Yielding less with a closed extraction system than I did with open blast

Realbax

Realbax

Well-Known Member
Maybe someone can tell me where I am going wrong here? Recently received a closed loop system. Just a pint sized 180g set up but a safer setup which is what I wanted. I had run a handful of open blast runs up till now and decided that I liked it enough to invest in a better solution. The open blast rig was similar size and the material was from the same batch which was dried and cured then frozen. The new setup gets a vacuum pulled on it and put in the freezer. As its winter I have been storing the butane which I distilled and recovered into a recovery cylinder outside where it remains a liquid. I pack the column but not super tight as i hadn't been able to do so with the other one and didn't want to choke the system. I remove the extractor and once outside I invert the recovery tank once it's all connected purge air from the line and fill the column. Isolate the chamber and set a timer for 10 minutes. First time being able to isolate like this so I have no idea what duration a soak should be. When I release the column into the collection base the pressure rises to roughly 30psi. I let it sit for 5 minutes while I pull a vacuum on the second recovery cylinder. Then use pressure differential and temperature differential to collect the butane for another run. I was shocked to see such a little amount of extract. When I ran the open blast i would average between 10- 15% return. With the new setup maybe 2%? Im not sure but hardly anything. Could someone please tell me where I'm going wrong here?
 
Fadedawg

Fadedawg

Well-Known Member
Realbax said:
Maybe someone can tell me where I am going wrong here? Recently received a closed loop system. Just a pint sized 180g set up but a safer setup which is what I wanted. I had run a handful of open blast runs up till now and decided that I liked it enough to invest in a better solution. The open blast rig was similar size and the material was from the same batch which was dried and cured then frozen. The new setup gets a vacuum pulled on it and put in the freezer. As its winter I have been storing the butane which I distilled and recovered into a recovery cylinder outside where it remains a liquid. I pack the column but not super tight as i hadn't been able to do so with the other one and didn't want to choke the system. I remove the extractor and once outside I invert the recovery tank once it's all connected purge air from the line and fill the column. Isolate the chamber and set a timer for 10 minutes. First time being able to isolate like this so I have no idea what duration a soak should be. When I release the column into the collection base the pressure rises to roughly 30psi. I let it sit for 5 minutes while I pull a vacuum on the second recovery cylinder. Then use pressure differential and temperature differential to collect the butane for another run. I was shocked to see such a little amount of extract. When I ran the open blast i would average between 10- 15% return. With the new setup maybe 2%? Im not sure but hardly anything. Could someone please tell me where I'm going wrong here?
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A good test for removal efficiency, is a 100X microscopic examination of the spent plant material. There should be no intact heads, only stalks and hairs remaining.

How much butane did you pass through the material and what size is the column? Did you weigh the supply tank before and after?
 
Realbax

Realbax

Well-Known Member
Thank you for the reply. I ran 15.5 oz of butane. At the end i recovered 12.8 oz. A bit of loss but I'll get that down soon hopefully. I will have to wait till lights go on, I left the microscope in there last night. I will definitely give it a check asap. Thabk you.
 
Fadedawg

Fadedawg

Well-Known Member
You didn't share your column size, but let's play with numbers to determine how much butane would be required for a three volume flood. I normally get from 3.5 to 4.1 grams/in3 packing density, depending on how I prepare the material.

180grams/3.8/inch3 grams=47.37 inch3

47.37in/3 X .0217 lbs/in3 X 3 = 3.1lbs butane

Sounds like you are shy at 15.5 oz.
 
Realbax

Realbax

Well-Known Member
Thanks for the reply. I have been limited to canned butane up on till now. Next week I'll stop by the wholesalers and pick up a few small tanks of r-600. I'll update once I try a run with at least 3lbs. Much appreciated
 
Realbax

Realbax

Well-Known Member
Fadedawg said:
You didn't share your column size, but let's play with numbers to determine how much butane would be required for a three volume flood. I normally get from 3.5 to 4.1 grams/in3 packing density, depending on how I prepare the material.

180grams/3.8/inch3 grams=47.37 inch3

47.37in/3 X .0217 lbs/in3 X 3 = 3.1lbs butane

Sounds like you are shy at 15.5 oz.
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I attempted a smaller load in the system this morning and found that the butane from the Recovery cylinder was dirty looking. Like it still contains extract? How can I ensure that any possible extract is contained in the collection pot and not recovered with the solvent?
 
DemonTrich

DemonTrich

Well-Known Member
Always distill any new butane to get rid of the mystery oil. It's been mentioned in nearly every bho/cls thread.
 
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Realbax

Realbax

Well-Known Member
I thought I had. Is that what is carrying the residual extract back to the recovery tank? Do all forms of butane contain mystery oil?
 
DemonTrich

DemonTrich

Well-Known Member
Before you pack tubes to do a run, always run new butane tanks thru your system like a bho dun. The mystery oil should stay in the collection pot, like where your bho would be. Clean, then maybe do once more for peace of mind.
Clean again.
Then your new tank has now been cleaned of mystery oil.
 
Fadedawg

Fadedawg

Well-Known Member
Realbax said:
I thought I had. Is that what is carrying the residual extract back to the recovery tank? Do all forms of butane contain mystery oil?
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Yes, mystery oil will be present at some level, but they shouldn't be transferring in any great quantity when pre-distilling.

How are you doing your pre-distillation?

What are you using for a recovery tank? Is it brand new?

How did you clean your brand new system of manufacturing oils and grime before using?
 
Realbax

Realbax

Well-Known Member
I had distilled it by running it through the system and cleaning the residue from the collection base. I cleaned it initially and after the distillation with 99% iso. The recovery tank was unused until last week. It sat in storage for a couple of years but was still in the manufacturer's wrapping. I even ran nitrogen through it to purge and help ensure that it was dry before pulling a vacuum.
 
Fadedawg

Fadedawg

Well-Known Member
Realbax said:
I had distilled it by running it through the system and cleaning the residue from the collection base. I cleaned it initially and after the distillation with 99% iso. The recovery tank was unused until last week. It sat in storage for a couple of years but was still in the manufacturer's wrapping. I even ran nitrogen through it to purge and help ensure that it was dry before pulling a vacuum.
Click to expand...
What temperature did you distill at?
 
Realbax

Realbax

Well-Known Member
I put the system and the sealed butane in the freezer over night. Everything would have been around -20. I read that chilling everything as cold as possible would help to leave undesired fats and lipids in the material instead of the extract. I would prefer to not have to get into winterizing. May have to though as the little i did pull isnt as clear as I was previously getting. I'm definitely going to need practice and more research, even though I've read everything I can get ahold of, because both quality and yield have suffered since I went closed column and I was truly expecting the opposite. I have fresh butane today I got rid of the previous butane and pulled a solid vacuum on the tank over night. I'm going to reread as much as possible before distilling the new butane and doing another run. The plan is to pack 90g not too tight and run 355 grams of solvent at room temperature let everything sit for 60 min in a couple of inches of ice water to hopefully help the extract in the vapor to condense. Hopefully this will help to recover just the solvent cleanly without any further residual extract getting picked up this time. I have to hope that this will work out today as I only have enough material left for one or two more columns till harvest and if I'm going to dry and cure it again instead of attempting to freeze fresh and go that route it will be at least a few weeks. Any tips for this next round?
 
Realbax

Realbax

Well-Known Member
K. So i did a run. I broke down and froze everything for a couple hours. Put the system under vacuum. Put the first 165g through as I was not going to do a soak. Let it sit in ice water to attempt to condense the vapors etc. I recovered the gas after 40 minutes. Or at least i thought I had. The pressure had equalized at around 8 psi and i couldn't get it to budge. I didn't want to waste time with temperature differential to collect the difference as i (wrongly) assumed it would be a small amount of vapor. I cracked the shut offs. The pressure on the gauge read 1 psi. Opened the collection base and inside was an inch or more of liquid. At first I thought I might have tipped the system and somehow managed to get water inside but that isn't possible for a few reasons. Its 2c here today so I was a little stunned at first to think that despite being above the temperature for evaporation and being at atmospheric pressure that it had managed to stay liquid. I realize that the temperature of the collection base has a lot to do with it. Currently I have it sitting on a heating pad at max and the bubbles have all but stopped unless it's disturbed. Is any of this seem right to anyone? Will this be a shatter when done? Thanks
 

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