Pentane is a bit harder to work with and it likes to evaporate around room temp so its a lot more dangerous to work with especially during LLE.
Stick with Heptane 1st or hexane 2nd.
Organic Layer
3-4:1
Solvent:oil
Aqueous Layer
Use the same volume of water as your oil dissolved in solvent.
I measured out 100 grams of crude.
Dissolved in 100ml of ethanol.
Added 200ml of Pentane (will switch to heptane)
Added 150ml brine water.
Agitated and let seperate.
@thesk8nmidget how does that sound to you?
No need to use ethanol next time as its easier to dispose of an aqueous layer that doesnât have solvent in it.
Use heptane first to dissolve the oil and increase the solvent to oil ratio to around 3 or 4:1 and use an equal amount of water.
While you have the oil in solution it may be a good idea to do a few washes at different ph levels to pull more impurities out and give abetter looking and better testing product. Just ensure the final wash is with a ph of 7 (bottled water is usually around 6)
Right on! Thank you. That will absolutely help streamline this process.
How long does the seperatation usually take? Iâve got a good bit of junk out but itâs taking quite a while. Approximately 4 hours to seperate 500ml of crude.
Actually he was onto something, By mixing in the ethanol. except u need to add more water to louch out the cannabinoids into the heptane layer.
By adding in ethanol your allowing the polar contaminants to attract to the aqueos layer better. Then u need to dilutr out the ethanol with water to get the cannabinoids to louch into heptane. Then filter cleaned heptane layer over AA to remediate thr caratenoids. I like to drip the aqueos layer thru a tall column of heptane with a sept funnel below. So ur essentially letting the aqueous layer drip thru another set of heptane to make sure u arent dumping any goodies along with the aqueous layer. I suggest using 3 parts water to 1 part ethanol to louch.
Just figured this out a couple days ago, so still figuring out whats best but i took brown ethanol looking extract and turned it into a light amber shatter without using roto or even doing ph swings on water washes, just louch and drip.
Still gathering data and pics and ill do a write up soon
Does my time seem right? It takes about 3-4 hours to fully seperate?
Mine took 10 min
I figured it should have been quicker. I wonder if its due to the sheer amount of junk in this crude or if the ethanol speeds it up?
Cuz ur ethanol is still holding onto the cannabinoids, its fighting with the heptane.
Add in 300ml water. Agitate and let settle again. The aqueous later is gonna be opaque white like
This morning I changed to @thesk8nmidget suggestion above.
I disolved 500ml of crude to 1500ml of Pentane. (Since thatâs all I have currently) then added water and agitated.
And its not seperating? Meaning theres a fat middle emulsion layer or the whole thing is still emulsified and wont create layers?
Itâs taking forever to seperate and there is a huge center layer
Dump it into a seperate container and keep working on the top pentane layer. Dont wait on the emulsion layer, dump it into its own vessel and keep working on it there. Most of the time its full of junk anyways
It takes forever for the Pentane to reach the top is the problem. I feel like alot of my Pentane is still in the emulsion layer.
I still canât get my head wrapped around why yours took 10 minutes and mine is taking hours to seperate.
You can try adding a few drops/squirts of ethanol to quickly break an emulsion into distinct organic and aqueous phases.
Also maybe try some salt (if youâre not using it already) to break the emulsion
make sure its non iodine salt. but it works great for making it not foam up
Washing with saturated brine is less prone to emulsions since itâs more dense than water by itself. Adding ethanol, just a little, decreases the surface tension breaking the emulsion. Depending on how clean the extract is, there could be some insoluble crud - waxes, etc. at the interface of the organic and aqueous layers that can be filtered off.
