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First Extraction Options
 
babyslate08
#1 Posted : 11/9/2012 2:46:25 PM
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So SWIM did his first ever extraction (STB) and everything went well up until the freeze precipitate. After around 72 hours in the freezer SWIM isn't seeing any crystals forming. Instead what is seen looks like a stringy mess settling to the bottom of each container. When attempting to pour off the excess solvent for drying, the precipitate at the bottom readily redissolves into the Naptha.

For informational purposes, SWIM's tek went as follows:



SWIM isn't sure what went wrong or why crystals aren't forming. Could seeding possibly be the solution?

Any help would be appreciated.
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somethingsintheway
#2 Posted : 11/9/2012 8:13:05 PM

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For a first timer you should have started out much smaller, with like 100g of MHRB. 400ml seems like a lot of napthpa to me, I've never used that amount. For one, the dmt in the naptha has to be concentrated for it to fall out of solution. So less naptha, plus more dmt in that naptha would have a better result. 4 pulls and then combined? I do one pull at a time in the freezer and usually have 500mg+ within 6 hours of freezing. My advice to you is to slow the f down. I'm sure you could save it just use half the naptha maybe and see what happens, make sure you are getting clear naptha when you are about to freeze it. Forget about the epsom salt and the cold water wash. 72 hours? If you don't see crystals forming in the first 4 hours you screwed it up.
 
ipumaestro
#3 Posted : 11/10/2012 12:16:57 AM

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step 1, evaporated naptha to half its quantity

step 2, try freeze precip again

if this dosent work, attempt salting with an acid of your choice

best of luck, and yes next time master a micro extraction before scaling up, we cant afford to squander our precious resources
achuma puma
 
Binary Drool
#4 Posted : 11/11/2012 2:04:15 AM

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Who is SWIM?... Why are you using plastic? In any event let 50% of your solvent evaporate then freeze prep again. I would be nervous letting a solvent sit in plastic for 72 hours. That stringy mess settling to the bottom could be plastic.

Be careful! Good luck!
We actually worship incomprehensibility as the highest form of explanation. ~TM
 
shardymarty
#5 Posted : 11/11/2012 3:01:39 AM

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NOO!! never ever put solvent in plastic!!! it will bond with and dissolve some (or all) of the plastic and create dioxins in your final product or just eat through the plastic and drip everywhere. i reccomend a small glass round pyrex freezer jar for EACH pull. you used a lot of solvent and a lot of NaOH. i reccomend 100ml of solvent per pull and less lye. no need for magnesium sulfate either. oh ps binary swim means, someone who isnt me.
 
babyslate08
#6 Posted : 11/11/2012 10:04:34 AM
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Thanks for the suggestions guys. Evaporating off 50% seems to have done the trick. And as for the plastics, the tek SWIM read said it was okay since Naptha is comprised of aliphatic hydrocarbons as opposed to aromatic. However, after further research it does seem as though HDPE and Naptha aren't a good combination. Switching to pyrex for future extractions.
 
 
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