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Fumarate -> FB conversion: Need Help

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oldsoul

oldsoul

Rising Star
I think my conversion using "Type 1 - Slow Crystallization Method" may have gone south, looking for any advice here on how to proceed next.

1. The dissolved fumarates created dark yellow translucent water (not clear, as in tek pics)

2. First problem: slight oily sheen on top, is that normal?
3. Possibly the fumarates weren't completly dry, and this is from d-limo traces?

4. Second problem: when creating saturated sodium carb solution
5. First I followed BLAB tek which says 7g sodium carbonate/100ml to create saturated solution.
6. After adding the entire 100ml and still seeing clouding, I suspected a problem
7. Then I looked at the conversion tek, which says differently up to 40g of sodium carb per 100ml for saturated solution
8. So I created another 100ml more saturated solution & started to add that.
9. I added quite a bit of this and still saw clouding, however it was very late so I put in fridge
10. In the morning sodium carb was crystallized in the small jar I was adding from
11. I removed from fridge and added more drops, still saw further clouding happening

12. Third problem: At this point I noticed orange film along entire sides and bottom of conversion vessel (what is this?)
13. This appeared as the pattern of wiping glass with a wet rag (small splotches everywhere)

At this point I stopped to create this post, because in the teks it says only a fraction of the saturated sodium carb solution would be needed, however I have now added almost 150ml.

A. Should I remove from fridge and continuing adding saturated sodium carb solution until no further clouding?
B. Or does this orange film on sides of the vessel and slightly oily sheen on top signify something serious gone wrong?
C. If this has gone wrong, can I do 3x pulls of d-limo on this solution and end up where I can add FASI & re-precipitate fumarates and start over from that point?

Thanks!!!!
 
After a couple days in the fridge... this is what I'm seeing.

Orange film has increased and formed bigger globules, some floating as well.

The liquid has gone mostly clear. I opened the container and tipped it to the side, and saw a quantity of large, transparent crystals (I assume this is excess sodium carbonate?)

The liquid *smells* highly like spice... I'm so close, I can smell it!

I'm guessing I need to backtrack somehow and start over... any tip or suggestion how to proceed would be highly appreciated :love:

Peace
 

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Were your starting fumarates yellow to begin with?

If there are impurities in solution they will often prevent freebases from preciping. Would recommend making the solution acidic again to pH 4-5 and then try defatting off the yellow impurities with naptha washes. It could be freebased again with h2o/saturated sodium carb, but might run into trouble with all those ions floating around and the large volume. Would recommend basing that acidic soln with some lye and pulling with naptha then freeze precip/evap.
 
Hi Kash! Yes, the fumarates were somewhat yello/orange, there are pics in this thread

Naphtha isn't available in my location, but I'm also very into the idea of a food-grade extraction without using petrochemicals.

I think I could just pull with d-limo then precip the fumarates again, clean them with sodium carb/IPA, then reattempt the free base conversion, but I don't know if d-limo would pick up the sodium carbonate too, there's like 15g of big crystal chunks of it in this water.

Thanks dude:grin:
 
What acids do you have available?

Are you sure you cannot find naptha, or any other clean solvent for that matter in a hardware store? Not sure how well freebase would precip from d-limo hmm. Too bad you have to use d-limo also, quite expensive.

Well then acidify it, wash it with 50-100ml d-limo a few times. You can try risking a freebase precipitation again at this point if you want or....

Basify solution with a little lye, pull it a few times into d-limo. Then you can mix up a 100ml acidic water solution and then pull the spice/d-limo. Mix a saturated 50ml sodium carb solution with the 100ml h2o/spice and should be good.:thumb_up: Gl
 
Hi Kash,

All I can get is 133ml bottles of Ronsonol for $5. Pure naphtha and acetone are banned by my good state of California. At these prices the ronsonol is about 4x more expensive per mL than d-limo

As far as acids, I have acetic (white vinegar)

So what do I do with the clear crystal chunks (excess sodium carb?) and the orange globules (is that spice??)? Just bust them all up, gather everything, and mix everything together real good before acidifying again?

I will recap your recommendation as I understand it, let me know if I've got what you're saying:
1. Acidify to convert the dmt-freebase and dmt-fumarate back to dmt-acetate
2. Pull with NPS (naphtha or d-limo) to remove plant fats proteins and other impurities
3. Basify acid solution to create freebase dmt, then pull with d-limo
4. You lost me here, with "Then you can mix up a 100ml acidic water solution and then pull the spice/d-limo."

Wouldn't that be the point where I add FASI & precip fumarates again? Can you explain a bit more? Before proceeding I'd like to understand exactly what is going on rather than following blindly

THANKS!!!!!:thumb_up:
 
Yup you got it right. You can FASI or do an acidic water pull of the d-limo, though SWIM has never FASI'd d-limo. If it worked last time it will work again.
 
I'd pull it all with limonene again instead, and FASI again.. Then I'd dry mix the FASI with sodium carbonate and add small amount of water just to make a paste, let it dry with hair dryer or fan, pull with IPA and FASI the IPA, and then this should be purer fumarates, which then I'd proceed to do the conversion and it should work much better because the fumarates will be cleaner.

I will check the sodium carbonate amounts to correct either BLAB tek or the conversion and will let you know.

doing as kash said to acidify and defat should work too but I find it to be a more wasteful process.

Whatever feels right for you, just remember to not throw anything away till youre finished, and if something goes wrong it can be recovered again :)
 
If its not alot of liquid, i'd evaporate it (dont put it on the stove, or out in the sun, but a dry, dark, warmish, spot with a small fan blowing across the dish.

then pull with dry ipa, and evap again to get just the freebase oil w/out the sodium carbonate. Then dissolve it in minimal fumaric acid & distilled water, filter and evap. Wash with a small amount of NP, or a completely dry IPA or acetone.

Base it again with either sodium carbonate or lime, using the 69ron paste method, dry it completely, and pull 3x with dry IPA or acetone, then fasa/fasi your pulls.

You could prob get away with it only using a few grams of lime/or about 3x more by weight if you use sodium carbonate, a gram or so of fumaric acid, and maybe 250ml of dry IPA or acetone per 2g of freebase oil you put in. You don't need limo, but it is another way to do it.

I personally prefer the fasa/i and freebase in dry alcohol technique, over freebase in limo and fasa/i, but they both work well. Your just assured no excess fumaric acid will precipitate, where as with limo, fumaric acid is not soluble in it, compared to acetone/ipa, where the solvent your freebase is dissolved in will solubulize any excess fumaric acid.

Should give you a fairly pure white to yellow colored precipitate, that if you keep dry when letting the residual iso/tone evap (evap cools the container, humidity in the air condenses and hydrates the dmt fumarate crystals, giving you gooey crystals until you dry them) , and always use dry iso/tone, it will be solid, and once fully dry if it gets wet, will stay dry and can be crushed into a fine powder.
 
Thanks for the replies everyone. It's very educational to see the different approach to same problem. I will try it out sometime this week after absorbing the info and I'll post again to let know the results.

Many Blessings :thumb_up:
 
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