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Recrystallization / mini-A/B? Options
 
#1 Posted : 9/1/2016 11:18:58 AM

Psilosopher


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Hey everyone!
I performed Cyb's Max Ion using around 100g of MHRB a few months ago.
The bark itself was over 2 years old, and I took breaks inbetween each pull as I didn't have the most optimal pipette and glassware at the time and I spent a few hours on every pull.
The basified bark + leftover naphtha often sat for a week or longer in the extraction vessel before taking the next pull, and due to my impractical pipette I also got little bits of base solution in with the pulls. No problem as I was going to recrystallize the end product a few times anyway.
Pulls were combined and left to entirely evaporate. I ended up with a small jar full of brownish waxy stuff, which I saved in an amberglass jar in my freezer.

Fast forward 5-6 months, I have been trying to clean it up a bit.
I did not weigh the product beforehand as it was far too gooey and would stick to everything it touched. I poured it straight into a small erlenmeyer flask, added a bit of heptane and put it on low heat on my hotplate, stirring it until fully dissolved. I separated the solution from the oily sediment and again left to evaporate (no freeze precip).

First re-x

Here is the result after first re-x:


Scraped up:


Second re-x

Dissolving impure dmt:


Fully dissolved (should I have stopped at previous picture instead?):


After evap:


Scraped up (weighed in two batches as it would not fit on there, 1.345g in total):


Third re-x

Sidement left behind in flask after third re-x:


After evap:


Scraped up:


As you can see, the end result is definitely looking cleaner after every re-x, it went from waxy brown to only slightly sticky mostly freeflowing yellow/orange crystallized powder. It seems like I am unable to remove the yellowing though, and I'm wondering if this is because I have lots of n-oxide or if there are still a bit of plant oils in there that I somehow can't separate using re-x.

I'm wondering if I maybe used too much heat during these recrystallizations? I used generous heat to make sure everything dissolved fully, and there was always some visible sediment, but at the same time my heptane is always colored a deep golden orange, kind of like honey:


Is it possible that I'm getting it too hot and impurities are also being dissolved into it? Where do you draw the line that you're no longer dissolving your DMT into the solvent but also the impurities?

Should I attempt a mini-A/B or "backsalting" to clean this up further, or does it look ok to vape as is?
From what I gather this means:
1. Add impure spice to minimal amount of naphtha / heptane
2. do three pulls with vinegar solution (ph 2-4; 100ml of pure 7% white vinegar can be used per pull? No need to let it soak for a while?)
3. combine vinegar, add lye until pH 12, mix thoroughly
4. do three more naphtha / heptane pulls
5. combine pulls and evap / freeze precip?
"The only way to deal with an unfree world is to become so absolutely free that your very existence is an act of rebellion." - Albert Camus
 

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FLeP
#2 Posted : 9/1/2016 7:54:35 PM

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Smoke it!

In my experience it can be a real pain in rear trying to get the color out of some MHRB and not really worth the while that I could tell.
 
Psilosopher?
#3 Posted : 9/2/2016 1:39:36 AM

Don't Panic

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Those first re-x crystals look damn fine to smoke. It's still very, VERY active.
"A common mistake that people make when trying to design something completely foolproof is to underestimate the ingenuity of complete fools."
 
#4 Posted : 9/7/2016 10:44:21 AM

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Thanks, I will leave the extract the way it is. It's easy enough to handle and smells pretty great.
I was just a bit surprised it didn't come out cleaner (whiter) after three re-x's and if maybe my technique was off or this yellowing is to be expected from such old bark. I know active charcoal could help here as well, but alas I don't have any on hand to try it out. I will definitely not underestimate its potency though :-)
"The only way to deal with an unfree world is to become so absolutely free that your very existence is an act of rebellion." - Albert Camus
 
Running Bear
#5 Posted : 9/11/2016 8:18:21 AM

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I'm going to be completely honest with you. I don't think i would be brave enough to smoke that. If I was you I would put your dmt in a small jar/ shot glass with about 75 ml of naphtha. Heat up the jar/shot glass and stir until all the dmt is absorbed into the naphtha. You will see the impurities drop 2 the bottom. Take your jar, cover it and put it in the freezer for 30 min to a hour. The naphtha will now be white/milky. if you notice that the dmt crystals formed its no problem all you have 2 do it heat it again and put it the freezer for a shorter period of time. After the freezer step all the impurities should be on the bottom of the jar and what you want 2 do now is siphon out the milky naphtha without getting any of the junk on the bottom. Put the naphtha on the glass dish (you may want to clean that dish first lol), Cover it with saran wrap. Put the glass dish in the freezer for 12 hours. After the 12 hours Dump the naphtha into a jar. Put the glass dish in front of a fan for about a day. You now have pure/white dmt.
 
null24
#6 Posted : 9/11/2016 5:13:17 PM

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Quote:
.I'm going to be completely honest with you. I don't think i would be brave enough to smoke that.


Really? Why, looks great to me?
Then again, I'm a"full spectrum" kind of guy?
Sine experientia nihil sufficienter sciri potest -Roger Bacon
*γνῶθι σεαυτόν*
 
Running Bear
#7 Posted : 9/11/2016 7:57:53 PM

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null24 wrote:
Quote:
.I'm going to be completely honest with you. I don't think i would be brave enough to smoke that.


Really? Why, looks great to me?
Then again, I'm a"full spectrum" kind of guy?


It probably is good lol. I always freeze precip my dmt and use naphtha 2 re-x. Maybe heptane turns it into a different color? On the 3rd pic he says Dissolving impure dmt and it looks like he hardly used any heptane and then on the 4th pic it looks like he mixed all the impurities with the clean dmt haha?
 
FLeP
#8 Posted : 9/14/2016 2:03:42 AM

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That spice looks tasty as all get out to me.
 
pitubo
#9 Posted : 9/14/2016 11:20:16 AM

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OP, if you redissolve your spice in solvent, then decant it from insolubles and finally fully evaporate the solvent again, that can be called a insolubles cleanup, but IMHO not a proper recrystallization.

A recrystallization usually yields less product, but of a higher purity. The mother liquor that is separated from the reformed crystals will contain the rest of the product in an even less pure condition than the starting material.

In fact, if the solvent you used contains nonvolatile impurities, you'll be adding these impurities to the result, negating much of the cleanup effort.

A mini-A/B would almost certainly give much more pure product, but also almost certainly less off it than a simple recrystallization.
 
 
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