Yeah, this is for distillate. I’ve gotten 99.4% total cannabinoids with the carbon involved. 98% with just t5 and t41. But that was at 165c vapor temp for the entire mains first pass. Took forever, so now I’ve opted for faster runs with slightly lower potency.
I am also doing room temp now over cold extraction due to higher yields.
I’d love to hear your room temp tek! That’s what I’m doing and I’m sure there is room for improvement. Thanks for sharing btw, your a gem🙏🏼
I do the same tek for the room temp. Im thinking of switching from organic etho to heptane denatured etho to see if i can pick up less water solubles at the extraction stage too.
That’s what I use.
What are your room temp soak times?
I do 8-10 min.
I’ve only done 1 x 5 min soak and 1 x 10 min soak. Yields were very similar. So it’s gonna be between that.
There’s a thread discussing the problems with using heptane denatured ethanol…
…something to consider. Maybe just go straight heptane instead. If you go that route just be aware of the differences in safety hazards associated with heptane compared to ethanol.
I’m going to use molecular sieve 3a to remove any water from the solvent.
You’re not worried about the highly exothermic nature of that process? Especially considering it needs to be done after nearly every run?
Are you using an actual re-purposed washing machine? If so, I’d advise against heptane denatured etoh because of possible compatibility issues with the seals. Sounds like the stuff chews through Panda spinners pretty quickly, and I can’t imagine what that’s leaching into the extract would be very healthy.
Also, if that’s the case, avoid straight heptane completely. Heptane and ethanol might both score a 3 on the NFPA diamond, but static ignition is real source for concern with heptane, unlike ethanol. Not to mention that heptane has much more potential energy than ethanol and it can’t be put out with water like ethanol can.
I’ve been REALLY wanting to extract with straight heptane myself, but I just don’t have the equipment to do it safely right now. I already feel like I’m pushing my luck with it just using it for LLE and filtration. I think I might stop filtering with heptane despite my spectacular results though. I’m also losing 33% of my crude post-filtration. I thought it was the magsil at first, but I think it might actually be the silica. Beaker mentioned that he had a hard time moving cannabinoids through silica 60 with pure hexane, and had to add about a 30% gradient to move it along with his DCVC experiments. Maybe a solvent gradient would be the answer to our yield problems??
Considering that using straight heptane would lead to a massive change in safety, using the beads in the 5 gal chamber i use for filtering wouldn’t be that much of a deal. I’m willing to try it out as my tries with etho and iso pull to much water solubles. That’s pretty much what I’m interested in.
@coppertop
I’ve removed most plastic in my panda so there is nothing sealing anything in it that i can see, so it should be fine. I’ll have to look further into it.
I still have enough etho for a while and i have tonnes more to read up about.
I’ve stopped haxane/ heptane washes now and am gonna try adding water washing straight in the roto instead.
I’m interested in how that works out. I’m having terrible seeing how you’ll use water in a rotovap to remove water solubles… I can definitely see it in a separatory funnel though.
I was told to do it by a member here, honestly im uncertain how it should work other than the water solubles carry through in the vapor phase. This is after all how they’ve carried over in the spd, which has lead to red spots and streaks in the head, condenser and rf.
I’ll try it out and get back to you.
Whenever I do a room temp wash, I make sure to do a brine wash with heptane after winterization to remove all the water solubles and some terps. This is where methanol REALLY shines because it’s so cheap. Right after I finish filtering through alumina to remove waxes I throw it all into a sep funnel and add heptane 4:1. I then add enough water to dilute the methanol to ~50%, mix thoroughly, allow to separate, then drain off the aqueous layer. I then do a wash with a bit of baking soda and another 2 neutral washes to neutralize, but that’s only because I use citric acid when I’m winterizing for degumming.
These are my results with a room temp etoh extraction on hemp and doing LLE and filtering through a column with heptane before distillation.
hot water in a sep funnel is what you need. ive done it and it worked great. I want to get @david to make me a specialized jacketed sep funnel soon to circulate hot water just for doing hot water wash. putting water in the roto didnt work out for me too good.
@coppertop
Nice! How do you use the critic acid when winterizing? Just straight in the etho cold or do you warm it up before winterizing? And how much do you use for 5 gal etho?
@square_root_pharms
I’m taking it that the water solubles stayed in the crude then? How much water did you use?
I add about 15 grams per liter of solution after I dissolve it in the methanol, then throw it in the freezer. Just note, it’s important to neutralize the acid before distilling or you’ll end up getting isomerization. Even the heat from a roto can cause isomerization while it’s acidic.
I’m not sure how throwing water in the roto with the crude would work? It sounds like the water would just distill off and leave the water solubles behind in the crude. Just because it’s soluble in water doesn’t mean it evaporated with water. 
EDIT: I dissolve the citric acid in water before I toss into the solution. I dilute my methanol to 90% in order to help precipitate waxes more efficiently. So say I have 10 liters of methanol that I’m mixing with the crude, I would dissolve 150 grams of citric acid into 1.1L of water and add it to the solution before freezing.
Most of my water solubles get pulled out by the t5. Im just trying to get the very last stuff that sometimes gets through the spd with the disty. So i know it has the possibility to carry over in the vapor phase. Not sure it will in the roto.
I did it to heat the mixture and dump straight into a sep funnel. Not really sure what I was hoping to gain but it was more experimental then anything. It was a mistake and from now on the way I will handle it is leaving enough ethanol in the crude to keep it fairly flowable add distilled water heat, stir or shake then sep funnel to separate. Then repeat a few times. This seems to really help with a light colored first pass and I don’t get as much gunk in the boiling flask when decarbing
So you don’t do ph brine washes? Just enough etho and distilled water?
Can help achieve gold premium color on first pass dm for SOPs.
