Warm ethanol extraction of trichome heads

Hello all. I have done all of my ethanol extractions at -50C to date, but my extracts have been a little "flat" compared to the high quality flowers that I am using as material. This is likely because many of the terpenes are not getting picked up in my ethanol wash. I have paid great attention to keep temps below 90F during distillation under vacuum and a purge in three stages over 6-8 hours at 90, 100 & 110F.

My current process involves making dry ice hash to fully remove almost all moisture. I was curious what I would pick up as far as contaminants and other undesirable elements if I did an ethanol wash at 30C-40C of ONLY the trichome heads. There would be minimal chlorophyll in the first pass material. I would do a -50C extraction on the bag material after to get a full cannabinoid extract of all material. Currently, I do the -50C wash on both.

Will I get any waxes or other crap that will reduce potency in my extract if I do this? Would there be a difference in grabbing water soluble terpenes using 190 proof (with 5% h2o) versus 200 proof ethanol?

WFF

I would guess that you're losing a lot of the micro trichome heads in your prep process. Lot's of aromatics falling thru your filter...

Hi prune. I use a 190 micron bubble bag for the dry ice hash step. I collect trichomes in bucket and save the material in the bag to be extracted. Are you saying that I am losing aromatics in the transfer? I ordered a ln2 dewar and some large ptfe coated screens as well as sheets of various micron mesh. I plan to test ln2 hash that is hand sifted into a stainless pan sitting on dry ice, with the thought being that material stays below freezing until extraction to lock in the terpenes.

WFF

I have found that the warmer the ethanol the darker the oil, not any less potent, or smell, taste, but much darker which nowadays seems less desirable.

WaterFarmFan said:

Hello all. I have done all of my ethanol extractions at -50C to date, but my extracts have been a little "flat" compared to the high quality flowers that I am using as material. This is likely because many of the terpenes are not getting picked up in my ethanol wash. I have paid great attention to keep temps below 90F during distillation under vacuum and a purge in three stages over 6-8 hours at 90, 100 & 110F.

My current process involves making dry ice hash to fully remove almost all moisture. I was curious what I would pick up as far as contaminants and other undesirable elements if I did an ethanol wash at 30C-40C of ONLY the trichome heads. There would be minimal chlorophyll in the first pass material. I would do a -50C extraction on the bag material after to get a full cannabinoid extract of all material. Currently, I do the -50C wash on both.

Will I get any waxes or other crap that will reduce potency in my extract if I do this? Would there be a difference in grabbing water soluble terpenes using 190 proof (with 5% h2o) versus 200 proof ethanol?

WFF

Click to expand...

There is a small amount of wax coating the trichomes, but most plant wax comes from coating the leaves, so starting with kif sidesteps that issue.

Extracting the terpenes is easy, holding on to them during purging is where the challenge lies.

How are you purging?

Gray Wolf said:

There is a small amount of wax coating the trichomes, but most plant wax comes from coating the leaves, so starting with kif sidesteps that issue.

Extracting the terpenes is easy, holding on to them during purging is where the challenge lies.

How are you purging?

Click to expand...

Hey GW! My last few batches I have done a sub-90F distillation under vacuum with external probe mantle, which removes 85-90% of ethanol, and then I let it sit in a flask for 2-3 days to remove another 5% ethanol and then single paddy on silicone mat in AI 0.9 vacuum oven. I start off at 90F at 29.5Hg and purge for an hour or so til the bubbling subsides. I then release backfill to send ethanol vapor to collect in cold trap, and then bring back vacuum and ramp 10F, which takes 10-15 minutes to reach. About and hour and half at this temp, bump, and raise to 110F for two hours. I dab samples to taste for ethanol and will push to 120F to see if more bubbling. Usually 5-6 hours under full vacuum during the temp ramp.

Does it need to be "burped" a little more often? Will evaporated ethanol re-condense back on slab? Any insights would be most helpful. Thanks!

WFF

On another note, I have been using flowers that have cured for 3-4 months. Would the combination of dried and aged flowers being converted to dry ice hash first diminish the terpene profile that I am collecting? Hmmmm...

WFF

Also, my thin film might not be thin enough. What range of gram per square inch of thin film would you recommend. If I had a 9" diameter thin film, which is around is around 63 square inches, how much shatter would a perfect thin film yield?

WaterFarmFan said:

Hello all. I have done all of my ethanol extractions at -50C to date, but my extracts have been a little "flat" compared to the high quality flowers that I am using as material. This is likely because many of the terpenes are not getting picked up in my ethanol wash. I have paid great attention to keep temps below 90F during distillation under vacuum and a purge in three stages over 6-8 hours at 90, 100 & 110F.

My current process involves making dry ice hash to fully remove almost all moisture. I was curious what I would pick up as far as contaminants and other undesirable elements if I did an ethanol wash at 30C-40C of ONLY the trichome heads. There would be minimal chlorophyll in the first pass material. I would do a -50C extraction on the bag material after to get a full cannabinoid extract of all material. Currently, I do the -50C wash on both.

Will I get any waxes or other crap that will reduce potency in my extract if I do this? Would there be a difference in grabbing water soluble terpenes using 190 proof (with 5% h2o) versus 200 proof ethanol?

WFF

Click to expand...

I do not extract because in Oregon although legal to posess, the act of extracting using a solvent of any kind is illegal without a license.

However, let me offer an idea. It is known that to denature proteins which all living cells are made up of that an alcohol of nearly any kind can be used. Denaturing the proteins in plant matter like marijuanna happen when the alcohol causes the DNA to unravel from a neat helix into a long random stringy looking white thing that normally precipitates out of solution once denatured. "Wax" is a very broad term and normally applies to a mix of things. Many call the DNA that precipitates out of solution a "wax" which is another way to say it is a denatured protein and a bunch of other things that are kind of creamy and smooth. Low temperatures may hasten the appearance of gooey white denatured DNA but the "wax" precipitates primarily owing to the denaturing of the DNA strands and other proteins. Take one gram of extract and drop it in a mason jar with a cup of methanol. Come back at one hour intervals all at room temp. You will witness DNA precipitating out of solution as a white gooey suspended substance no longer in solution with the rest of the extract. Since the compound disolved completely in the methanol (wait for it and stir but no heat), and since if covered the solvent does not change in composition or heat, then the only explanation for precipitation at room temp is denaturing of the proteins if you observe the same things I have doing this. You cannot help water from entering the alcohol from atmosphere so water will always be present to some degree and is nearly always increasing as we work with it (from atmosphere).

My point though is how is this useful information? Well, there is a reason that rubbing alcohol that is used in hospitals for disinfecting our skin is mixed at a ration of 70% alcohol to 30% water and it has nothing to do with patient comfort or costs. One paper written in 1920 that studied proteins pointed out even back then that when pure alcohol was applied to kill germs that the proteins on the outside of the cell denatured and adhered to the outside of the cell which prevented the alcohol from passing the membrane and unravelling the DNA. This means it damaged but did not necessarily kill the germs that were being targetted. They found that they needed to add 30% water for complete penetration of cell walls which killed the pathogen.

I would suggest running the product twice. The first time soak as you normally would in a mix of any alcohol at 70/30. Then immediately follow that after decanting the liquid with a second soak at the best purity you have and normally use.

Evaporate off the solvents and see what you get. The 1920 study I cited was studying spinach proteins and which concerned itself with chlorophyl removal just as this industry does. It would be interesting to hear from an extractor if a 70/30 mix leaves anything behind that a stronger mix of say 99% alcohol extracts. Rather than adjusting temps you may find a binary solvent system of alcohol and water to at some ratio to be more effective at targetting what you are after than alcohol alone.