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What is going wrong with this STB xtract? Options
 
GonePhishin54
#1 Posted : 10/8/2009 1:18:44 AM
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SWIM is having a lot of trouble doing a not so troubling STB extraction.

He is ending up with a waxy sticky substance that smears when he tries to scrape it out (instead of collecting together) but still smells like spice

Here was his procedure

200g powdered MHRB

He slowly mixed 200g of 100% lye (Rooto) into 5 cups of distilled water in a stainless steel stewing pot

Then mixed this solution with the 200g of powdered MHRB in a tall skinny glass vase (so the naptha layer would be thick without being a lot of naptha)

He stirred and broke up the clumped mimosa then added roughly 1 cup of naptha, stirred, and let sit for 30 minutes

Then he made his first pull and got none of the dark layer, he put that into a pyrex dish and put it in a very cold freezer.

He then added another half cup of naptha, stirred and let sit for 30 minutes (lye and water was still warm when more naptha was added) then made his second pull, not getting any dark layer material, he put this into a different pyrex dish and let that sit in the very cold freezer.

these both at over night, in the morning he could see a few small white crystals had formed and there was somewhat of a thick layer on the bottom of the dish (assumed to be much much smaller crystals). the naptha had some crystals floating in it, but it was never yellow, always clear or maybe a little foggy, he dumped this naptha out and allowed it to dry (i live in colorado and the air is very dry, evaporation happens quickly) it just turned out stick, not able to scrape up, a friend suggested to him to add clean naptha to the dish and re freeze.

whats going on here? please help!!!!
 

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soulfood
#2 Posted : 10/8/2009 1:23:13 AM

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Is it possible that water got into the freezing vessel by condensation or other means?

If not, just redesolve in minimal naphtha and refreeze.
 
geeg30
#3 Posted : 10/8/2009 1:26:55 AM

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Sounds like your getting Oxides forming but then again it could be a variety of things.

What type of Naptha are you using - light or heavy? How much water are you using? Is it old MHRB? have you tried a better solvent?

It might be that you just find that your bark is bunk. A bit more experimenting is required.

Here you!!! Gonnaenodaethat

"Iceberg???? - What Iceberg????"
 
GonePhishin54
#4 Posted : 10/8/2009 2:02:42 AM
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SWIM used 5 cups of water, using VM&P Naptha from hardware store, bark is from celestial source, out of portland oregon. isnt there condensation in all freezers? he does smell spice so i know the bark isnt completely bunk, i don't know how long they (celestial source) had it for though.

really hope there's a solution to this, SWIM added new naptha to the dish and its currently in the freezer
 
GonePhishin54
#5 Posted : 10/8/2009 2:25:18 AM
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is this a common problem? and how long does he let it sit in the freezer for the second time?
 
geeg30
#6 Posted : 10/8/2009 2:32:30 AM

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5 cups?? around about a litre, a litre and a half??

For 200g you should be using around 3000ml of water, your naptha is fine - swim uses VM&P, bark source - never used them. As for freezer condensation, its only a consideration when your vessel contents are exposed to air - depending on the humidity really.

Add some more water to your mimosa (if you not around 3000ml) and heat up your naptha a wee bit and add to your mimosa, mix well every now and again for a good few hours at least and then try anothe freeze precip. You should see something starting in a couple of hours, swim leaves his freeze precip for at least two days in the freezer - its amazing just how much crystal will form after the first day in the freezer.
Here you!!! Gonnaenodaethat

"Iceberg???? - What Iceberg????"
 
GonePhishin54
#7 Posted : 10/8/2009 2:44:36 AM
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wow, so SWIM was using about half of that, so would you say there is still a lot of spice in the MH? should he say screw what he has going on now and do all new pulls with more water?
 
GonePhishin54
#8 Posted : 10/8/2009 2:48:34 AM
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basically asking, should he discard the 2 he has in the freezer and put new pulls into them? will adding more water get rid of this waxy substance or is his bark to fatty?
 
GonePhishin54
#9 Posted : 10/8/2009 2:56:54 AM
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and what would be a better solvent for STB? SWIM thanks you very much for your advice
 
geeg30
#10 Posted : 10/9/2009 1:09:11 AM

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Stick some more water in and then add some fresh naptha, maybe using 100 to 150ml - shake every now and again and then extract the naptha after say 6 hours and then freeze precip. Then compare the results with the freeze precip you already have, if its a good result then try recrystallizing your previous wax, if not a good result then it would seem you have bunk bark

VM&P naptha is very good for getting DMT and a bit of oxides as well, so if it is just these compounds you are after keep using the naptha otherwise use DCM, Limonene, xylene etc. D Limonene is about the safest to use but tends to not evap too good nor can it be used in freeze precips. There are a few teks out there for limonene.
Here you!!! Gonnaenodaethat

"Iceberg???? - What Iceberg????"
 
GonePhishin54
#11 Posted : 10/10/2009 2:33:36 AM
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i added more naptha to my pyrex dish, refroze over night and no result, ill try adding the extra 1500ml of water, my water/bark/lye solution is still good right?
 
geeg30
#12 Posted : 10/10/2009 10:09:35 PM

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Your solution will be fine for ages (that's if there is any spice in it). Swim has used solutions for over a month with no problems.

Anyway - add 1500ml of water and then add 150 ml of warm naptha and freeze precip. If you have still nothing try one of the other solvents. If there is still nothing then I would have to put it down to bunk Mimosa.

Is your lye mix black and thick (syrupy)?
Here you!!! Gonnaenodaethat

"Iceberg???? - What Iceberg????"
 
GonePhishin54
#13 Posted : 10/11/2009 7:22:23 PM
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yeah its black and sludgy
 
geeg30
#14 Posted : 10/12/2009 6:23:41 PM

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I say go for it and add more water, warm naptha (not too warm say 40C), mix for a few hours, remove naptha and freeze precip (or evap). If you still have nothing then I would say bunk bark - although you could try different solvent just incase your bark has mostly oxide and jungle spice.

Good luck
Here you!!! Gonnaenodaethat

"Iceberg???? - What Iceberg????"
 
GonePhishin54
#15 Posted : 10/12/2009 9:13:39 PM
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finally! SWIM added 1500ml of distilled water and warm naptha and freeze preciped over night. SWIM is now seeing lots of small/medium sized crystals forming with a lot of crystals still floating.

whats the best way to dry?
 
geeg30
#16 Posted : 10/13/2009 8:42:16 PM

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Swim finds that freeze preciping for a few days is best, best way to dry is to pour of naptha (through a filter if necessary), reheat the naptha and reuse. Blow a small fan over your pyrex dish or even just blow over it yourself to evap the remaing naptha. Any spice on your filter can be scraped off - if you want the tiny remainder from the filter you can pour fresh warm naptha through your filter or even acetone etc.

Swim's method is to freeze precip in 250ml plastic bottles and then pour off naptha (filter if necessary) and then pour small amount of acetone into the bottle to dissolve the spice. Evap the acetone for a crystal wonderland. Acetone is best used Anhydrous

Enjoy your spicyness
Here you!!! Gonnaenodaethat

"Iceberg???? - What Iceberg????"
 
 
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