@ maps, do you own a vaccuum purge?
I dont have a vacum but I'm planning on getting methanol and doing multiple washes as suggested. Hexane is not that toxic in small amounts and you can really pollish your extract.
From
http://skunkpharmresearch.com/
Alcohol/Hexane wash:
One way to clean up an alcohol extraction, is to reduce its volume to a manageable level given your resources, and pour it in a separatory funnel to about the one third level, followed by the same volume of n-Hexane and then of water.
We use an HPLC Reagent grade for this purpose, which we get from the local scientific supply store.
Shake well and then lift the lid long enough to burp any pressure, before setting it in a stand to stratify into layers. After it has separated, bleed off the water and emulsion layer. They contain both the undesirables, and the alcohol as well, with the cannabinoids left with the hexane.
Add water again and repeat the wash step until you are satisfied with the clarity, before evaporating off the hexane, to yield the pristine oil. More on hexane purging in the subsequent process description for serious scrubbing:
To put this process into perspective, I once collected all of my pipe bowl scrapings and roaches until I had about a pint of them, and dumped that into the container of black denatured alcohol, that I had been cleaning my pipes in.
I shook the mixture well and let it soak for a day to extract the material from the roaches and scrapings, before straining it through a wire strainer and then a coffee filter.
Because I didn’t want to mess up a separatory funnel with the black foul smelling mess, I poured the solution in a 1 gallon Ziploc bag, to which I added equal amounts of water and hexane.
After shaking it well, I hung it from one corner, to let it stratify, and after it had, I clipped off the lower corner of the Ziploc bag, and by pinching it, and controlling the bleed rate, I was able to bleed off the water, alcohol, and emulsion layer, so that only the now gold hexane solution remained.
I filtered the hexane and poured that into a Pyrex pie plate, which I blew air over with a fan to evaporate off. Attached are pictures of the amber oil that I extracted.
While the black color was gone, slight ashtray undertones could still be tasted, so further refining was necessary with activated charcoal, but we will cover that as a separate subject.
I am not suggesting this process for reclaiming ashtrays, but simply to make a point.
Hexane/Saline water wash:
Joe came up with this process, which has produced our most pristine creations. It involves re-dissolving the oil in a hot highly non-polar solvent such as hexane and repeatedly washing the solution with saturated salt water until it is mint quality.
Salt water washing uses a separatory funnel as above, but we start out dissolving the extraction to be cleaned directly into hot n-Hexane, and then washing the hexane solution with saturated salt water.
The magic trick is two fold. The saline exposes any proteins hydrophobic surfaces, making them insoluble in water, so that they precipitate out, and the saturated water has no room for anything but the alcohol, which aids that process.
We start out by making four or five liters of saturated salt water in a glass (or ceramic) container, by mixing sodium chloride (table salt) in hot tap water with a hand mixer until no more will dissolve. We buy the salt cheap by the bag, using salt intended for water softener use.
We perform the salt water wash of the hexane mixture, by simply pouring the salt water and hexane into the separatory funnel together in about equal parts and shaking well and burping, before allowing the mixture to separate out into layers.
After carefully bleeding off the bottom layer of water, we continue to replace it and repeat the wash process of both the emulsion layer and the hexane solution, until the emulsion layer disappears and the hexane has bell clear clarity.
At that point we stop washing and evaporate off the hexane. While we use HPLC grade hexane, light naphtha containing only Pentane & Hexane will also work for this process. Check the MSDS because the word light naphtha only means it boils between 30C and 100C, so it can contain Benzene..
Purging Hexane:
While n-Hexane is a delightfully non polar solvent, that enables us to do some amazing things, it has two more carbons and four more hydrogen atoms in the chain than Butane, and so due to the greater Van der Waal forces involved, is not as easy to get rid of as Butane.
The most effective way that we’ve found to remove the residual hexane, is either with multiple ethanol washes, usually around three, or thin film vacuum.
To wash with ethanol, redissolve the hexane honey oil in ethanol at a ration of about 10 to one and boil off the alcohol. When it is almost all gone, do it again, and repeat, until there is no decernable hexane odor.
For thin film evaporation, we place about .200 inch of it in a six inch Petri dish, which we place in a vacuum chamber and evacuate down to 29.5 mm Hg and ~80F for 30 minutes.
N-Hexane boils at about 69 °C/ 156 °F and has a high vapor pressure, so it is easy to evaporate, but harder to completely purge. Given our 30ppm taste sensory threshold and our 130 ppm odor threshold, we can detect its presence, long before we reach levels of concern.
Because it is a simple Alkane and relatively non toxic, hexane is used extensively in food extraction, but should not be viewed as being as salubrious as mother’s milk.