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Old 11-20-2017, 03:34 AM #1
c03rcion
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Ethanol Cold Wash Yields

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?
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Old 11-20-2017, 09:15 AM #2
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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%.
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Old 11-20-2017, 11:04 AM #3
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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.
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Old 11-20-2017, 02:02 PM #4
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Quote:
Originally Posted by c03rcion View Post
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.
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Old 11-20-2017, 07:43 PM #5
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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!
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Old 11-20-2017, 08:58 PM #6
c03rcion
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Quick Wash

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Originally Posted by Gray Wolf View Post
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?
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Old 11-21-2017, 01:57 AM #7
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Quote:
Originally Posted by c03rcion View Post
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.
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Old 11-21-2017, 04:26 AM #8
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Originally Posted by WaterFarmFan View Post
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.
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Old 11-21-2017, 04:34 AM #9
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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?
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Old 11-21-2017, 07:42 AM #10
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Quote:
Originally Posted by c03rcion View Post
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_n...e+silicone+mat
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