears it up well, thanks! Now I got the mental picture finished. So, to get it back to smoking material you just add carbonate again? What confused me on the dry limtek was that the spice/vinigar water(acid) when dried can be turned to base by heat...still acid i would think..heat is NOT a base. I know thats a diiferent thread but using that as example why i am getting detailed on this. You seem to be well grounded in this, good mentor materialWink
 
endlessness
#7 Posted : 1/3/2012 10:45:39 AM

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Hey Smile

Yeah to get it back to smoking material, redissolve fumarates in water and add saturated sodium carb solution. Check this out for more detailed instructions (I much preffer type 1, slow crystallization method)

As for the acetate to freebase conversion, you are right that heat is not a base and that seems confusing. The theory behind it is that the bond of the acetic acid ion to the dmt molecule is weak and that acetic acid evaporates easily, so the heat is supposed to evaporate the acetic acid, even the one bonded to the molecule, leaving dmt freebase. To be honest though, im not sure it works that well, at least in my experience even with extended drying/heating it still had a somehow vinegary-smell. I think some people doing this conversion might be smoking a bit of acetates too, which might not be so bad but on the long run it might also be more harsh on the lungs (amor fati seems to agree with me and he was testing extensively this method). When playing with acetates I preffer doing the sodium carb acetate paste conversion as written in BLAB tek. . I already tried crystallizing acetates like the fumarate methods and it didnt work with sodium carb, with lye it worked for some people but I also had it not work before, so its safer to do the paste and pull method.
 
Purges
#8 Posted : 1/3/2012 6:44:49 PM

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Thank you for this, performing it now, added too much water to the 'paste' so its taking AGES to dry out with the hairdryer - add little amounts of water until the lot is dissolved, don't just dump water in!!!
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Purges
#9 Posted : 1/15/2012 10:53:51 AM

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So I did this with IPA - added 1.727g of JimJam the the sodium carb paste. Pulled 5x, added FASI and ended up with 50mg white powder?! 50mg?! Crying or very sad

Luckily I have saved the left over sodium carb, but SRSly what have I done wrong?! Think I'm going to try pulling it with Acetone this time and see if I can salvage some of my spice...


Any suggestions besides this ^^^?
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Purges
#10 Posted : 1/15/2012 12:14:30 PM

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I can only conclude that IPA must be a crap solvent for this part of the extraction...
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narmz
#11 Posted : 1/15/2012 1:52:54 PM

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IPA is quite possibly the best solvent to use for cleaning DMT Fumarate. DMT fumarate is fully soluble in boiling hot 99% IPA. Dissolving the fumarate in hot IPA and then allowing it to cool/freeze precip renders some of the cleanest DMT fumarate you will have ever encountered. The oils/contaminants stay dissolved in the IPA, while the fumarates precip out cleanly. Usually one cleaning is all that is needed but it can be repeated.

Here is a link to a quick step-by-step posted on the nook: Cleaning DMT Fumarate
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Purges
#12 Posted : 1/15/2012 2:22:37 PM

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The link doesn't work... Thanks for the info though, I have added moar FASI to the leftover IPA from the above procedura and iit seems to be precipping! Will bung it in the freezer and see how that goes. Thank you.
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narmz
#13 Posted : 1/15/2012 3:38:15 PM

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you must be registered at the nook to view that subforum - just register, login, and click on the link again
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xibalbaNOW
#14 Posted : 1/24/2012 12:59:43 PM

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I'm going to be cheeky and ask if someone can repost the steps from that IPA tek linked above? I'm very choosy with the forums I sign up to...

x
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narmz
#15 Posted : 1/24/2012 4:28:55 PM

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Here is a quick run-down of cleaning DMT fumarate of excess fumaric acid and plant oils.

1. Dissolve your DMT fumarate in boiling Hot 99% IPA.
2. Filter solution with cotton (especially if there remains a small amount of undissolved solids)
3. Place solution in Freezer over night.
4. Decant IPA and dry your fumarates.


First Image: Before Cleaning
Second Image: After Dissolving in Hot IPA and precipitating, the top Jar is the decanted IPA, the bottom Jar is the remaining fumarates.
Third Image: End Result
narmz attached the following image(s):
small1.JPG (476kb) downloaded 2,848 time(s).
small2.JPG (473kb) downloaded 2,839 time(s).
small3.JPG (426kb) downloaded 2,843 time(s).
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endlessness
#16 Posted : 1/24/2012 4:32:59 PM

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Narmz, how much IPA per gram of DMT fumarate, more or less? How did you heat the IPA?
 
narmz
#17 Posted : 1/24/2012 4:43:26 PM

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I think that jar was about 250ml of IPA there - and the dissolved fumarates was about 2 grams I believe, the end result was about 1.77 grams. Use caution when heating IPA, a ring stand was used to suspend the IPA with the dissolved fumarates within a pot of boiling water without letting the jar touch the pot at any point in time (suspended/heated in the water -- typical double boiler setup) - continuous stirring was employed.
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jamie
#18 Posted : 1/24/2012 5:13:45 PM

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I am going to try this with my fumerates and see if they make me feel less gross when I eat them once they are cleaned up. I can really taste the fumaric acid in them right now and it bothers my stomache to eat them.
 
Purges
#19 Posted : 1/24/2012 5:22:25 PM

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narmz wrote:
I think that jar was about 250ml of IPA there - and the dissolved fumarates was about 2 grams I believe, the end result was about 1.77 grams. Use caution when heating IPA, a ring stand was used to suspend the IPA with the dissolved fumarates within a pot of boiling water without letting the jar touch the pot at any point in time (suspended/heated in the water -- typical double boiler setup) - continuous stirring was employed.


I tried this today on 1g of fumarates and managed to spill the IPA / Fumarate solution in the pan of boiling water! D'oh! Its going to be an effort to salvage Sad
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YTXian
#20 Posted : 2/3/2012 9:48:23 PM

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I'm thinking of trying this on some chali-fumarates...then maybe the IPA boil Narmz posted...Anybody body have some input they want to add before I do this (in the innovative spirit of exploration and development we share on this nexus)?

Perhaps I should do the IPA clean first and then try the soda paste/FASA-A/B conversion cleaning second...

Ultimately my goal is to yeild solid freebase crystals from Chaliponga without tomany toxic solvents. Fumerate was made by extracting Chaliponga/hydrated lime 4-1 ratio and percipitated with FASI (though the first pull was percipitated with FASA before I noticed and then looked up and learned from the wiki that FASA doesn't work to good with D-limo)...

I'll post pictures and results.

Anyone? Got till tonight before I start.
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