Cryo hexane crude

Ok some ok clippings 6 months old
Brought to cryo temps -80C some n-hexane also -80C
150g biomass in Buchner and 2.5 liter solvent (I know way to much )
Came out looking ok @Kingofthekush420 :upside_down_face:
Bored as I am I made a colum with
Botom to top
Celine,b80,activated alumina , ground to powder x13
Well something is catching colors and it looks like it’s x13


O by the way this is not a joke :grin:

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Yes I will start a cold evap in a while
Yurt started the chiller
Wonder is any cannabinoids in there :joy::joy::joy:

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Ok so next would be nice if any chemist can chime in on this
@krative @photon_noir @richpel @anon93688
Hexane has a very low scent threshold 30 ppm
And boiling it of even with vacuum is a pain
So I plan on doing a LLE with methanol
To get the cannabinoids in methanol
Wich has a easier scent treshhold
But I can t see the diffrance :joy::joy::joy::joy:
Wich colorant can I ad to hexane to see what’s happening :joy:
Damn it s water clear

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You can use a TLC plate and either a UV lamp or iodine stain to keep track of what is in your hexanes or methanol.

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UV it is got that right here thx

Alumina catches a lot of junk from plant matter. I used to teach undergrads how to separate chlorophyll and the different carotenoids from spinach using alumina.

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I wonder what x13 sieves do in the head of an spd ? :grin::thinking:

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I’m going to start cryo heptane extracting and skipping winterization, I’m 95%sure with hot condenser tech I can eliminate any fats and lipids that are pulled at low temp with heptane.

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Why do you want to liquid liquid?

I’d run that clear how it is to see what you make.

You’ll be able to tell if theres fats and lipids in there

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Definatly the x13 taking most of whatever out added some extra afraid it would get saturated
You can see new bands above the first load


O a trick of the trade instead of a sep funnel dripping in the column I placed a funnel with some teflon tape :joy::joy:

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The LLE is for the winterizing
And wonder if I can get rid of the scent of hexane so that shatter and the rest are options

Throw a little ethanol in there once you’ve purged it, its food grade and the ethanol will push any hexane out before it boils since the hexane has a lower boiling point

I’d use heptane over hexane

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Hmmm I work with hex a lot and it takes up to 3 boils to get below scent treshhold same recipe good old gray wolf has from skunk farm

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Ok so the test from yesterday gave a very pale light yellow oil but a very very low yield
My contact time with the biomass was also very short so tried again today
This time 250gr in 5 liter hex soaking for 30 min at -80C
What came out was green as the grinch
Hmmm not used to so green ???
Any way to make mattters worse
I set up a Buchner with 1/2 " layer of x13 and 1/2 of activated alumina and ran the frees stuk treu
Almost no color change so I decided to place 1/2 inch layer on top of the 2 already in the Buchner of B80
O my the damn green grinch got almost dark dark green
So I call it a day tomorrow again
I will check ph of both samples see if any has changed can t find a damn booklet :angry: Of litmus paper

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Welcome to research, where half the shit is irreproducible and most things are made up but still work.

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Very very very low yield is probably due to the fact that 13x’s pore sizes will include cannabinoids.

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Color change to green was probably due to you letting the hexane evaporate from the plant mass after the initial extraction. It probably got warm and pulled the chlorophyll to the outside of the plant material as it vaporized. Then when u re-washed with hexane the chlorophyll was soaked all throughout the material and was easily extracted.

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Agreed, are you sure the temp stayed below -72c?

I wonder if you’re biomass is colder than your hydro carbon if itll melt fats and lipids /maybe pull some chloraphyll like butane will if the solvent is warmer than the material

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Nice experiments, @Roguelab ! Just keep track of your variables, one at a time!

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