Ethanol Cold Wash Yields

c03rcion · Nov 20, 2017

Yields are low, around 4%, when washing bud with 200 proof ethanol, distilling off the ethanol, and vacuum purging the slurry to yield a shatter.

The bud is whole bud that has been freeze dried and kept in a -86 C freezer.

Ethanol is kept in -86 C freezer as well.

Bud steeps in sub-zero ethanol for 30 minutes and color of solution is yellow-gold. Looks great and excellent clarity.

Problem is the find yield of the shatter was 5.7 grams out of 153 grams of the above mentioned bud. I don't know the THC percentage of the bud, but it was sun grown and possibly 15%.

I was hoping my yields would be closer to 10% because anything less is just not worth it.

Any ideas?

WaterFarmFan · Nov 20, 2017

More detailed response in the other thread, but put 10 grams of the material in a oven at 175-200 F for 15-20 minutes and then weigh the material again. If the material weighs 5 grams, then your yield is actually 8%.

Gry · Nov 20, 2017

OT: ATF used to do a similar bulk extraction using the lab at St Elizabeth’s - same place Hinkley would later be kept.
Results were parcelled out for R&D.

Gray Wolf · Nov 20, 2017

c03rcion said:
Yields are low, around 4%, when washing bud with 200 proof ethanol, distilling off the ethanol, and vacuum purging the slurry to yield a shatter.

The bud is whole bud that has been freeze dried and kept in a -86 C freezer.

Ethanol is kept in -86 C freezer as well.

Bud steeps in sub-zero ethanol for 30 minutes and color of solution is yellow-gold. Looks great and excellent clarity.

Problem is the find yield of the shatter was 5.7 grams out of 153 grams of the above mentioned bud. I don't know the THC percentage of the bud, but it was sun grown and possibly 15%.

I was hoping my yields would be closer to 10% because anything less is just not worth it.

Any ideas?

5.7/153 gm= 3.7% yield, which is very low.

At -80 you typically need more than a 30 minute extraction and need agitation or flow.

Check your spent material with a microscope to see what is left.

Bjorn to farm. · Nov 20, 2017

I started out making iso oil out of trim and then switched to bud when I had enough.
I did the 30 second wash with frozen isopropahol and weed. Then when i looked at the spent material under a scope? Trichomes everywhere!

c03rcion · Nov 20, 2017

Quick Wash

Quick Wash

Gray Wolf said:
5.7/153 gm= 3.7% yield, which is very low.

At -80 you typically need more than a 30 minute extraction and need agitation or flow.

Check your spent material with a microscope to see what is left.

Thanks GW. I'm looking at some of the 'washed' material and I am still seeing trichomes. Any recommendation for how much time is needed at -80C?

I want to wash the previous washed bud again to get the end to end yield but afraid ill pull a lot of the chlorophyll out. I rewashed some other bud and while I could see some gold there was a lot of green.

I have tried using Oil Dry Diatomaceous earth to make a cake and pass my green solution through but didn't seem to help. Would my best bet be UV radiation to clear up that green? Will it affect the taste?

WaterFarmFan · Nov 20, 2017

c03rcion said:
Would my best bet be UV radiation to clear up that green? Will it affect the taste?

I watched a video from a cancer doctor that performed room temperature etoh extraction yielding a VERY dark green extract. He placed the volume out in the sun for an hour and it was virtually all gone. I bet you could simply place a flask on the windowsill if it is excessive. The little bit that I pick up seems to disappear quickly on its own with just some LED lighting in the lab space, and heat also seems to help also.

How are you distilling and purging the ethanol solution? If using glassware to distill, you really need to wash with a tiny bit of etoh at each step as there are lots of ways to lose yield with thin films sticking to everything.

c03rcion · Nov 21, 2017

WaterFarmFan said:
I watched a video from a cancer doctor that performed room temperature etoh extraction yielding a VERY dark green extract. He placed the volume out in the sun for an hour and it was virtually all gone. I bet you could simply place a flask on the windowsill if it is excessive. The little bit that I pick up seems to disappear quickly on its own with just some LED lighting in the lab space, and heat also seems to help also.

How are you distilling and purging the ethanol solution? If using glassware to distill, you really need to wash with a tiny bit of etoh at each step as there are lots of ways to lose yield with thin films sticking to everything.

I actually did this today when the sun finally decided to show itself here in Oregon. I delivered 4 liters of dark green ethanol-cannabinoid solution to 4 mason jars and placed in the sunlight for a couple of hours. Definitely helped to get some of the green out, but still hints of it. The solution is still pretty dark and shining a light on it I can see the red pigment present.

Any idea on how to remove this red pigment, or do you know what it is? I have tried using Oil Dry Diatomaceous Earth in a manner similar to how a Celite cake is made and pass the solution through a Buchner and qualitative filter paper, but didn't see much improvement in solution clarity.

I have considered preparing a mixture of 1 part activated carbon (peat based) and 9 parts Celite but funds are low at the moment....

I attached a before and after photo. One photo of the Green solution from the top down, another of the "Sun Bleached" solution from the front.

c03rcion · Nov 21, 2017

Ethanol is recovered via rotovape. Purging done under vacuum in oven at 35 C. Yes I did find that having very thin films of shatter in the silicone baking mold it was very hard to remove. I am definitely in the discovery period of this process. I once used a pyrex dish for purging and it was very difficult to scrape out. I understand PTFE to be one of the best materials for purging slabs, could you recommend it?

WaterFarmFan · Nov 21, 2017

c03rcion said:
Ethanol is recovered via rotovape. Purging done under vacuum in oven at 35 C. Yes I did find that having very thin films of shatter in the silicone baking mold it was very hard to remove. I am definitely in the discovery period of this process. I once used a pyrex dish for purging and it was very difficult to scrape out. I understand PTFE to be one of the best materials for purging slabs, could you recommend it?

I started with large glass petri dishes and then pyrex pie pans, but I just ended going with silicone mats directly on the vacuum oven shelves. Like you, I could never seem to get all the film from corners, and the mat method is so simple to get it all. Just cool and the shatter peels right off. Buy square mats to fit your shelves exactly. Easy peezy...

https://www.amazon.com/s/ref=nb_sb_noss?url=search-alias=aps&field-keywords=square+silicone+mat

Gray Wolf · Nov 21, 2017

c03rcion said:
I actually did this today when the sun finally decided to show itself here in Oregon. I delivered 4 liters of dark green ethanol-cannabinoid solution to 4 mason jars and placed in the sunlight for a couple of hours. Definitely helped to get some of the green out, but still hints of it. The solution is still pretty dark and shining a light on it I can see the red pigment present.

Any idea on how to remove this red pigment, or do you know what it is? I have tried using Oil Dry Diatomaceous Earth in a manner similar to how a Celite cake is made and pass the solution through a Buchner and qualitative filter paper, but didn't see much improvement in solution clarity.

I have considered preparing a mixture of 1 part activated carbon (peat based) and 9 parts Celite but funds are low at the moment....

I attached a before and after photo. One photo of the Green solution from the top down, another of the "Sun Bleached" solution from the front.

UV deprotonates the chlolrophyll molecule, which turns into pheophytin, which is olive brown, versus the green produced by the same molecule, but with the magnesium ion in the head.

PDX Dopesmoker · Nov 21, 2017

How viscous is the ethanol at -86? Everclear starts to get a little syrupy at -30 in my deep freeze.

c03rcion · Nov 22, 2017

PDX Dopesmoker said:
How viscous is the ethanol at -86? Everclear starts to get a little syrupy at -30 in my deep freeze.

The ethanol becomes almost like syrup.

PDX Dopesmoker · Nov 23, 2017

I doubt the solvent is going to contact the inside of your flowers that way. I shred all my stuff pretty thoroughly before soaking in Everclear (or Clear Springs) for that reason. You can shred it with a machine and make beaucoup particualtes or you can gently open up the flowers by hand and make a lot of meticulous labor for yourself.

If you can grow flowers with a really open structure you might not run into the problem of getting whats trapped inside the bud to come out without making a lot of particulates or meticulous labor. I have this idea of breeding a plant where the seeds are so big that you only have a few super big calyxes on each plant and all the resin is on the outside instead of some convoluted structure where yeah the resin is all on the outside, but its on the outside of some ornate fractal shape and buried inside a larger structure thats not accessible to solvent soaks.

Gtir · Nov 23, 2017

How long should -80 be soaked to extract everything?

Mikell · Nov 23, 2017

PDX Dopesmoker said:
I doubt the solvent is going to contact the inside of your flowers that way. I shred all my stuff pretty thoroughly before soaking in Everclear (or Clear Springs) for that reason. You can shred it with a machine and make beaucoup particualtes or you can gently open up the flowers by hand and make a lot of meticulous labor for yourself.

If you can grow flowers with a really open structure you might not run into the problem of getting whats trapped inside the bud to come out without making a lot of particulates or meticulous labor. I have this idea of breeding a plant where the seeds are so big that you only have a few super big calyxes on each plant and all the resin is on the outside instead of some convoluted structure where yeah the resin is all on the outside, but its on the outside of some ornate fractal shape and buried inside a larger structure thats not accessible to solvent soaks.

PDX Dopesmoker · Nov 23, 2017

I had one that did that to me this summer. Its real tasty too, but only put on about half the weight of her more conventionally shaped sisters.

Gray Wolf · Nov 23, 2017

Gtir said:
How long should -80 be soaked to extract everything?

That is the question of the hour, isn't it? As far as I can tell, none of us know, cause we've never extracted that cold.

c03rcion · Nov 23, 2017

PDX Dopesmoker said:
I doubt the solvent is going to contact the inside of your flowers that way. I shred all my stuff pretty thoroughly before soaking in Everclear (or Clear Springs) for that reason. You can shred it with a machine and make beaucoup particualtes or you can gently open up the flowers by hand and make a lot of meticulous labor for yourself.

If you can grow flowers with a really open structure you might not run into the problem of getting whats trapped inside the bud to come out without making a lot of particulates or meticulous labor. I have this idea of breeding a plant where the seeds are so big that you only have a few super big calyxes on each plant and all the resin is on the outside instead of some convoluted structure where yeah the resin is all on the outside, but its on the outside of some ornate fractal shape and buried inside a larger structure thats not accessible to solvent soaks.

I've moved away from doing the entire wash at -86 and now do the wash at -20C and find that I am removing nearly all the trichome matter. I inspect the buds under the microscope, and pull them open to see, and find I am getting most of the material (including the inside of the bud).

To be clear, I chill the ethanol and bud in the -86 and do the wash in the -20C freezer. The ethanol slowly warms from -86 to -20 and in the process pulls out cannabinoids and water solubles (very slowly) so I know when to stop when I detect the faintest green.

Reminds me of doing titrations.

c03rcion · Nov 23, 2017

Long soak at -86

Long soak at -86

Gray Wolf said:
That is the question of the hour, isn't it? As far as I can tell, none of us know, cause we've never extracted that cold.

So i took a gram bud and placed in a 50 ml flat centrifuge tube, along with about 15-20 ml of ethanol, and placed in the negative 86 C freezer. I checked it after 2 hours and found the solution was still clearish-yellow. I was going to check it after another hours but forgot and went home. When I checked it the next day, after filtering the solution with a 0.2 micron filter and HPLC syringe, here is what I found (photo attached)

This was a 1 gram bud placed in about 15-20 ml ethanol in a test tube, shaken vigorously every 30 minutes, and left in a -86 C freezer for about 24 hours and yielded a faint yellow-gold solution.

Ethanol Cold Wash Yields

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