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Recrystallization Teks and tips

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BGTM236

Rising Star
Ive looked all over, and i havnt found a cohesive thread for recrystallization. If there is one out there, i apologize for the redundancy. However, I think there needs to be one in the nursery.

SWIM has attempted a handful of recrystallizations and has had moderate success. The biggest problem he encounters is what to do with the oily substance once SWIM has dissolved all his DMT in the solvent. SWIM has trouble removing it without removing a large amount of DMT also.

SWIM would like to know how the more experienced re-xers do it.
 
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To be honest altho many will disagree, I have come to dislike the recrystalizations all together, well the ones where your trying to clean up (isolate) a big yellowy mess, such as what comes out from a stb, thats why I got my a/b method down so only a very simple re'x can be done.

the reason why I say I dislike it is one because for me in order to go from yellow to crunchy clear, I have to heat up the heptane over 140 F. in order for everything to dissolve and hold it there for to long burning away spice. For me the only way to get glass spice from a yellow mess would be to dissolve all the spice in the NP then insulate the vessel allowing it take a total of 5 days or so to cool down..... the whole time you keep the vessel at a 45 degree angle, all the gunk will go down to the corner. when all done it's very easy to scrape away your crystals from the orange oily (hardened) mess.

the quick re-x's where you dissolve everything, allow to cool for a minute then isolate the goo away proceeding to throwing your heptane/naptha in the freezer works ok, but never have I gone from yellow to clear doing this method and I have tried many different ratio's. however I find using a pipette with one of those thumb wheels on the end works great for just accuratly withdrawing what you want (in this case the yellow goo). the regular pipette with just a squeeze bulb is way to hard.
 
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SWIM's "tek" for recrystalization is pretty simple.

#1:First soak the impure spice in naptha that is luke-warm, like 25-30 C, but no need to be too exact. This will pick up the white N-N-DMT.
This can be done once or twice to make sure.

#2:Next do another wash with warmer naptha, almost as hot as hot tap water. That will pick up what SWIM assumes says is the "stubborn" N-N-DMT that hangs out with the yellow N-oxides.

#3:There will likely be some dark yellow/brown goo left. Add naptha as hot as you can get it (be careful) that will dissolve the N-oxides

All of the naptha pulls can be seperately freezer precipitated, though the 3rd one would probably be better evaporated, as well as the 2nd one after freezer precipitation. Naptha doesn't freezer precipitate n-oxides as well. Though SWIM prefers the experience of N-oxides once you get past working with a goo. Evaporating it onto some herb appearently works well.

All of the naptha should be heated with a hot water bath, DO NOT heat it directly or you are asking for a fire.

Cheers.
 
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really you guys use naptha for re'x?
n-heptane is alot better,
I dont think you can get chunky clear with naptha,
just white......
n-heptane takes roughly 30ml per gram....
it's commenly sold as bestine in art supply stores.
 
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q21q21 said:
Mr. Kush said:
it's commenly sold as bestine in art supply stores.
Click to expand...

a while back, called all the listed ones... none have it.
Click to expand...


Look online. You know the site named after the rain forest? You can get 2 32OZ cans for about $40. Thats only about $10 more than you would pay from an art supply store or a wood working shop. Those 2 cans should easily last you through 600-800G worth of extraction, re-xing, and pipe cleaning if you are using a vaporgenie.
 
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Mr. Kush said:
really you guys use naptha for re'x?
n-heptane is alot better,
I dont think you can get chunky clear with naptha,
just white......
Click to expand...
Never used anything but naptha for re-x and I've grown large (nickel to quarter-sized base) clear crystals, don't really care to take the time to do that generally though. Imo it's not worth the time/effort and as I don't like pure DMT as much as wide-spectrum pulls or DMT/n-oxide combos i stopped making clear crystals a while ago.

EDIT:

And what soulfood says below is true, a curved bottom container works great. I used to use a really wide wine glass to make real thick crystals, the trick is not disturbing it once you put your solution in there.
 
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BGTM236 said:
What kind on container should i use for a re-xing? Ive been using a pyrex baking dish, the same thing i use during the extraction process.
Click to expand...

I use a small dish about 2 inches wide that's rounded at the bottom so the crystal formation seems to collect more towards the bottom.

After a slow re-x I can pick up a crystal in my hand and drop it without any shards coming off :)
 
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soulfood said:
BGTM236 said:
What kind on container should i use for a re-xing? Ive been using a pyrex baking dish, the same thing i use during the extraction process.
Click to expand...

I use a small dish about 2 inches wide that's rounded at the bottom so the crystal formation seems to collect more towards the bottom.

After a slow re-x I can pick up a crystal in my hand and drop it without any shards coming off :)
Click to expand...


A dish that has a 2 inch diameter seems incredibly small, how much dmt are you re-xing when you use that?

Is it a good thing have a high solvent to surface ratio with the container youre using? I have a few small brandy glasses with a rounded edges and a small well in the bottom, but 30ml of solvent would be almost half of the volume capacity. Would a ceramic cereal bowl work well?

How does SWIM perform a slow re-xing? After melting his DMT in heptane, SWIM has let his container sit in a cold water bath for about an hour, then in the refrigerator for 12 hours then in the freezer for another 4-8 hours.
 
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Well forming crystals get attracted to crystals already formed, so if you put a flat crystal in the middle of a DMT saturated solvent it's easier for the DMT crashing out to find the crystal in a smaller container. Otherwise you get lots of smaller crystals all over the place.

Also a smaller diameter of surface area makes for slower evaporation if you want to take that route, which will also give you slower forming and therefore more thoroughly structured crystals.

When I re-x I heat my naphtha with water from a hot tap and then mix in as much DMT until the solvent is saturated, then I pour that onto my seed crystal and I let that sit in the same warm water I heated the naphtha with and allow it to cool to room temperature over the space of a couple of hours. Then 4 hours at room temperature, then 4 hours by an open window, then 12 in the fridge then up to 24 in the freezer.

More often than not I don't require my spice to be THAT solid though :) But it is nice to be able to handle it more solidly at least once or twice in your life. Also as I said earlier I seem to be getting glass shards on the first and only freeze precip as I cool that quite slowly aswell. Slow crystal formation is a cleanup stage of its own that doesn't require any additional materials.
 
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hmmm I get the Idea some are referring to a re-x in the manner that there just growing out the crystals and some are trying to isolate impurities by taking advantage of the different solubilities at different temps.

How does SWIM perform a slow re-xing? After melting his DMT in heptane, SWIM has let his container sit in a cold water bath for about an hour, then in the refrigerator for 12 hours then in the freezer for another 4-8 hours.
Click to expand...

hmm yes doing it slow I find is the only way to go from yellow to clear...
first of all for this the taller-skinnier the vessel the better....
with heptane I like to use 35ml per gram of spice.
for best insulation to allow the heptane to cool the slowest you will need a mini cooler (i like the gallon sized round ones).
fill the cooler with hot water around 140F. to the level the vessel you are using stands..
place heptane and spice in your vessel and heat up using a hot water bath until all of it is dissolved.
now quickly place your vessel into the cooler so that it's submerged in the hot water and close the lid.
leave at room temp for a couple days,
leave in fridge for a couple days,
now the freezer for a couple days,
during the whole cooling process you want to have the cooler leaned at a 45 degree angle this makes the impurities bunch up better.
once you take it out of the freezer you should see a glob of nasty orange goo on the bottom and clear/white crystals that are very hard and dense on top and all around the sides, they are very easy to scrape away from the gooey mess.

anyways this method is what worked best for me to clean up goopey shit with heptane, never could I just decant at the right moment or such.

however i'm still not to fond as I feel like I always burn spice away from leaving the spice in to hot of heptane for too long. when theres lot's up impurities one MUST go over 140F. to dissolve everything.
well this is what I have found through trial and error hope it helps.
 
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Mr. Kush said:
however i'm still not to fond as I feel like I always burn spice away from leaving the spice in to hot of heptane for too long. when theres lot's up impurities one MUST go over 140F. to dissolve everything.
well this is what I have found through trial and error hope it helps.
Click to expand...

Why not just use a little more solvent at a lower temperature?
 
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Why not just use a little more solvent at a lower temperature?
Click to expand...

not sure if it's possible to get it to solute into the heptane regardless the amount,
other people were useing 25ml a gram,
this is why I stepped up to 35ml per gram,
at 35ml I still had to heat it up to about 155F.
and this was with already pretty clean spice that was from an a/b and had been washed with activated carbon.
going to try 40-45ml next time, just not sure.
 
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What about heating a saturated solvent slowly? If you were to warm your heptane in a hot tap water bath, then add your spice, then move your container with the saturated solvent into a boiling water bath, would that prevent, or help prevent some of the spice from burning away?
 
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my friend does heat his NP solvent slowly,
he gets it to about 100-120F. then adds his spice then continues heating.
it's when your doing a slow cool down and it stays over 140F. for to long that spice burns.
 
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Dmt in shot glass, place in pan. Place second shot glass in pan,
Add small amount of naptha to shot glass,
Add hot water to pan,
Add hot naptha to shotglass with dmt, drop by drop,
Swirl shotglass around decant naptha from the amber goo,
collect in new shot glass and freeze,
pour off naptha(save for reuse) and sit to dry,
place shot glass back into pan,
add hot water to pan,
watch dmt melt,
leave at room temp to dry,
collect dense clean dmt.

This is done after a SC wash.
 
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