How to perfect the process of extraction at home

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Eskander

Eskander

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I had also read that DOW had the best grease, but had a hard time finding it. I am actually glad I couldnt get it as I believe the Haynes is the better option for this application.

My lab ended up with a case of the dow corning grease right as we were told to switch to apeazon for compliance reasons so it is all I've ever used. I'm a bit surprised it made that much of a difference for you as I usually have an extremely light coating on my joints. I wipe them and then rub them essentially dry with a lint free cloth. You sure you don't have a screwed up joint? You can always test with a cap to see what the pump can pull down to. Just add one piece at a time until you see the ultimate vacuum drop and you'll have your bad joint.

If you are pulling a better vacuum, you can always use a sous vide to control your temps at more modest ranges.


I will say though that your distillation rate is painfully slow looking. Any idea how long it takes to run a liter through?

-Eskander
 
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cronicoldguy

74
18
Hey Eskander.

Yes, almost painful. I can distill a liter in about 1.5hrs. Not as fast as a rotovap. But kicks the dog shit out of the ST.

Now that I have this still kinda figured out, I am somewhat regretting ordering a $3600 rotovap! It should be here by the end of next week. I might have been better off just buying a bigger still and cold trap. Use the rest of the loot on other equipment and supplies. I could have got a short path still as well. The money was an inheritance and not expected. So it doesnt hurt too bad.

With the Molykote, I first only applied it as you described. I couldnt get a seal so I plasterd it on. Still no seal but grease thin enough, it was getting pulled thru. The joints all felt seated. Discouraged, I left it for a few days to ponder. Then I had a 'duh' moment. You got other grease to try fuckstick! I tried the Haynes. Night and day difference in vacuum performance. And as you described, just a light coating.

Funny you mention the Sous Vibe. I was looking into that. A buddy had suggested it. I am still considering it. I will go with the Polyscience unit likely. It seems the most robust. Another option I was looking at is an actual lab unit. I have a J-Kem 210 Temp controller coming I got off ebay. Tired of being disappointed with cheap Chinese junk and deceitful listings. I got 2 different heating mantles off Amazon. Both garbage. The second one I got, actually had a brand name soI though it would be safe. NOT! Avoid Labasics.

I am presently distilling 1700mls of roach solution. This is the 2nd round. After the first distillation, it still grossly smelled like ass. So I poured it all back together. I added some fresh solvent and 2 heaping tablespoons of charcoal to it. Thru it in the freezer for another day and filtered thru Celite and charcoal once again. It actually smells not bad now. About 400mls to go.

EDIT: I am thinking I will raise the temp in still to just under 120C towards the end. Maybe I will get lucky and have fully decarbed oil. Maybe not. Its roaches so makes for a good experiment. But given it is roach material, would it not already be decarbed from the heat of the doobie?
 
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Eskander

Eskander

149
43
Hey Eskander.

Yes, almost painful. I can distill a liter in about 1.5hrs. Not as fast as a rotovap. But kicks the dog shit out of the ST.

Now that I have this still kinda figured out, I am somewhat regretting ordering a $3600 rotovap! It should be here by the end of next week. I might have been better off just buying a bigger still and cold trap. Use the rest of the loot on other equipment and supplies. I could have got a short path still as well. The money was an inheritance and not expected. So it doesnt hurt too bad.

With the Molykote, I first only applied it as you described. I couldnt get a seal so I plasterd it on. Still no seal but grease thin enough, it was getting pulled thru. The joints all felt seated. Discouraged, I left it for a few days to ponder. Then I had a 'duh' moment. You got other grease to try fuckstick! I tried the Haynes. Night and day difference in vacuum performance. And as you described, just a light coating.

Funny you mention the Sous Vibe. I was looking into that. A buddy had suggested it. I am still considering it. I will go with the Polyscience unit likely. It seems the most robust. Another option I was looking at is an actual lab unit. I have a J-Kem 210 Temp controller coming I got off ebay. Tired of being disappointed with cheap Chinese junk and deceitful listings. I got 2 different heating mantles off Amazon. Both garbage. The second one I got, actually had a brand name soI though it would be safe. NOT! Avoid Labasics.

I am presently distilling 1700mls of roach solution. This is the 2nd round. After the first distillation, it still grossly smelled like ass. So I poured it all back together. I added some fresh solvent and 2 heaping tablespoons of charcoal to it. Thru it in the freezer for another day and filtered thru Celite and charcoal once again. It actually smells not bad now. About 400mls to go.

EDIT: I am thinking I will raise the temp in still to just under 120C towards the end. Maybe I will get lucky and have fully decarbed oil. Maybe not. Its roaches so makes for a good experiment. But given it is roach material, would it not already be decarbed from the heat of the doobie?
Partially burned material aught to be partially decarbed. Stuff closer to your mouth isn't going to get hot enough.

The sous vides will all hit the target temps an maintain them. They are cheap as dirt cause they sell so many unlike the lab gear which is only purchased by industry and nut jobs like us. The expensive sous vides are just more expensive. The best mark of the being made by someone with a clue is that they DON'T have a built in timer, wifi or bluetooth.

So the three gallons or so of Iso wash distilled down to pretty dark even after a decolorizing pass of the bulk solution but it smells good and is noticeably viscous. This is a salt brine wash to drop protein out. This is the second step of that which involves some citric acid to denature more protein. The white precipitate at the bottom is the result of that. The initial brine hit dropped about 2 inches worth out but some of that is salt so it is hard to quantify. I followed that with a MgSO4 drying and it is in the freezer now. That aught to drop the vast majority of residual sugars.

IMG 5223


I will next filter it and then distill off all the Iso and redissolve in 95% EtOH for winterization. What I do from there depends on how it looks and smells but I'll probably end up distilling it down and doing a decarb run on it. if it tastes fine then I'll leave it. If it is funky than I'll probably do a hexane/saline wash and see if that cleans it up. Hexane is pretty funky though and requires a lot of precautions for indoor use (which I have), as well as significant purging after you have distilled off the majority. Does a bang up job of cleaning extracts though.

-Eskander
 
Eskander

Eskander

149
43
So after decarb the was done, it was about 2/3rds black oil and 1/3rd solids that resembled asphalt when cooled. Far and away the worst looking shit I've ever made lol.. So obviously that needs some clean up. I redissolved in EtOH and filtered which got out this:
IMG 5253

The white is the coarse filter paper on to of the DE cake. It usually doesn't do much for filtration but keeps the cake from being disturbed when pouring solutions into the funnel.

Still pretty funky shit so I did some small scale tests with hexane. The best result was 1:1:1 EtOH:Hexane:DI Water which is what SkunkPharm recommends. The hexane pulls everything lipid soluble out of the ethanol since once it is diluted to 50:50 it isn't nearly as good at dissolving canabanoids. The crud that ends up in the interface between the organic and aqueous layers aren't soluble in either but was soluble in EtOH.
IMG 5251


Scaled up shaken thoroughly and left to settle for 12 hours (because the interface is slow to collapse outside a centrifuge) got me this:
Sep


I'm sure for all you RSO fans the black shit at the bottom here is what has all the magical properties. Certainly looks like something that would be great for you...
IMG 5261


So that is still pitch black which I don't really care about in of itself, but since I'm just playing here I'm going to do a few Hexane/Saline washes and see if anything else comes out. I've saved some small samples of each step so I can run them on TLC. I'll update as I progress.

-Eskander
 
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cronicoldguy

74
18
Time for some extracting. It is presently -28C outside and going to drop further into the -30s. Thinking about moving the reactor to the garage and do some sub zero extracting. Room in there to set evrything up. Might be a bit cold to work in, ..........but the rewards. I have already moved all solution from freezer (-17C) to outside for winterizing. Winterizing....ya literally. ha ha.
 
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Godfish

15
3
So after decarb the was done, it was about 2/3rds black oil and 1/3rd solids that resembled asphalt when cooled. Far and away the worst looking shit I've ever made lol.. So obviously that needs some clean up. I redissolved in EtOH and filtered which got out this:
View attachment 1307638
The white is the coarse filter paper on to of the DE cake. It usually doesn't do much for filtration but keeps the cake from being disturbed when pouring solutions into the funnel.

Still pretty funky shit so I did some small scale tests with hexane. The best result was 1:1:1 EtOH:Hexane:DI Water which is what SkunkPharm recommends. The hexane pulls everything lipid soluble out of the ethanol since once it is diluted to 50:50 it isn't nearly as good at dissolving canabanoids. The crud that ends up in the interface between the organic and aqueous layers aren't soluble in either but was soluble in EtOH.
View attachment 1307643

Scaled up shaken thoroughly and left to settle for 12 hours (because the interface is slow to collapse outside a centrifuge) got me this:
View attachment 1307642

I'm sure for all you RSO fans the black shit at the bottom here is what has all the magical properties. Certainly looks like something that would be great for you...
View attachment 1307645

So that is still pitch black which I don't really care about in of itself, but since I'm just playing here I'm going to do a few Hexane/Saline washes and see if anything else comes out. I've saved some small samples of each step so I can run them on TLC. I'll update as I progress.

-Eskander
I don't really understand all that your doing? but can I ask if you could clean it up with charcoal power? I've seen videos of people doing that? would it help or does it remove to much THC?
 
Eskander

Eskander

149
43
I don't really understand all that your doing? but can I ask if you could clean it up with charcoal power? I've seen videos of people doing that? would it help or does it remove to much THC?
This actually went through charcoal once already. At the time I was unaware of quite how much canabanoid loss that would result in but MoeRed and literature suggest it is between 1 and 50% with the 1% guys typically coming from people selling carbon products. I'll run TLC on some before and after samples and see what I'm loosing. In any case, a lot of what I'm scrubbing out now would not come out in charcoal anyway. Initial extracts that come out green don't just have canabanoids, terpenes and chlorophyll, if they are green they have picked up plant sugars, proteins, waxes and other random pytochemicals too.

There are things that can selectively remove most or all of some of those undesirables. Winterizing drops out the waxes. Hexane/Saline washes drops out sugars, protiens, some of the phytochemicals and because of the partial polarity of chlorophyll, it will slowly wash that out too. The first rinse with saline was so laden with random crap that the aqueous layer came out with the consistency of applesauce. This is kind of a pain in the ass and it does take a damn long time as the layers especially early on can take 12 hours or longer to fully separate but the results are are solid improvement in the extract quality with little loss of desirables. Once enough saline washes have been done to get as much crap out as you want, you need to distill or boil off the hexane and then thoroughly purge out the remaining hexane as it is toxic.

I'm mostly just playing around seeing if I can take the 5 pounds of low quality trim and refine something decent from it. The reality is that this amount of effort is in no way worth my time but it has been a fun to play with.

-Eskander
 
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Godfish

15
3
This actually went through charcoal once already. At the time I was unaware of quite how much canabanoid loss that would result in but MoeRed and literature suggest it is between 1 and 50% with the 1% guys typically coming from people selling carbon products. I'll run TLC on some before and after samples and see what I'm loosing. In any case, a lot of what I'm scrubbing out now would not come out in charcoal anyway. Initial extracts that come out green don't just have canabanoids, terpenes and chlorophyll, if they are green they have picked up plant sugars, proteins, waxes and other random pytochemicals too.

There are things that can selectively remove most or all of some of those undesirables. Winterizing drops out the waxes. Hexane/Saline washes drops out sugars, protiens, some of the phytochemicals and because of the partial polarity of chlorophyll, it will slowly wash that out too. The first rinse with saline was so laden with random crap that the aqueous layer came out with the consistency of applesauce. This is kind of a pain in the ass and it does take a damn long time as the layers especially early on can take 12 hours or longer to fully separate but the results are are solid improvement in the extract quality with little loss of desirables. Once enough saline washes have been done to get as much crap out as you want, you need to distill or boil off the hexane and then thoroughly purge out the remaining hexane as it is toxic.

I'm mostly just playing around seeing if I can take the 5 pounds of low quality trim and refine something decent from it. The reality is that this amount of effort is in no way worth my time but it has been a fun to play with.

-Eskander
I'm sure lots
 
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cronicoldguy

74
18
@Eskander
I am a bit confused now. So using charcoal as a filter medium can actually result in a loss of THC? I have been mixing liberal amounts into the solution prior to winterization as well as a layer in Buchner Funnel in tandem with DE post winterization.
Could I be harming my extract?
 
G

Godfish

15
3
I'm sure lots of people would like to know what role Charcoal plays in removal of THC? It's really good at removal of the green color but what also is getting removed?, although I'm starting to like the idea of a little green in my cookies.
 
G

Godfish

15
3
@Eskander
I am a bit confused now. So using charcoal as a filter medium can actually result in a loss of THC? I have been mixing liberal amounts into the solution prior to winterization as well as a layer in Buchner Funnel in tandem with DE post winterization.
Could I be harming my extract?
I'm no expert but I think it can remove oils? I do my QWISO then after I add 1/8 tsp to my QWISO then filter again through the Buckner, If it's still green I'll do the same again, Before I'm done I'll run clean ISO through the Buckner in a hope to recover any oil that the Charcoal is holding. I don't use any DE because I use the Buckner filter paper as the filter.
 
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cronicoldguy

74
18
I'm no expert but I think it can remove oils? I do my QWISO then after I add 1/8 tsp to my QWISO then filter again through the Buckner, If it's still green I'll do the same again, Before I'm done I'll run clean ISO through the Buckner in a hope to recover any oil that the Charcoal is holding. I don't use any DE because I use the Buckner filter paper as the filter.
Thanks for the reply Godfish.
I really hope it isnt a significant amount. Because as I said, I have been using liberal amounts. I wasnt concerned about charcoal wastage. I was more concerned with end result. Same as when I am using DE. So I really hope I havent been compromising THC/CBD content potential.

And as you said, I too run a rinse thru the Buchner with fresh solvent at same sub zero temp to reclaim residual. I am using a cereamic Buchner with filter paper and filter medium(s), not a fritted funnel. Is a fritted funnel better? DE scrubs as well does it not? That is why I have been using it.
 
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Godfish

15
3
Thanks for the reply Godfish.
I really hope it isnt a significant amount. Because as I said, I have been using liberal amounts. I wasnt concerned about charcoal wastage. I was more concerned with end result. Same as when I am using DE. So I really hope I havent been compromising THC/CBD content potential.

And as you said, I too run a rinse thru the Buchner with fresh solvent at same sub zero temp to reclaim residual. I am using a cereamic Buchner with filter paper and filter medium(s), not a fritted funnel. Is a fritted funnel better? DE scrubs as well does it not? That is why I have been using it.
I have very little experience with this and I'm reading like I have a test the next day, but from what I've seen DE is just an extra layer of filter? works like the filter paper, The Charcoal is what is removing color and taste. To be on the safe side, I use as little Charcoal as I can get away with to remove most of the green.

Do you know if it's better to decarb before QWISO or decarb the oil after? I'm having lots of issues with the decarb after, Not knowing if I'm going long enough or to long, My thinking now is to just decarb before at 240/40.

By the way have you gone through PsychedelicSam info on Grasscity? its really heavy to get through 1316 pages but so much good info and lab test data.
 
Eskander

Eskander

149
43
I can test loss with charcoal on a fairly small scale by dissolving some extract in 2ml of ethanol and then dividing that, adding activated charcoal to one and shaking it for a bit then centrifuging both tubes down, purging both tubes on some preweighed parchment and then weighing them both. To be fair I need to wash the charcoal tube at least once to limit loss from adsorption and I might as well purge that separately so we can see if a meaningful amount is just in matrix. After that I'll TLC them side by side so we will have the mass difference as well as concentration difference.

If the charcoal is a perfectly selective filter then the total extract mass will drop while concentration of THC goes up and the mass of the THC in both stays the same. I don't expect that.

-Eskander
Do you know if it's better to decarb before QWISO or decarb the oil after? I'm having lots of issues with the decarb after, Not knowing if I'm going long enough or to long, My thinking now is to just decarb before at 240/40.
So if you want bulletproof decarb after, boil off the solvent and then put the oil in one of these and put it in a pressure cooker and once at pressure cook it for 20min. 121C for 20min is a complete decarb. The only issue is that the off gassing of CO2 can pop the bag which limits how much can be put in each pouch. 25ml in the largest sized pouch seems to be about the right limit.

 
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Godfish

15
3
I can test loss with charcoal on a fairly small scale by dissolving some extract in 2ml of ethanol and then dividing that, adding activated charcoal to one and shaking it for a bit then centrifuging both tubes down, purging both tubes on some preweighed parchment and then weighing them both. To be fair I need to wash the charcoal tube at least once to limit loss from adsorption and I might as well purge that separately so we can see if a meaningful amount is just in matrix. After that I'll TLC them side by side so we will have the mass difference as well as concentration difference.

If the charcoal is a perfectly selective filter then the total extract mass will drop while concentration of THC goes up and the mass of the THC in both stays the same. I don't expect that.

-Eskander

So if you want bulletproof decarb after, boil off the solvent and then put the oil in one of these and put it in a pressure cooker and once at pressure cook it for 20min. 121C for 20min is a complete decarb. The only issue is that the off gassing of CO2 can pop the bag which limits how much can be put in each pouch. 25ml in the largest sized pouch seems to be about the right limit.

I sure this question has been answered before, but because BRO Science and what I suspect "censoring" it's hard to find an answer? The best info I could find was from "Media Bros" <--- LOL more BRO Science? they say it will adsorb cannabinoids and terpenes. So it's better to use as little Charcoal as possible?

Thanks for the tip on the pressure cooker bags, but at the amount I process (2oz every 2weeks) I'm not sure how to handle the small amount of goo in a bag? My wife would kill me if I buy more "more Fken weed stuff" I don't have a rotovap or fancy vacuum pumps, I use a small heated glass Essential oil Distillation apparatus for recovery of the ISO, it takes about 2 hours and I try to keep the heat to 190f I think this process is decarbing at the same time? that's why I wanted to decarb the oil after but it's confusing me and I don't want to over decarb.

The feedback I get is that it's good for pain but the buzz is not as good as smoking? I may need to just up my concentration in what I make?
 
Eskander

Eskander

149
43
Thanks for the tip on the pressure cooker bags, but at the amount I process (2oz every 2weeks) I'm not sure how to handle the small amount of goo in a bag?
I just suck it into a syringe with a blunt needle. It is hot enough that it flows freely and is easy to collect from the corners of the bags. Depending on your use, you could just toss a ml of MCT in the bag after you get what you can directly and then collect what dissolves in the MCT too.

-Eskander
 
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Godfish

15
3
I can test loss with charcoal on a fairly small scale by dissolving some extract in 2ml of ethanol and then dividing that, adding activated charcoal to one and shaking it for a bit then centrifuging both tubes down, purging both tubes on some preweighed parchment and then weighing them both. To be fair I need to wash the charcoal tube at least once to limit loss from adsorption and I might as well purge that separately so we can see if a meaningful amount is just in matrix. After that I'll TLC them side by side so we will have the mass difference as well as concentration difference.

If the charcoal is a perfectly selective filter then the total extract mass will drop while concentration of THC goes up and the mass of the THC in both stays the same. I don't expect that.

-Eskander
Hello Eskander, have you been able to test the Charcoal?

I made some pain cream with trimmings and leafs, it works, I think?..
 
Moe.Red

Moe.Red

Staff
Supporter
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Hello Eskander, have you been able to test the Charcoal?

I made some pain cream with trimmings and leafs, it works, I think?..
Lucky you, I've never gotten anything topical to work.
 
Eskander

Eskander

149
43
Hello Eskander, have you been able to test the Charcoal?

I made some pain cream with trimmings and leafs, it works, I think?..
No, been tied up with work.
Lucky you, I've never gotten anything topical to work.
I played with it a bit after I had an accidental exposure that floored me. Dosing is hard to control and the effect is enduring so if you go over, you are on that train for a while. Decided it wasn't worth pursuing unless I had someone that couldn't smoke, vape or take an edible which seemed unlikely. Dosing a delicate area seems to speed it up but the first time I got hit it was handing a shitload of edibles without gloves on so it clearly will go through fairly thick skin. Bear in mind the effect was like an edible, there was no discernible localized effect.

-Eskander
 
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Godfish

15
3
Lucky you, I've never gotten anything topical to work.
I used a paper shopping bag of leaf and trim, ground it all, ending up with 2000ml of plant matter, QWISO, distilled and decarbed it, added it to 237ml coco oil and 40g Bees wax, added Eucalyptus and Spearmint for smell.

I've never used a Topical cream like this before and I didn't know what to expect? I walk like a Pirate because of an Ankle injury long ago, The pain is constant and never ending. The first time I used it, It helped very little, 2nd time I had no pain. It lasts for about 4 hours, and sometimes I feel a little dizzy? I've never heard that you can feel effects through the skin? I'll have to be careful.
 

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