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Need some help freeing the spice from solvent please... Options
 
merkin
#1 Posted : 7/20/2017 10:14:09 AM

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Hi, I'm starting a new thread for simplicity and clarity but this is an ongoing problem plaguing me (see this thread for other pix)

I currently have a tray in the freezer (photo attached) which is full of spice. Problem is this: it has always worked like this, get spice in freezer, as I decant etc, it either stays with the solvent or very soon the mushy crystal pile disappears back into liquid solvent. Sometimes I manage to keep some of it on filter paper - anything handy - and I get the crystals in the lower pic. They come out quite light and mushy like a pile of slush puppy (see that linked thread for pics) - but before they dry they dissolve back into liquid -- more than half is lost every time.

No ways I can dry it in glass or even put upside down in freezer - it always goes. What doesnt happen to stay on the filters is lost. If I evaporate the naphtha, every single time I get oil/goo.

How best can I get these lovely guys out of the naphtha? I know the naphtha is not ideal and I have other solvents now to try, but given all that beauty in there - is there a way to get it out mostly as crystals?

It is definitely a heavy naphtha (not sold under that name here in my country no-one has heard of naphtha) but it extracts like a champ - unfortunately takes ages in freezer to get to this and weeks to evaporate. I just can't seem to get at the spice in there. In the freezer it was clear for 3 solid days, then today (4.5 days) it is suddenly full of crystals.

The pic isn't that clear thanks to the shrinkwrap cover but there's all that suff, sorta coherent but swimming in the yellow naphtha.

How can I best get these crystals? Is there a process to somehow get them into something less "clingy" that will maybe precip better than this naphtha - but without losing what I got?

Would really appreciate advice cos this is where I am failing every time. Naphtha definitely seems to be the reason so its the area I need to work on. MHRB is excellent (that's pull 1-3 out of 6) - already got 400+mg out of 4-6 and lost a LOT of that in the same decant process. Too scared to touch this at the moment but it doesnt help just sitting in the freezer like that!

It feels soooo close...! Much frustration
merkin attached the following image(s):
trapped spice.jpg (203kb) downloaded 111 time(s).
 

Live plants. Sustainable, ethically sourced, native American owned.
 
Ulim
#2 Posted : 7/20/2017 12:28:44 PM

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Seems like your freezer isnt cold enough.
Also why are you unable to pour off all the naptha without pouring away the crystals?
 
blue.magic
#3 Posted : 7/20/2017 3:30:36 PM

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Another problem may be the container heats up too quickly. I use pyrex dish with fairly thick glass so it stays cold for a while after moving it out of the freezer. My freezer is -18 C.
 
merkin
#4 Posted : 7/20/2017 4:00:55 PM

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These are lids of pyrex dishes. Here is what it looks like out the freezer with some naphtha decanted. If you touch it its mushy and will slowly return to liquid standing out.

As for pouring it, it seems the naphtha is embedded in that entire crystal structure?

merkin attached the following image(s):
outthefreezer.JPG (174kb) downloaded 83 time(s).
 
urtica
#5 Posted : 7/20/2017 5:55:51 PM

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I think you either have some water in your final product or LOTS of plant oils still in your final product. Are you doing an STB? Maybe try doing a mini A/B to clean it up?
urtica is a fictional character. nothing written by this fictional character has anything to do with reality. if urtica was real, and performing any activities that are restricted by certain governmental forces, these activities would be performed in Heaven where nothing is true & everything is permitted.
 
urtica
#6 Posted : 7/20/2017 6:09:26 PM

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OK I looked though your thread. You say that getting lab solvents is not a problem? Get some straight heptane or something like that & see what happens.
urtica is a fictional character. nothing written by this fictional character has anything to do with reality. if urtica was real, and performing any activities that are restricted by certain governmental forces, these activities would be performed in Heaven where nothing is true & everything is permitted.
 
Ulim
#7 Posted : 7/20/2017 8:17:30 PM

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merkin
#8 Posted : 7/20/2017 10:54:35 PM

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Hi urtica. I have some n-heptane now. Should I just dissolve all of that icy conglomerate in the heptane and begin the freezer stage again? At present it is upside down in the freezer. A good chunk fell into the lid underneath abut most is still sticking to the top lid. Its obviously still full of the naphtha but the frozen structure seems to prevent it drying out like that.

(yes, stb - noman's tek)
 
merkin
#9 Posted : 7/27/2017 2:32:29 PM

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Okay well that didn't go anywhere! Didn't really know what to do so I tried a "mini A/B". Ended up with absolutely nothing in any extraction! No precipitation whatsoever this time, just a big waste of time and energy. Only bit I got was a portion of that huge amount that redissolved to dry so only managed to keep about 80mg of yellowy white powder. Second time I've tried a "mini A/B" and got absolutely zero result. The solvent was nice and dark and there was definitely a lot of material there that I couldn't free from the naphtha but that I know existed because it was both visible and I actually was able to dry a little bit on a filter paper. Not very encouraging


*edit* Honestly, the principal problem I always had was solvents. Because there is no product called "Naphtha" here it was a bit of a crapshoot. Trying this and that, reading MSDS's etc. Once I gave up on finding "naphtha" mentioned I tried some easily available local options and eventually got all back on track and consistent pull after pull. After going on a testing binge to find a suitable locally available solvent for freeze precip I am now happy with one cheap and easily available stuff called "Benzine" here and have none of these problems above any more!
Results of that at the end of this thread - may be of use to Saffas Smile - https://www.dmt-nexus.me...aspx?g=posts&t=74000
 
 
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