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Best way to recover freeze-precip'd DMT that melts into transparent drops? Options
 
Jagube
#1 Posted : 10/5/2019 12:45:29 PM

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When I freeze-precipitate naphtha pulls from Phalaris, I get off-white blobs, which upon warming to room temperature and air drying melt into transparent drops. I'm guessing those drops (and the initial off-white blobs) contain a lot of water.
The dish smells like DMT.

Eventually the dish is left with a very thin white residue that's hard to scrape off as it's too thin and the blade and dish surface are not even enough to catch it.

I guess I could wash the dish with IPA, collect it into a smaller area (a titled plate or something) and evaporate it? Or is there a better way, maybe one that would avoid the drop formation in the first place?
Jagube attached the following image(s):
droplets.jpg (1,696kb) downloaded 88 time(s).
 

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coAsTal
#2 Posted : 10/5/2019 5:49:55 PM

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You'll be far, far better off consolidating your solvent into a smaller jar like a half-pint or pint mason -- that will allow it to form much larger crystal in the denser space.

I quit using large trays/containers like yours almost immediately after starting this journey because of your exact problem-- it was more pain in the ass to get the results off the damned glass than it was to just consolidate the solvent in a smaller container and let it all form up in it.

Also, your product may well liquify at room temp or warmer-- if I warm even solid glass crystal too much it will become an oil-- still 100% good to use assuming you have removed all the solvent. By conventrating your solvent into a smaller cup you'll reduce oil film if you freeze, as the crystals seem to form far better in that environment than in a flat pan.
 
pete666
#3 Posted : 10/5/2019 7:20:22 PM

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Yes, good advice.
I always use beaker sealed with plastic film and rubber band when put into the freezer. Once removed, I remove just small hole to carefuly pour of the solvent. The main reason is not to allow any air into the beaker. Any air bears a lot of water which will condensate when exposed to low temps of the beaker or crystals. Once poured off, I put the beaker upside down onto plate, removing the saran wrap first, again trying to minimize any air exchange. Then it is left as is hour or two to get to room temp. Once at room temp I turn it back and leave it 12-24 hours with the fan blowing air over the beaker.
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Jagube
#4 Posted : 10/6/2019 12:35:14 PM

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Thanks guys.

Now that I think of it, it makes sense. The large surface area makes the DMT more spread out and makes it harder for the molecules to find one another and clump into crystals.

But then, with MHRB it worked just fine. There may still have been losses, but I didn't notice them as there was still a lot of DMT to scrape up.
 
blue.magic
#5 Posted : 10/9/2019 5:29:44 PM

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Yes seal your freeze precip container - cold surfaces attract water by condensation.

What I do is to colllect the extracted solvent and dry it with magnesium sulfate (do not use calcium chloride as amines don't like it). Then I filter it and concentrate to near saturation point.

Finally, the saturated soln. usually drops an oily drop. I carefully pour off the solvent into the freeze-precip Pyrex dish and wash the flask 2-3 times with small amount of fresh hot solvent, keeping the dirty oily drop in the flask.

I still often get oily sediments, but this is usually when I am not careful about solvent temperature. Recrystallization resolves this.
 
downwardsfromzero
#6 Posted : 10/9/2019 8:04:55 PM

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Quote:
(do not use calcium chloride as amines don't like it)

While the overall sentiment here is broadly correct, one could rather say to avoid use of calcium chloride because amines like it too much in that they stick to it forming a complex. /chemist humour

Anyhow, I've also described elsewhere how using anhydrous sodium carbonate as a drying agent for post-base-pull solvent appears to work. I chose this in order to optimise yield by avoiding most chances of acidity whereas even magnesium sulfate is very weakly acidic.
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Tony6Strings
#7 Posted : 10/10/2019 8:49:22 AM

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coAsTal wrote:


I quit using large trays/containers like yours almost immediately after starting this journey because of your exact problem-- it was more pain in the ass to get the results off the damned glass than it was to just consolidate the solvent in a smaller container and let it all form up in it.



I can see that in this situation and similar, where someone is working with minimal alkaloids. When pulls contain significant spice (a half gram or more) collecting it from the bottom of a casserole dish is no problem. In my experience that is, ymmv. I love my corningware. Love
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coAsTal
#8 Posted : 10/10/2019 3:58:56 PM

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It's certainly do'able, but the reason I do my evaporations in small containers is very simple-- once I have all my spice in solid form, then that same container is my storage place Smile

Maybe I'm just lazy-- but I like to use the same container to dose from that I evapped in, and having everything readily condensed in a small jar allows me to both produce and use the crystal without having to move it.

Also, when all/most of the solid is used, it's super easy to put a couple ml's of everclear and leaf (damiana, mullein, mugwort, caapi etc...) in the jar and scrub off the film/oil to make sure I get the jar clean and every last bit of spice into my enhanced leaf.

All methods can be good- it's just up to you what you like Thumbs up
 
TalkingGarden
#9 Posted : 10/10/2019 5:56:40 PM
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So I found out pritty quick after the freeze putting it in front of the fan any smaller xtals or thin layer would collect water droplets and quickly turn to a oil. This happends especially in summer cause well its hot and humid! So now I always tilt the dish 1 way during the freeze dump out solvent tilt the other way back in the freezer so any remaining solvent drains to the other side after a couple hours I put it in front of a fan BUT I don't use a regular fan...I use a de humidifier this way the air coming out is drier and also it happends in a room where the de humifier has been running I think that helps! Recently I have started to only even blow it with that for a short time just to get the major part of the solvent evaped. Once I know there isn't a lot of solvent left it goes into a vac chamber and dries in there. It will minimize oxidation as well and has the benefit of me feeling safer ALL the solvent is gone....If I get bigger crystals after that I will even break them up and put them back in the vac chamber for a little bit that eases my fear about any residual solvent being trapped! Some is not needed but like I said it makes me FEEL better and that makes for a better experience! worrying your sice isn't good pre trip is not good!
 
blue.magic
#10 Posted : 10/14/2019 3:00:42 AM

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downwardsfromzero wrote:
Quote:
(do not use calcium chloride as amines don't like it)

While the overall sentiment here is broadly correct, one could rather say to avoid use of calcium chloride because amines like it too much in that they stick to it forming a complex. /chemist humour

Anyhow, I've also described elsewhere how using anhydrous sodium carbonate as a drying agent for post-base-pull solvent appears to work. I chose this in order to optimise yield by avoiding most chances of acidity whereas even magnesium sulfate is very weakly acidic.


Whoa, thanks for extending my chem knowledge!

Yes using basic salt makes sense - I never knew Na2CO3 can be used like that and that it hydrates easily enough to be used as a drying agent.
 
 
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