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Dry ice to precipitate NMT carbamate out of NP solvent for ACRB extract Options
 
endlessness
#21 Posted : 9/1/2013 9:10:11 PM

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As mentioned before, the NMT carbamate could be re-converted and recovered by redissolving and basing the solution with lye, after you have separated it from your DMT.
 

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DonPeyote
#22 Posted : 9/4/2013 2:21:13 AM

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Hypothetically, why not sublimate the final step (non-polar extraction), of an AB extraction of ACRB with Dry Ice?
After the NMT has precipitated out as a carbamate, you should be left with DMT in solution, which you could then precipitate, freeze or otherwise.

Does this make sense, or am I missing something?

DP
 
arcologist
#23 Posted : 9/4/2013 2:28:32 AM

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Yup, that's the plan in the future. I only did it after doing FASA because I wanted to try that first. It worked great to add dry ice to my raw xylene bark pulls and I'm sure naphtha would work too (or any NP solvent).

Basically:
1. A/B or STB extraction -> NP solvent pulls
2. Add dry ice 3x or until nothing else precipitates
3. Warm water bath to raise to room temperature/redissolve DMT
4. Decant solvent away from carbamates
5. Freeze precipitate/FASA/evap solvent
 
DonPeyote
#24 Posted : 9/4/2013 6:19:08 AM

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I currently have 4-5g of NMT/DMT 'Goo', some of which I plan to sublimate with dry ice tomorrow.
Other than using a "high walled" container, are their any specific tips or concerns using dry ice?

I will experiment with 1 gram to start, then as I understand the reaction better,
attempt a larger amount.

DP
 
arcologist
#25 Posted : 9/4/2013 6:48:46 AM

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You'll need to wear gloves or risk getting freezer burn on your fingers. Definitely be wary of violent frothing, only use small pieces of dry ice at a time (<2cm^3). There's a very small possibility (or maybe not) that if you put too much in at once it could cause temperature shock, causing the glass to crack as it cools too quickly. Warm up the solvent after adding dry ice the last time to put the DMT back into solution. Other than that it's pretty idiot-proof. Good luck!
 
lysurgeon
#26 Posted : 9/4/2013 7:27:32 AM

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I wonder if bubbling CO2 gas from a tank or a CO2 generator would be a feasible option, or if the exothermic nature of the reaction requires dry ice?
 
arcologist
#27 Posted : 9/4/2013 7:57:12 AM

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I'm sure it would work with gaseous CO2, but the reaction might take a lot longer to complete. I think I read one report of someone who tried it and had some very small amount of precipitate, but not nearly the amount that I observed precipitate in under a minute. The dry ice is great because it saturates the solvent with many CO2 bubbles, so that no part of the solvent isn't reacting.
 
DonPeyote
#28 Posted : 9/5/2013 12:30:22 AM

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I tried the CO2 gas method, albeit using acetic acid and sodium bi-carbonate as my gas generator.
At room temp and atmosphere, nothing.

At increasing temperature and pressure, I managed to squeak out some red colored precipitate.

Admittedly, this could be done much better with lab equipment and bottled gas.

The beauty of dry ice is the simplicity of the reaction: sublimation.

Its hard to see how CO2 gas can beat sublimating frozen CO2, bubble for bubbles.

DP
 
Precog
#29 Posted : 9/5/2013 12:47:48 AM

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Many props to Arcologist for what so far is a highly intriguing discovery with beautiful results. I'm very eager to see if you can produce something similarly promising, DonPeyote. Best of luck and keep us posted!
"The peak experience might be likened to a spot on a mountain top from which the surrounding panorama may be viewed; yet being on the top of the mountain does not supply more than the possibility of seeing, whereas this process of observation is different from that of mountain climbing[...]insight is distinct from the mental state from which it originates, and constitutes the result of a creative act in which consciousness at a certain height is directed toward what lies below."
--Claudio Naranjo

There is no becoming, no revolution, no struggle, no path.
Already you are the monarch of your own skin.
--Hakim Bey
 
DonPeyote
#30 Posted : 9/5/2013 12:56:18 AM

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I just finished NMT-DMT separation using dry ice.

It's actually fun to do!Smile

I started with 2.5 grams 'goo', which I re-dissolved in about 60mls of naphtha.

Thrice the solution was treated with dry ice (each cube about 2cm/side).

The result was warmed to re-dissolve the crashed DMT crystals, then decanted into a dish, sealed, then placed in the freezer.

Looks like about 1/2 the original material was left behind as an off-white/reddish colored goo, which conveniently stuck to the bottom of the jar.

And now the wait....

Thanks arcologist!

DP
 
Parshvik Chintan
#31 Posted : 9/5/2013 9:34:13 AM

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can we expect pictures in the near future?
My wind instrument is the bong
CHANGA IN THE BONGA!
 
DonPeyote
#32 Posted : 9/5/2013 7:33:56 PM

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Nice crystals formed overnight in the freezer!
I decanted the naphtha, and set the dish in a 'cool, dark place' to evap the residual solvent.
From experience, living in the tropics, it takes a few days to re-crystallize after freezer precip.
And lately its been bloody HOT and humid here, so that may add a day or so.
But of course I will photograph and share the results.
Patience....

DP
 
arcologist
#33 Posted : 9/5/2013 8:07:04 PM

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Did your crystals stay solid after you poured off the naphtha? If not you might not have gotten all of the NMT out. I had to redo one batch because they melted. It also helps to let as much cold naphtha drip out (hold container upside-down) as possible, then put 4-5 feet away from a fan. It shouldn't take more than an hour or two to dry out under those conditions.

Looking forward to your results!
 
DonPeyote
#34 Posted : 9/6/2013 2:46:34 AM

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Yes the crystals mostly melted, but the same thing happened with MHRB. It took several days for the crystals to regrow.

I'll give it a few days. If it stays a goo, I'll re-do your 'Dry Ice Method'.

Most of the NMT was locked up in a carbamate, but who knows?

DP
 
DonPeyote
#35 Posted : 9/7/2013 7:08:48 AM

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Slowly the crystals ARE regrowing.

Perhaps a few more days, and then I'll post a photo.

The next time I use dry ice to separate NMT from DMT, I will use a bit more dry ice, and cause a more violent sublimation.
As long as the reaction dosent spill over the sides of the container, why not?

Is there any danger that some of the DMT will precipitate as a carbamate, thereby lowering the yield?

In any case, its a breakthrough technique for generating pure DMT during ACRB extraction.

 
arcologist
#36 Posted : 9/7/2013 8:14:33 AM

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Nice, hopefully they continue growing Smile There shouldn't be any danger of reacting with the DMT because it's a tertiary amine and won't be able to react in the same way as NMT to form a carbamate. I'd say overdo it - add dry ice 3 times, warm bath, then decant away into another container, then add dry ice again and warm bath until you don't get any more clumpy precipitate formed. At some point there won't be any reaction that occurs once the NMT is exhausted.
 
DonPeyote
#37 Posted : 9/10/2013 5:37:32 AM

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Well, its taking forever, but there is still some NMT goo that wont dry, maybe 5%?
I have a new batch of ACRB (1 kg. extraction), AND I will treat both with successive dry ice, until no furthur carbamates form.
I think I have a handle on the process...
Photos coming soon.

DP
 
arcologist
#38 Posted : 9/10/2013 6:44:29 PM

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It seems like if there is any NMT at all (probably >1%) that the result won't crystalize at room temperature. That tiny proportion of NMT keeps a strong DMT crystal lattice from forming.

I've been experimenting with the resulting NMT I've gotten from this process - I dissolved the carbamates in acidic water, based with NaOH, then pulled with xylene, then added FASA to precipitate NMT fumarate. Surprisingly, the resulting salt crystalized into an off-white powder that stays solid. This is in contrast to when I FASA precipitated a mixture of NMT/DMT, resulting in a goo. I guess since I was dealing with very pure NMT it was able to crystalize in a way that a mixture of NMT/DMT fumarate wouldn't. It seems like the fumarate should be a good way to store/handle the NMT. I will try converting it to freebase to see if I can get NMT freebase crystals to form in the absence of DMT.

Let us know what kind of yields you get from that kg extraction, DP. My extraction for this thread was also a kg of hawaiian ACRB, and my final yield of pure DMT was just above 6g, slightly disappointing based on the reported ~1.5% DMT content of the bark. I think with a more streamlined extraction and doing more pulls (I only did 4), you could probably do better.
 
DonPeyote
#39 Posted : 9/12/2013 1:45:27 AM

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I finished the extraction, did 4 'pulls', and treated each pull with dry ice.

To be sure there was no lingering NMT:
After initial dry ice treatment, I brought the solution back up to room temperature in a warm bath (dissolving the DMT back into solution), decanted the solution into a clean jar, and re-treated with dry ice.

Whats odd, is the first pull had no DMT whatsoever.Surprised

The second pull has nice white crystal formation, as well as the third.

I added 100g rock salt to the fourth pull, which just went into the freezer.

The 2nd and 3rd pulls precipitated carbamates like crazy! After filtering, the solutions were pretty much NMT carbamate free. But I had 2 pounds of dry ice to play with, so I thought, why not be sure?

I did put in one chunk of dry ice too many, which caused some over-spill. Live and learn I sayNeutral

Hopefully, I will report success in the near future. Until then, it's a waiting game. Again.

By the way, I also re-treated the previous batch, which never fully dried (due to a tiny amount of NMT), with dry ice. Although 100mg of it DID dry, as perfect white crystals, the rest measured .75g of NMT/DMT. So from an initial 2.6g, I went down to .85g, and it will no doubt go down again after this final? re-crystalization.

One last note:
Most TEK's say its preferable to re-use the naphtha from one pull to the next, as its saturated with DMT. After thinking about it, that can't be right. If the naphtha is already saturated, how is it able to pick up any additional DMT?

DP
 
arcologist
#40 Posted : 9/12/2013 3:56:23 AM

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Are you doing A/B or STB? I noticed my first STB pull was kind of weak but I chalked it up to the bark having not broken down enough.
 
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