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Fumarate to Freebase problem

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Attention All Shipping

Rising Star
About 2 weeks ago I tried to convert ~200mg of fumarate to freebase using 69Ron's tek:

69Ron wrote:
1 - Mix DMT fumarate with 1 part calcium hydroxide (calcium carbonate should work as well).
2 - Add enough water to make it wet and mix. (Freebase the DMT again)
3 - Spread it out and let it dry completely.
4- Dissolve it in acetone and filter out the solids. (At this point only alkaloids like DMT should dissolve)
5- Evaporate the acetone to get nearly pure freebase DMT.
Click to expand...

I've got to step 5 with no problems but now it seems the acetone just isn't evaporating any more, I've got a fan on it & everything but There are still little gooey clumps of goo that won't evaporate, along with parts that have evaporated as expected.

Here's a pic:
P6010014.jpg

P6010016.jpg

P6010008.jpg


What's the problem, it surely shouldn't take tis length of time to evaporate, should it?
 
2 weeks for 200mg!? Sounds like SWIY's probably got some serious moisture contamination. Perhaps scraping it up and working it around would help? 2 weeks is a long time though, so hopefully none of that oxidized. How deep is that dish? SWIM either uses a pie dish or a shallow dish lid, upside-down. Was the location fairly dry? SWIM leaves his on a cupboard near the ceiling in the kitchen. SWIM has regularly dried upwards of a gram at a time within less than a week without any problems.

On second glance, SWIM really thinks those top two pictures look like it's ready to be scraped anyway...not sure what's going on with that third one.
 
SWIM had the same problem recently. It never crystallized, just stayed a runny reddish-yellow goo. He eventually did a naptha extraction and freeze precipitated crystals from it, but will eventually have to evap the naptha to recover it all, as he's noticed quite a bit says in the naptha even after a freeze precip.
 
Tribal said:
SWIM had the same problem recently. It never crystallized, just stayed a runny reddish-yellow goo. He eventually did a naptha extraction and freeze precipitated crystals from it, but will eventually have to evap the naptha to recover it all, as he's noticed quite a bit says in the naptha even after a freeze precip.
Click to expand...

Reddish? That doesn't sound quite right. Perhaps some contamination containing bark material? Did SWIY reduce the volume of the naphtha befor freeze-precip?
 
Not reddish exactly, more like dark yellow, almost orange. He was freebasing the most yellow of the fumarate that was extracted. He didn't reduce the amount of naptha, but instead did several extractions/freezes with a small quantity.

All in all about 3/4 of the original was recovered, which seems about right taking the fumarate weight loss and mechanical losses into consideration, not including what is probably still in his naptha.

Attention All Shipping - one possibility if you don't want to mess with the naptha would just be to redisolve it in a little more acetone and make enhanced leaf by adding it 1:1 with a preferred smoking medium. It always crystallizes that way and smokes much easier. Mullein works well.
 
Tribal said:
Not reddish exactly, more like dark yellow, almost orange. He was freebasing the most yellow of the fumarate that was extracted. He didn't reduce the amount of naptha, but instead did several extractions/freezes with a small quantity.
Click to expand...

Yes, that's actually the best way. SWIM hasn't used naphtha in some time.

All in all about 3/4 of the original was recovered, which seems about right taking the fumarate weight loss and mechanical losses into consideration, not including what is probably still in his naptha.
Click to expand...

3/4 is almost exactly what SWIY should recover. The fumarate's only about 73% DMT at best. Why does SWIY think there's so much left in the naphtha?
 
There probably isn't a lot still in the naptha, since he used such a smaller amount repeatedly, but there is always a measurable amount recovered after he evaps it.

The point being, I guess, that redisolving in acetone and making enhanced leaf would be much easier, faster, and have less loss than fooling around with naptha extractions.
 
amor_fati said:
2 weeks for 200mg!? Sounds like SWIY's probably got some serious moisture contamination. Perhaps scraping it up and working it around would help? 2 weeks is a long time though, so hopefully none of that oxidized. How deep is that dish? SWIM either uses a pie dish or a shallow dish lid, upside-down. Was the location fairly dry? SWIM leaves his on a cupboard near the ceiling in the kitchen. SWIM has regularly dried upwards of a gram at a time within less than a week without any problems.

On second glance, SWIM really thinks those top two pictures look like it's ready to be scraped anyway...not sure what's going on with that third one.
Click to expand...
It wasn't left near any moisture & its just in a normal pyrex pie dish. I'll try scraping it about though before trying redissolving in naphta or acetone.
All the pics are of the same dish its just the last pic on a white background gives a clearer view of undried blobs, though not the dried bits.
 
Neither SWIM nor some of his FOAFs have ever had this much trouble with this. It may be easier for some to just skip the acetone all together and just use naphtha and freeze precip.

SWIM wonders though, what brand of acetone is being used? SWIM only ever uses kleanstrip.
 
The brand/supplier is hyperclene, its sold as Acetone UN-1090, which I take to be 100% acetone.

I've now scraped about the gooey bits, though they don't spread out well. I'll leave it under the fan & see if it makes a diference.

Is oxidisation likely to be a problem? I'd thought that as I was just freebasing fumarate and as the fumarate contained the full spectrum of alkaloids, including those that'd oxidised, there wouldn't be any risk of further oxidisation.
 
^ Filtration and/or decanting should work. No problem with smoking if some of the lime would end up in the freebase.
So far I've only done this with sodium carbonate; this falls to the bottom very quickly, and filters out easily from the aceton.
 
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