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Weird sediment during freeze precipitation? Options
 
topfbrauten
#1 Posted : 3/14/2010 7:03:36 PM
SWIM decided to use Noman's tek to extract from powdered MHRB, and it's not turning out so well... This odd off white (almost flesh tone) rock hard ice like substance formed in the bottom of the container, and it melts if removed from the jar. Is this normal? Also, there's been no crystal formation whatsoever even after 20 hours.

Any words of wisdom for SWIM?

Thanks!

PS: maybe SWIM's measurements were wrong? Used 750ml of water and 50g of crystal lye, and 50ml of Naptha per extraction.
 
random
#2 Posted : 3/14/2010 7:42:59 PM
i really can;t offer any advice on that TEK as neither myself nor SWIM has used it or seen it done Sad i can however give you some small advice for your next attempt. seek out some pickling lime (can get it from amazon.com) and follow q21's vinegar/lime A/B. SWIM can;t stress enough how easy it was, and how great his yield was. best of luck to SWIY for fixing this batch though, i keep reading that even if you make a mistake somewhere along the line, that you can most likely get the goodies out eventually..so don;t throw it out! i'm sure someone here will help you out eventually...everyone here is extremely helpful, and alot of the folks here are very experienced Smile
 
The Wizard
Chemical expertSenior Member
#3 Posted : 3/15/2010 12:22:52 AM
perhaps its water?
 
Jumper
#4 Posted : 3/15/2010 4:22:24 AM
Swim had something similar happen once. It turned out to be water. How it got in there I don't know. As far as the sediment goes, it could be lye, so do a sodium carb wash on the naptha to be safe.
Disclaimer: All words and images posted herein under the username Jumper are strictly for entertainment purposes only, and are fictitious in nature. Swim is the imaginary character of a schizophrenic and all posts connected to said entity are the deluded ramblings of a madman, who admits that all posted data herein was electromagnetically beamed into his brain from a HAARP antenna array.
 
mogascreeta
#5 Posted : 3/15/2010 5:50:56 AM
topfbrauten wrote:
SWIM decided to use Noman's tek to extract from powdered MHRB, and it's not turning out so well... This odd off white (almost flesh tone) rock hard ice like substance formed in the bottom of the container, and it melts if removed from the jar. Is this normal? Also, there's been no crystal formation whatsoever even after 20 hours.

Any words of wisdom for SWIM?

Thanks!

PS: maybe SWIM's measurements were wrong? Used 750ml of water and 50g of crystal lye, and 50ml of Naptha per extraction.

If at first you don't succeed, try try again
"I'm creeping back to life, my nervous system all awry, I'm wearing the inside out. Look at him now, he's paler somehow, but he's coming round. He's starting to choke It's been so long since he spoke, well he can have the words right from my mouth. And with these words I can see, clear through the clouds that covered me, Just give it time then speak my name. now we can hear ourselves again" Pink Floyd- Wearing the Inside Out
Mogascreeta is a pathological liar and should not be taken seriously under any circumstance.
 
alicedee25
#6 Posted : 3/15/2010 5:59:10 AM
when swim did their first extraction they used saran wrap to cover, this caused little whiteish ice chucks in the solvent. Check the pH and make sure its 12-13. if not add more lye. heat some water and add your solvent vessel to it away from flame. Repull and precipitate with an airtight lid with one wasnt used. Also how much material was used to start with?
 
topfbrauten
#7 Posted : 3/15/2010 1:32:58 PM
SWIM used 50 g of MHRB powder in his mix. The largeish chunks have broken apart and are chilling in the bottom :/

Maybe they are water? SWIM is gonna let it precipitate for 48 hours, does that sound right? And when done SWIM should drain out the naptha then scrape out the crystals or othr way around the filter?

Many thanks from SWIM!
 
topfbrauten
#8 Posted : 3/15/2010 4:54:58 PM
SWIM took the jar out of the freezer and found no elf spice crystals whatsoever, just a bunch of the odd off white chunks. They melted when placed on a coffee filter. Also, all that was left on the filter was an oily residue, and the only thing left on the walls of the freezed container was a similar thicker oily residue. SWIM is very very confused... Did SWIM calculate something wrong? The oil did nothing when smoked, it just crackled.

Also, a second batch was being air evaporated and it left a similar oily residue.
 
endlessness
Moderator
#9 Posted : 3/15/2010 5:10:36 PM
did you do an evap test in your solvent before using it, to see if it leaves residues?

maybe try redissolving in minimal amount of warm naphtha and into the freezer again
 
dtabbler
#10 Posted : 3/15/2010 5:33:30 PM
pictures of course would help greatly to me, swim has always done a basic nomans tek with great results and ease so i can offer some assistance i hope!

when swiy pulls the naptha off the top, make sure not to get any of the second layer. go straight into a cassarole dish or something similar, and put it in the freezer uncovered for approx 2 hours.

DO THIS STEP QUICKL!
after 2-3 hours or so have gone by, pull dish out of freezer and pour naptha out into another dish, there should be a whole bunch o whitish crystals stuck to the bottom of the casserole dish. IMMEDIATELY cover the casserole dish with the crystals in it with saran wrap and lean it up on one side so any leftover naptha goes to one end and you can easily pour it off. dont uncover until the dish feels like its room temp!

my guess is the odd stuff is water. personally i would just let the whole darn thing naturally evaporate at room temperature, add some warm naptha after thats done and re-freeze precip. a sodium carbonate wash is great if you happen to have some laying around, but i assume you probably dont!

also you'll want to skip the ammonia wash in nomans tek and do a recrystal a few times.

a/b teks are too much unnecessary work for swim. his nomans style tek works well and ends a short evening with a whole bunch o smokable spice
Who's this SWIM person and when do I get to meet them? They sound friken cool!
 
DeMenTed
#11 Posted : 3/15/2010 5:39:13 PM
I would pour off the naptha and wash that with sodium carbonate and refreeze, the chunks that are left from pouring off the naptha should be left on an evaporating dish untill no moisture is present, the dmt will appear once its completely dry.
 
topfbrauten
#12 Posted : 3/15/2010 5:42:48 PM
What exactly is an evap test?

And SWIM is going to try again with the leftover Naptha
 
alicedee25
#13 Posted : 3/15/2010 6:08:31 PM
topfbrauten wrote:
What exactly is an evap test?

And SWIM is going to try again with the leftover Naptha


Take a small amount of naptha from the can and place it out to evaporate. If any oils or residues remain your solvent is impure. These impurities will collect on the dmt and also make it oily and hard to crystalize.
 
topfbrauten
#14 Posted : 3/15/2010 6:51:56 PM
Ahhh ok. Well SWIM decided to just eff it and make another batch hahahaha, maybe too much of something was put in. This time SWIM put in 20 MG of powder and re-measured everything else accordingly.
 
topfbrauten
#15 Posted : 3/15/2010 8:50:39 PM
SWIM put the 20 ml of Naptha in a little glass butter dish thing, and sure enough, there's a whole bunch of tiny little white crystals!!!

SWIM would like to re-crystalize, but SWIM doesn't quite understand how to do it. The Noman's tek is a little unclear... Any tips?
 
corridors of my cells
#16 Posted : 3/15/2010 9:06:57 PM
It should be water.. happened to me 2 times before..
 
topfbrauten
#17 Posted : 3/15/2010 10:20:45 PM
Well SWIM got his crystals, but theres still some naptha? in the container around the crystals. Should the container be left alone so the stuff can evaporate?
 
topfbrauten
#18 Posted : 3/17/2010 8:47:55 PM
SWIM is getting MAJOR crystals now Very happy

Thanks dtabbler!
 
mumbles
#19 Posted : 3/18/2010 1:07:38 AM
Use some alfoil and a rubber band to keep moisture out of your freeze precip dish. Having that ice melt and run through your new crystals and ruining them isn't much fun. Oh and don't evap the naptha off completely unless you have a thing for smoking plant oils and other shit.
 
 
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