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Evaporation vs Freeze Precipatation? Options
 
behindthelight
#1 Posted : 10/28/2011 5:18:30 AM
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I have found a few teks and some of them say to pull the naphtha out and put it into a jar and "freeze precipitate" it.

Other say to just put the naphtha into a glass pyrex dish and let it evaporate. Here is an example:
"Take all of the clear naphtha and pour all of it into as large a flat glass container you can find for evaporation. Using a fan to blow air across the top of the fluid will help speed the rate of evaporation several fold faster."

So do Evaporation and Freeze Precip achieve the same thing? You can do whichever you want?

Thanks.
 

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endlessness
#2 Posted : 10/28/2011 9:05:49 AM

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Freeze precipitation results should result in cleaner crystals. What happens when you freeze precipitate is that with the lower temperatures, DMT is less soluble in the solvent, and then it precipitates, but at the same time certain plant oils and other impurities are still soluble in the solvent. This way you are separating the DMT from some of these impurities that ended up in the solvent. With evaporation, your end result will be the mixture of every single thing that there was in the solvent. Also, with freeze precipitation you can reuse your solvent, with evap you cant.

Depending on a few variables of your extraction (amount/temperature of solvent, how well it was mixed and how long it was standing, original plant material, etc), the naphtha wont really pick up much impurities at all, so a simple evap will yield you some nice crystals. In general though it is quite common that evaporated pulls will yield more oils.

A good thing about evaporating is that you can very easily grow large crystals by just semi-covering the evaporating container so that it evaporates very slowly. Nevertheless if you have impure solvent, the crystals that might grow might also be very yellow or surrounded by a lot of oil, that when you scrape will mix with your crystals. So if you want to grow large crystals, it is recommended to first freeze precipitate and/or recrystallize to get something pure, and then redissolve in naphtha and evaporate slowly.
 
behindthelight
#3 Posted : 10/28/2011 5:00:27 PM
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Nice detailed reply thanks for that.

Let's say I wanted to use the pyrex dish to FP, I could put the dish in the freeze and cover it with Foil right? Then once the crystals have dropped out, I could pour the naphtha off and then let the crystals dry in the open air.
 
Dan
#4 Posted : 10/28/2011 5:26:42 PM

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how much bark did you start with and how much solvent was used per pull? how many pulls were done? if you used excess amounts of solvent then you may need to evaporate it down to 1/2 or 1/3 of the original amount first so you can super saturate your solvent and it will crash out easier in the freezer.

good luck.
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endlessness
#5 Posted : 10/28/2011 5:32:07 PM

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As zion said..

Regarding the freez container, simple foil around it might not really close it well, so your freezer can smell of naphtha after... Maybe some kind of jar instead?
 
behindthelight
#6 Posted : 10/28/2011 6:46:52 PM
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Ok, so for my first run, I just wanted to test thing out to make sure I was doing it right, so I used a pint ball jar and only 20 grams of MHRB. It worked fine, I got crystals to drop out after I put the jar in the freezer. Then I poured the Naphtha back into the other jar and I had DMT crystals. I noticed it is kind of hard to get the crystals out though, that is why I was asking about the pyrex dish. Maybe I just need to use a bigger jar like a quart jar or something.
 
endlessness
#7 Posted : 10/28/2011 6:52:54 PM

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you could pour the naphtha out, then get a little bit of fresh naphtha and warm it up and redissolve the crystals and evaporate them on a pyrex dish slowly. This way you have cleaned up from the oils after freezing, and also get some nice crystals on pyrex dish that are easy to scrape

Or find a better tool/bigger jar.
 
behindthelight
#8 Posted : 10/28/2011 8:58:58 PM
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thanks man....will do.
 
nemo
#9 Posted : 11/4/2011 2:28:08 AM

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At first I had some problems with my freeze precip crystals sticking to the sides of the jar and being very difficult to get out, but after changing the following Ive had no such problems..

First I began slowing down the cooling process, started with heated naphtha and letting it cool slowly to room temp, then slowly to fridge temp (in and out of fridge a few times over half a day) and then into the freezer for another day or two. This helps the crystals grow a little larger and chip off the sides cleanly.

Second I made a special top for the jar to pour the naphtha out. The top just has two small holes punched in it, this allows me to pour out the naphtha with the minimum amount of needed air (which has water which condenses on the sides) getting into the jar. I then put the airtight top back on, put it upside down and let it slowly warm to room temp before opening. I let the few drops remaining in the jar into a dish to evap and catch any spice left in it.
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behindthelight
#10 Posted : 11/4/2011 3:21:09 AM
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nice man..!!!
 
 
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