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Questions regarding evaporation/black gunk in NaOH/lye mixture Options
 
TruthSeeker
#1 Posted : 5/14/2011 4:53:25 AM
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Hey guys and girls, I have a couple of questions about an extraction that was began that could not be found on the forum. This is a first time extraction.

Here we go- First of all, is it normal for the black gunk of the MHRB/Lye/Water mixture to be stuck to the sides of the jar above the solution before naphtha is added? Will the black gunk be removed from the sides when the naphtha is added and shaken up?

Second of all, when the naphtha is siphoned out of the jar with a turkey baster, can the naphtha sit in a glass pyrex dish outside in the heat to evaporate rather than freeze precipitation? It was planned to go with the freeze precip method, but the jars currently available have a texture that would make it difficult to scrape off the extract.

Thank you! Smile


 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
Skeet
#2 Posted : 5/14/2011 7:28:32 PM

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What form is your MHRB in? From SWIMs experience doing a STB with powdered bark, the base solution softens it and settles to the bottom after it separates into layers. What are you using to hold the solution in?

Also, you want to "swoosh" the base solution around, more then you want to shake. Though I have never had an issue, too much force can form as emulation that can be a pain to settle and layer.

And yes, you can air evap the final product to a useable form. I would still re-xstyl after that of course.
 
TruthSeeker
#3 Posted : 5/14/2011 8:22:23 PM
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The MHRB is powdered form. The black gunk is still on the upper sides of the slightly hourglass shaped pasta sauce jar. Sorry- I actually meant to say that the solution is stirred rather than shaken, as shaking is notorious for causing emulsions. Whenever a turkey baster is purchased, naphtha will be added. Hopefully the black gunk will get off of the sides where the naphtha layer is supposed to be. Next extraction will be completed with freeze precip followed by recrystallization. Thank you for the help! I will keep you updated on the extraction.
 
Skeet
#4 Posted : 5/16/2011 9:11:37 PM

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I would not worry so much, the longer the bark sits in the base solution the better broken down it will be, SWIM swirls his jars around, tilts em left to right, sometimes sings to em, and he gets a little lye/bark in the rim and the lid. Never has been an issue.

If you are using a baster, let me offer some advise that worked for me pre-sep funnel. Baste the solvent out and into a jar/beaker, then with a pipette or a dropper, pull it into your pans/shots for crystallization. Some people have issues with the aq base getting into the solvent, and some don't. Sounds like you are doing a-ok, keep us updated!
 
endlessness
#5 Posted : 5/16/2011 9:18:33 PM

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Its normal, black stuff is sticky. What might happen is when you separate the layers a bit of that black could come across, so do a sodium carbonate wash to get rid of it. Check FAQ for instructions
 
TruthSeeker
#6 Posted : 5/20/2011 4:50:35 PM
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The naphtha has been added, separated, and ALMOST evaporated. Last night the evaporation began and it finally turned into a yellow oil. It is left to evaporate overnight next to the fan. The pyrex dish is checked in the morning and it is still the same yellow oil it was last night! Any suggestions? Maybe put the dish on the stove at the lowest temperature?
 
Skeet
#7 Posted : 5/20/2011 6:14:24 PM

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I could be wrong, but I thought using air current to air evap was generally discouraged to prevent oxidation of the spice?
 
slayed
#8 Posted : 5/21/2011 10:57:09 PM

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Air even with a fan works fine for me, but I wouldnt put it outside in the sun. I tried this once and all I got back was waxy oil.

I wouldnt try using any heat to help it evaporate. Use a wide pan as your evaporating dish with a small fan over it. Surface area and air circulation are key. Evap most of it and then throw it in the freezer, itll snow.
 
TruthSeeker
#9 Posted : 5/22/2011 12:23:16 AM
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Never again will I do a complete evaporation. It turned out to be a very impure brownish oil which wouldn't dry out. It was barely smokeable. I want white spice and nothing else. I will do a freeze precip with a larger amount of bark soon. If anyone could give tips on successful freeze precipitation, please let me know. Thanks!
 
 
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