Hey folks! Just wanted to say a big thank you to this wonderful resource, it’s put me months if not years ahead of where I would’ve been unaided.
I had a question surrounding the following procedure
“Take some rubbing alcohol at 70/30 isopropyl alcohol to water and put your compound into it. Then bring the solution to a low boil and boil the compound. As you boil the isopropyl alcohol will deplete and water will become dominant. You will see then that the oil is mostly just rolling around in water. The water will be milk white if terpenes are present. Isopropyl alcohol forms an azeotrope with water so will not be boiled away completely. This water and alcohol will swell the gunk including the green chlorophyll stuff. Furthermore there is a bunch of DNA that gets extracted as a rule and is lumped into a category called “waxes”. Isopropyl alcohol is the only alcohol that will not disolve those DNA strands (long and spindly white gunk) and it is for this reason that labs analyzing DNA use isopropyl alcohol to recover DNA. So the bonus here too is that any DNA if present (there is a lot present in crude). All alcohols will densture DNA (it unwinds the helix strand of the DNA) but only isopropyl alcohol will leave them alone and undisolved so they can be then filtered as described.Then redisolve it all in 70/30 rubbing alcohol at room temp.”
Has anyone done this before?
I read on another thread that you need to do this process at cryo temps for best results, and somewhere else said re-dissolve into ethanol and then cryo pull.
Does anyone have any experience with or without the extra cold step?
Those words are mine though I am not sure where I typed them. Any more I only post on IG or here.
After you boil the compound in iso a cryo bath does indeed help when you go to filter. However if any other solvent is present then I have had problems capturing all the gunk and green. The trick is to use iso that is cut with water by at least 10% or so so it is not as good at disolving stuff. Then chill and pull through alumina. Pure iso or any other solvent is a little too good at solvating the gums and green stuff and will pull especially the green right on through the alumina. It is a delicate operation this way and pre chilling the filter as well as prewetting the filter with water will help. However prewetting only lasts so long as does pre chilling.
I prechill by just cooling some iso and water mix along with the solvent and compound then use the clean iso and water to chill the filter and then as a wash through in the end. The gunk seems to want to freeze out of solution somewhere just colder than -60°C and when the iso is cut 10% with water it too will get slushy at about that temp. Keep in mind that this can be done at room temp too and if careful in making sure there is plenty of water in the iso then I have caught up significant enough green to definately be worthwhile. As I recall I once used 70/30 iso off the shelf as rubbing alcohol and this did the trick at room temp.
That sounds right except I add the water before using the iso. Also consider 10% water to be a mininimum really but in a cryogenic environment more water will freeze up the solvent quicker. You will likely find a better ratio and I myself am trying to find the right combo of cryo filter and iso to water ratio since I am trying to do two things with one step. If I only proceeded first at a room temp operation and filter and then proceed with winterization I suspect the extract would be much cleaner to start.
The cold treatment winterizes and also removes a great deal of the slimy waxes and gunk but again if done at room temp with enough water mixed in it can be fairly thorough on its own without chilling. Done at very cold temps it sure seems to grab just about anything related to waxes but the green removal is best done with a slightly higher ratio of water to iso in my experience.
From what I’ve read traditionally winterization is done with a 10:1 solvent to oleoresin. Is doing it with a minimal amount of iso then chilling it down to -60 going to drop out cannabanoids as well? Do I need winterize the extract beforehand? (I’m just doing a -15c ethanol pull so there are moderate waxes present).
I gotta be honest here insofar as my submersion chiller is new to me in this process. You kicked my gray matter into gear frankly and thanks. I realized as I pondered your response that my tech has gotten more sophisticated and lo and behold I have strayed away from the old tried and true tehcniques used for a very long time.
Sometimes it takes a kick in the head to see the boot in front of the face lol. I believe after thinking on it, and medicating a bit lol, that my error is in trying to nail it down in one process. Arrogance from the compliments and such clouded the intellect. I do believe that next month I will run the stuff just as I did prior to my chiller. Then after that I will proceed to winterize. I often have difficulty translating the images I have in my head into explanations. I remember now how delighted I was at the simplicity of my old boil it in alcohol, dump off the water, then redisolve in rubbing alcohol (70/30) and pulling through alumina was. I introduced problems by trying to combine the two because I had to get higher purity to withstand the freeze but then was blinded a bit that a key feature (green removal) was all that more complex in trying to figure out ratios.
Trying to hit a grand slam and I kept hitting foul balls lol. Sincerely thanks for bringing this up because I had been a bit stumped how to proceed to improve this and the answer seems to be a fall back to the old room temp style THEN on to a cryogenic bath to grab the gums and scums left over.
Don’t get me wrong at all; feel free to heap lavish praise on my methods as you see fit. My head still fits through the door so a little inflation is still ok… I will likely revisit several issues over this for a simple reason - I was easily dealing with some of the refinement using low tech and simple but as I tried to reduce steps I have added challenges not yet solved really. Somewhere in between is a happy medium. I do have a thermostat on my chiller (many are full on or full off) so I could dial in a much higher temp and accomodate then a higher water to iso ratio.
Isn’t it always the case that procedures born out of a best-I-have-to-work-with situation can produce as good or better solutions than throwing equipment at the problem? The chiller is a game changer for sure and I love the wax removal it can do but I will need more time to dial it in. A year or two and I will have this stuff nailed down.
So you’re thinking a room temperature sit and first pass kinda scenario.
Then do a cryo pull afterwards with a 90/10 for the remainder?
Also, as another question in the iso/water mixture and boil… I’ve read a few articles stating that thc and the like are moderately soluble in water, especially under heat. There’s up to a 50% loss in cannabanoids with bud being boiled in water. I’m curious if the milky water portion that is pulled off contains noticeable levels of thc? Have you tested that before?
There is some cannabinoid that can get pulled along with the water for sure. When the water is chalk white there is not any I can detect. However milk white to white/brown a bit indicates some cannabinoid. I always freeze the white portion in my kitchen freezer. This will precipitate the cannabinoid out of the water and leave it stuck to the dish. After several ounces (several months for me) I end up salvaging what is there but it is generally not all that much. I have just tossed the milky white stuff to later realize I was tossing usable stuff. Really though it amounted to just several large dabs worth but as far as solubility in water per se I have not noticed an issue except as noted above.
The simple test is just evap the water and you will get a good idea of what you pull along with it. I definately plan just a simple room temp operation next time and then a cryo winterization though I am not sure if I will cut the iso with water or not then. I am curious how low I can go with iso and compound before it freezes hard. Also curious now how much wax will be recovered when the winterization is a step two process and this will tell me how effective the room temp procedure is.
PCR is incredibly sensitive, and you can definitely find DNA wherever you decide to go looking for it. but yeah, I’m in the same camp, there should be very little DNA in an ethanol or hydrocarbon based extractions (not as sure about CO2. 'cause I’ve not had the chance to play with it). DNA pretty much prefers sea-water…
I read into one of your dcvc discussions that the latter brown layer was waxes. Does the DCVC effectively dewax/winterize? The winterizing just adds so much extra steps into the equation between filtering/evaporating etc.
Also, how “waxy” of an extract have you done a successful dcvc with? I’m doing the etoh/water technique.
Wax is a term that actually describes many compounds. I have noted that wax cannot be disolved very well or at all in alcohols though I have not tried ethanol. Wax can indeed show up in an alcohol concentrate or at least part of what are called wax does. Scums and such often called waxes too are involved and will disolve in alcohol.
I have run all sorts of configurations and believe for a higher refinement it pays to winterize the “waxes” and catch them off in a seperate process. The resolution seems to be better when there are fewer compounds by mass trying to pull through a column. My methods grossly overload my columns anyway compared to say a quantification sort or run and are preporatory only. Be cautious of my words when I say waxes or scums because I am talking generally and some parts of “wax” will elute in different orders according to mobile and stationary phases.
To answer your question then, DCVC will indeed partition waxes or rather components of waxes and I have found it to be an effective treatment for dewaxing at room temperature. I never run columns at temps other than ambient so cannot attest to the behaviours at other than ambient temperatures. The best way to know is to just run a column and see. The stationary phase will have a huge impact on what elutes when and so will solvent gradient but you cannot really botch up compound with a poor run. It IS possible to leave a bunch of good compound in a column and not realize it so my suggestion is to run the column until you have pulled across everything you want but it will be tough to get all the later eluting stuff through if that is your goal. I just run it until I am past the green bands and then trash the column.
At times there is little overlap into the green fraction of the THC and sometimes a lot but I have yet to see it extend past the green. I am talking standard phase and silica gel too and I think you are pioneering advancements in reverse phase over alumina so your observations will be different.
Trying a cold gradient run right meow I’ll post the results! Starting at 60/40 etoh/water.
I tried fully 95% cold temp over alumina just to see what happens. There was very little resolution (no kidding). I have a feeling the waxes and chlorophylls are actually moving through faster at cold temps, but we’ll wait and see.
If i can just keep one solvent through the whole process I think I’ll be in a good spot.
I’m trying to avoid evaporating off solvent, then redissolving in etoh, then winterizing, then putting back in etoh for the dcvc.
It might make sense for me to just stop the first solvent pull 3/4 of the way through and then put that in the freezer to winterize. It’s just hard to hit that 8-10x solvent to resin that’s optimal for the winterization.
Awesome! I love the research spirit and can see you WILL figure out precisely what is going on and how to control it. It took me a LOT of experiments to dial in my tech and every time I posted stuff at first I got the internet once over by those who had a different vision.
The real trick to making this all work is simple: confidence and ignoring the detractors. I look forward to your results.
Methinks I’ve stumbled upon something moderately useful?
The first pull at 75% dropped out a whole whack of waxes with a bit of cannabanoids. I’ll post a photo series in a bit but it came out in some pretty neat layers. Next layer is coming out a super nice orange. I think I’m onto something!