How to perfect the process of extraction at home

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cronicoldguy

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So I have a dilemma. I have 2.5 gallons of solution to distill. Have been using a fractional still in the past. But it takes quite a while and needs to be monitored closely. Hoping @Moe.Red and others in the know will reply.

I already have a 5L glass jacketed reactor. Would it be as efficient and do as good as a job as a rotovap if I purchased a circulating heated water bath, and distilled with the reactor instead? I realize it wont be as fast, but will it do as good of a job?

I also already have a circulating chiller. But it only goes down to -5C. If I purchased a heater/chiller combo, I could extract, winterize, and distill in the reactor. I am already using it to extract. Works very well. Constantly stirring during extraction, and temp controlled if I had a heater/chiller. I made a cheesecloth bag and stainless steel cage that fits inside the reactor kettle. It retains the biomass for easy removal.

Reason I ask is because both are relatively the same price and I could really use the heater/chiller for the reactor. But at the same time, I want to be efficient and cost effective. The reactor is so versatile, I am leaning towards the heater.

I am wanting to purchase ASAP.

EDIT: Does anyone know if it is possible to configure 4X Soxhlet Extractors with my reactor? Would the 5L volume of the kettle have the capacity to supply 4 extractors at same time? Or is that too greedy? Maybe only 2 Extractors?
 
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Moshmen

Moshmen

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So I have a dilemma. I have 2.5 gallons of solution to distill. Have been using a fractional still in the past. But it takes quite a while and needs to be monitored closely. Hoping @Moe.Red and others in the know will reply.

I already have a 5L glass jacketed reactor. Would it be as efficient and do as good as a job as a rotovap if I purchased a circulating heated water bath, and distilled with the reactor instead? I realize it wont be as fast, but will it do as good of a job?

I also already have a circulating chiller. But it only goes down to -5C. If I purchased a heater/chiller combo, I could extract, winterize, and distill in the reactor. I am already using it to extract. Works very well. Constantly stirring during extraction, and temp controlled if I had a heater/chiller. I made a cheesecloth bag and stainless steel cage that fits inside the reactor kettle. It retains the biomass for easy removal.

Reason I ask is because both are relatively the same price and I could really use the heater/chiller for the reactor. But at the same time, I want to be efficient and cost effective. The reactor is so versatile, I am leaning towards the heater.

I am wanting to purchase ASAP.

EDIT: Does anyone know if it is possible to configure 4X Soxhlet Extractors with my reactor? Would the 5L volume of the kettle have the capacity to supply 4 extractors at same time? Or is that too greedy? Maybe only 2 Extractors?
Sorry I can not help here and Moe is on vacation , but I can bump it up to the top
 
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cronicoldguy

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Ordered! Hope this dont bite me in the ass! After two failed attempts ordering one from China, I said fuck it and ordered one from here in Canada.

Went with this rotovap: 2L Electric AquaVap Turnkey System

1668229850280

I already have the same circulating pump. Guess I have a spare now.
I really hope this works well for me. I wanted to go with a 5L unit that can utilize 1L and 3L boiling flasks as well. But cost was much higher, and a delivery date of over 1 month. I am already months behind. Not sure if getting the circulating water bath instead would have been a better move.
 
Eskander

Eskander

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Ordered! Hope this dont bite me in the ass! After two failed attempts ordering one from China, I said fuck it and ordered one from here in Canada.

Went with this rotovap: 2L Electric AquaVap Turnkey System

I already have the same circulating pump. Guess I have a spare now.
I really hope this works well for me. I wanted to go with a 5L unit that can utilize 1L and 3L boiling flasks as well. But cost was much higher, and a delivery date of over 1 month. I am already months behind. Not sure if getting the circulating water bath instead would have been a better move.

I'm pretty happy with my chicom rotovap but I got it off eBay from guys with American stock. Think I ended up paying a hundred more for it that the same ones on aliexpress but I think it is worth it not to deal with the issues you have had. I'd invest in a large receiving flask and an adjustable support for it. These guys make decent quality:

Proper chillers are crazy expensive for what they are. They don't seem to come up used and working for that much of a discount either. I thought about building a Peltier cooling array on a bunch of heat exchangers but found an easier solution.

For coolant I use a big aluminum pot full of antifreeze that I keep in a chest freezer. When running, 2 12v fuel pumps pull it through tubes in a foam lid I fitted to the freezer, through the condenser and back. Had one of these and was great while it worked:
Really high capture rates for delicate flavors at high vacuum and low bath temp. That mostly matters for making fresh brandy and stuff like that. Broke after 3 months but I paid for the 3 year coverage and they just refunded me cause they didn't have replacements in country at the time. If I hadn't just bought a -86C freezer, I'd get another and just swap them around as they go tis up. Regular chest freezers from Home Depot can do -25C though and that works just fine for simple ethanol recovery as long as your vacuum isn't pulling too deep of a vacuum.

Not sure I get the point in the CPF. Wouldn't you be better off with a chamber and a pump to circulate through the material under pressure? Would be a lot simpler and you would be able to run it with the solvent at whatever temp you want. A chamber like this but longer:
With DE filtration at the bottom and seals at both ends, you could force liquid though to extract then blow out the remaining solvent with air once you were happy with your extraction. Pressures would be higher since vacuum can't exceed 1 bar so flow should be faster. Clean out would be easy with both ends open, you could just push out the puck. Still seems like overkill given that everything we are trying to extract is on the surface of the material. Insulated bucket and a spatula to stir with is probably functionally fair close.

-Eskander
 
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cronicoldguy

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I'm pretty happy with my chicom rotovap but I got it off eBay from guys with American stock. Think I ended up paying a hundred more for it that the same ones on aliexpress but I think it is worth it not to deal with the issues you have had. I'd invest in a large receiving flask and an adjustable support for it. These guys make decent quality:

Proper chillers are crazy expensive for what they are. They don't seem to come up used and working for that much of a discount either. I thought about building a Peltier cooling array on a bunch of heat exchangers but found an easier solution.

For coolant I use a big aluminum pot full of antifreeze that I keep in a chest freezer. When running, 2 12v fuel pumps pull it through tubes in a foam lid I fitted to the freezer, through the condenser and back. Had one of these and was great while it worked:
Really high capture rates for delicate flavors at high vacuum and low bath temp. That mostly matters for making fresh brandy and stuff like that. Broke after 3 months but I paid for the 3 year coverage and they just refunded me cause they didn't have replacements in country at the time. If I hadn't just bought a -86C freezer, I'd get another and just swap them around as they go tis up. Regular chest freezers from Home Depot can do -25C though and that works just fine for simple ethanol recovery as long as your vacuum isn't pulling too deep of a vacuum.

Not sure I get the point in the CPF. Wouldn't you be better off with a chamber and a pump to circulate through the material under pressure? Would be a lot simpler and you would be able to run it with the solvent at whatever temp you want. A chamber like this but longer:
With DE filtration at the bottom and seals at both ends, you could force liquid though to extract then blow out the remaining solvent with air once you were happy with your extraction. Pressures would be higher since vacuum can't exceed 1 bar so flow should be faster. Clean out would be easy with both ends open, you could just push out the puck. Still seems like overkill given that everything we are trying to extract is on the surface of the material. Insulated bucket and a spatula to stir with is probably functionally fair close.

-Eskander
Thanks for the interest.

LeDab offered me a better price on the same stand-alone model I bought, but I would have had to wait for it from China. I could find better in my price range. But ran out of time. Ideally, I wanted a 5L with optional 1L and 3L evaporating flasks. I could get a R5001 clone with that config for $3600CAD, but had to wait another month for delivery.

As for chillers, yes, stupid expensive. I love your freezer idea though! I have this -5C 5L circulating bath.
1668489018061

It holds -5C with a 300mm Graham Condenser on a 1L and 2L fractional still no problem. So I am hoping it is sufficient for the 2L rotovap. Or am I going to need a heftier chiller?

Please, I have broad shoulders. If you or anyone see anything to pick apart, fly at it. Please point out my mistakes. There is likely lots of shit I have posted some are shaking their heads at. If so, please correct me. There is nothing worse than a forum full of bullshit. Not that it is the case here at THCFarmer. I just dont want to be talking stupid shit. I am here to learn and share.

"given that everything we are trying to extract is on the surface of the material."
The reason I was using the CPF was to ensure I was leaving nothing behind. The soxhlet process continually circulates a given volume of distilled ethanol until no available ethanol or user stopped. I only used it to pull the last bit after 2 soaks/washes. I can remediate most all undesirables, so I thought I would pull everything. Or is this pointless? Bad idea? Waste of solvent?

Now filtering. That is my next project. I am only filtering down to maybe 2.5 micron with a Buchner funnel and filtrate papers. If I am even achieving that. Also, is it best to do all filtering while in the extracted ethanol solution isnt it? I am hoping to find or somebody can point me towards an affordable simple filtering system. I want '0' particulate if all possible. Small batches, 0.25lb-1.0lb.

Can you explain DE filtration further? The biomass is sealed and pressurized for the 'soak', then released, passing thru filter(s)? If that is the case, I can already do that on small scale with a HTHP Filter Press I have. But only about a 1.0oz batch. I have used it to do BHO extractions as experiments. Can actually soak the biomass in butane with it.

Bottom line is I need to refine my post winterization filtering. I make my oil to vape. So I am targeting '0' particulate. At the end of the day, I want to be able to make the highest quality FSO in my own home. In time, I am hoping to venture into the world of distillates.

Thanks for taking the time to read. All suggestions welcome.
 
Eskander

Eskander

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It holds -5C with a 300mm Graham Condenser on a 1L and 2L fractional still no problem. So I am hoping it is sufficient for the 2L rotovap. Or am I going to need a heftier chiller?
If you are pulling a light vacuum and using a fairly high bath temp then -5C is just fine. Remember the 20 degree rule for rotovaps. The bath temp should be 20C higher than the BP at that pressure and the condenser should be 20 degrees or better colder than the vapor temp. Vapor temp will be way lower than the bath temp so the only way to know is with a thermometer in the vapor tube. A colder condenser will capture more and saturate slower so your solvent recovery rate will improve. At -40C I had to run insulation over the lines and put the pumps in a styrofoam box to keep them from condensing a half inch of frost but the capture rate was great and I could us a bath temp of 30C. That matters more for distilling things to drink then for solvent recovery though.
"given that everything we are trying to extract is on the surface of the material." The reason I was using the CPF was to ensure I was leaving nothing behind. The soxhlet process continually circulates a given volume of distilled ethanol until no available ethanol or user stopped. I only used it to pull the last bit after 2 soaks/washes. I can remediate most all undesirables, so I thought I would pull everything. Or is this pointless? Bad idea? Waste of solvent?

The beauty of the soxhlet is that it exposes the material to fresh solvent on every cycle which helps in extracting substances that have low Ka (or KEt I guess). THC is soluble at nearly 1:1 in ethanol and with a rotovap, we are recovering most of what we use. You can flood the material with several volumes of ethanol and waste very little. Soxhlet is going to be some pretty long cycles and a fairly small increase in capture efficiency over just a soak. Your rig would be good for testing that. Do a soak at room temp on a small batch and then run the same material in your rig and see if you recover enough to make it worth the effort. My swag is that getting another 5% would be optimistic but try it. You already have a functional set up that is good for methodological development.
Now filtering. That is my next project. I am only filtering down to maybe 2.5 micron with a Buchner funnel and filtrate papers. If I am even achieving that. Also, is it best to do all filtering while in the extracted ethanol solution isnt it? I am hoping to find or somebody can point me towards an affordable simple filtering system. I want '0' particulate if all possible. Small batches, 0.25lb-1.0lb.

Can you explain DE filtration further? The biomass is sealed and pressurized for the 'soak', then released, passing thru filter(s)? If that is the case, I can already do that on small scale with a HTHP Filter Press I have. But only about a 1.0oz batch. I have used it to do BHO extractions as experiments. Can actually soak the biomass in butane with it.

You can see the DE (Celite) filtering taking cloudy crap to clear as a bell in one pass here:
I tend to use a thicker cake of DE now with a coarse filter paper on top of it to keep the cake intact while pouring in what I want to filter. I also strain my wash through a nut milk bag to exclude the big crap. If you are going to do batches in the 1 pound range my suggestion would be to get a fairly large funnel. Even with a frozen funnel, it will help with winterization if you aren't filtering for an hour...
Best to have some chilled EtOH on hand to wash the filter cake free of residue after filtering for either particulate or winterization. It pulls fairly dry but the lessons beaten into me during Quant are not quickly shaken off lol...

To prepare the cake, just slurry the DE in clean ethanol and run it through to get it formed. You might see some DE get through the fritted glass so passing that ethanol back through the filter, and giving the flask a rinse with more clean ethanol isn't a bad idea. Making a charcoal cake on top of it is the same approach but nothing will pass through the DE. I find running green dragon through a charcoal cake is more effective than slurring powder into the green dragon and then filtering it. One pass essentially always does the trick but it is noticeably slower filtering than the DE alone. To clean the fritted glass, you can run room temp Iso through it a few times and if you feel it is still clogged, soak it in a hydrochloric acid bath.

I've also had decent luck with salting crap out of FECO with anhydrous magnesium sulfate. You add enough to get it swirling like a snow globe and that is a pretty good sign you have bound all the water up. Chill it to further to precipitate outs much as possible and you will end up dropping most of the sugars and protein from the plant material out of solution. You can then add water back to it to get to 95% so winterization will be more effective.

Recently I've been playing with decarbing flower prior to extraction rather than as oil but so far there seems to be less crap dissolved in the first place with decarbed flower. My guess is that the heat denatures the proteins in the cells and that matrix does a fair job of binding up sugars and other crap. End result of the FECO fraction (I'm doing a QWET wash first) is a lighter color for sure. Smell of decarbing is not subtle though lol...

-Eskander
 
Eskander

Eskander

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@cronicoldguy Not much going on today so I modeled the end caps for an extraction chamber like I mentioned. Capacity would be about 2 1/4 gallons and it aught to be fairly cheap to have the caps printed. Should go together with some 3/8 all thread and the following parts. End holes are sized for a 1/2 NPT and the caps can be SLS printed in nylon. Both the Viton O-rings and the Nylon are resistant to ethanol and all the materials should be tolerant of cryogenic temps. Only real question is what the pressure tolerance would be but a few atmospheres at least is a safe bet. I'd wear eye protection though...

Screenshot 2022 11 15 at 105900 AM



Here is the cap file:

With a DE cake at the bottom, you could circulate ethanol through it till your hearts content and go straight into a flask to rotovap. I think it is still over the top for a first pass but for a second pass to get everything, I think it will be faster and cheaper than the soxhlet. If you feel like trying this approach, order the tube and give me precise measurements on the ID and OD and I'll refine the model as needed.

-Eskander
 
Eskander

Eskander

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Also, because I like to give things the worst name possible; I dub this extractor "The Weedish Penis Pump".

Might actually make sense for Hexane extraction on fresh material. Closed loop to contain the funky ass nature of hexane. Drain it out and recharge with new material and run the same solvent across it until you have finished. Material compatibility is still there.

-Eskander
 
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Moshmen

Moshmen

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So I got a list from a extraction business that’s going under and selling everything
Large rotovap , chillers , vacuum pumps ect. If you guys are interested in the list message me and I can email it to you , there’s to much to post here , keep in mind most is commercial size equipment
 
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cronicoldguy

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@Eskander thank you very much for taking the time to reply. It is greatly appreciated. Please excuse my ignorance. I am learning as I go. I have very little chemistry (enough to be dangerous), but I have a knack for learning if I am interested. Creating the highest quality FSO is of great interest. Something I can be proud to say I made. This is more a hobby for me than anything. I have had pipe dreams of owning and operating an extraction business though. But only pipe dreams.

Again, sorry for my ignorance. I wasnt sure what you meant by DE. And yes, I am using Celite 545 and Activated Charcoal with a Buchner funnel. Prepared, dried, and froze. I was mixing the DE into a slurry right inside the Buchner on top of the filter paper. Your approach seems more logical. The very first time I used filtering mediums, I had made 1/2" cakes of each , charcoal above DE. I had also mixed charcoal into the ethanol solution. The end result was what you showed in the vid you linked, an amber liquid. The next few baches, I made a 1/2" DE cake but no charcoal cake. I had mixed approx. 4 table spoons charcoal into the gallon jar and stirred for about 10 mins on stirrer then winterized. End result was an amber liquid not different from filtering with a charcoal cake. I dont make a charcoal cake any more. I just mix it into the solution and filter it out with the DE. Should I still be making the charcoal cake layer? Prior to distillation, I pass the filtered solution thru 2X coffee filters.

With that said, I am still seeing particulate. That is why I asked about filtering in the previous post. How can I filter down to the lowest micron possible?

Onto FECO. Is FECO and FSO one the same? To be considered FECO, must the extract retain all attributes of the plant? Including fats, waxes, lipids, chlorophyll,....? Also, is an extract still considered FSO if it has been winterized?

Can you please explain your method/procedure of decarbing flower and oil? I have read so many different conflicting methods. Conflicting temps and times. I am scared to even decarb flower now. I vape my oil so decarbing shouldnt be an issue. No? Decarbing the flower makes the most sense to me because flower would be totally dehydrated and ready for extraction.

Thank you very much for posting the The Weedish Penis Pump. I was thinking of Soxhlet because the ethanol is being recycled thru-out the process. Less wastage. I realize I am recovering the majority of ethanol, but it becomes water contaminated with time/usage. To the point I wont use it for extracting. I will have a stock pile of useless ethanol. Although a feeble attempt, I have tried distilling the used ethanol to get it back to 95%, but have had no success.

Thanks!
 
Eskander

Eskander

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If there is a functional difference between feco and fso, I’m unaware of it. I think to call it rso, it needs to be the lowest quality of unrefined extract possible though…

If you are stripping color adequately in a slurry then by all means, keep at it. If you are going through celite and are getting particulate still, something is off. Are you using the funnel type with the holes poked in the base or the fritted glass type that I showed? My guess is that you have some liquid bypassing the cake somehow.

You can recover the ethanol to anhydrous With this:


Just keep adding it and mixing until it swirls around like a snow globe and then filter it and you are at 100% EtOH. That actually sucks for winterizing though and you need to add water to get it back to 95% there or the solubility of wax is too high.

For decarbing oil I either use a hot plate/stirrer or I put it in a retort pouch and run it through the pressure cooker for 20 min. Decarbing flower I do on cookie sheets in the oven. The retort pouch works there too but it ends up smelling like hay and tasting like ass.

-Eskander
 
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Godfish

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Getting to the goodness, Thank you guys. I'm reading and learning a lot.
I have a question about distillation, are lower temps necessary? I bought a small distillation unit off amazon does one thousand milliliters and uses a hot plate as a heat source for the flat bottom flask, no vacuum. Is the higher temps 180+ hurting the THC? what I ended up with makes you sleepy but not high? I decarb the oil, not the flower.

My process was QWISO after 24 hours in the freezer (2 pass 1min each)
then ran through filter to remove any plant material, comes out almost clear.
the oil i got comes out like a light honey, I then decarb the oil on a hot plate in a beaker until it stops bubbling.

Is it possible the oil is getting converted to CBN?
I don't use the oil for anything special just cooking, mostly making gummy bears
 
Eskander

Eskander

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Traditional distillation is fine. It will be slower and require more energy that distilling under vacuum but that is the only meaningful difference. The boiling point for iso is low enough that you aren’t really getting conversion to CBN in meaningful quantities. It is also an oxidative process and the solubility of gas (oxygen) in a boiling liquid is essentially zero so it is unlikely to happen at that step anyway.

When you decarb the oil, what temps are you getting it too, for how long and what kind of thermometer are you using?

-Eskander
 
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Godfish

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Traditional distillation is fine. It will be slower and require more energy that distilling under vacuum but that is the only meaningful difference. The boiling point for iso is low enough that you aren’t really getting conversion to CBN in meaningful quantities. It is also an oxidative process and the solubility of gas (oxygen) in a boiling liquid is essentially zero so it is unlikely to happen at that step anyway.

When you decarb the oil, what temps are you getting it too, for how long and what kind of thermometer are you using?

-Eskander
I used 242f I did it on the hot plate in a pot half filled with canola oil, and a candy thermometer, after the temperature stabilized I then put the oil into decarb. I didn't do it in the oven because I thought the oven temperatures would go too far out of whack.
 
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cronicoldguy

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If there is a functional difference between feco and fso, I’m unaware of it. I think to call it rso, it needs to be the lowest quality of unrefined extract possible though…

If you are stripping color adequately in a slurry then by all means, keep at it. If you are going through celite and are getting particulate still, something is off. Are you using the funnel type with the holes poked in the base or the fritted glass type that I showed? My guess is that you have some liquid bypassing the cake somehow.

You can recover the ethanol to anhydrous With this:


Just keep adding it and mixing until it swirls around like a snow globe and then filter it and you are at 100% EtOH. That actually sucks for winterizing though and you need to add water to get it back to 95% there or the solubility of wax is too high.

For decarbing oil I either use a hot plate/stirrer or I put it in a retort pouch and run it through the pressure cooker for 20 min. Decarbing flower I do on cookie sheets in the oven. The retort pouch works there too but it ends up smelling like hay and tasting like ass.

-Eskander

Again, I am very grateful and appreciative for the time spent by yourself and @Moe.Red replying to my questions. Forums can be an invaluable wealth of knowledge. But please forgive my ignorance. Some questions I ask may seem elementary to some. I would rather ask a dumb fuckin question and face the backlash, than having a major fuckup. My prerogative is; its only dumb question if a person asks more than once. My chemistry is basic at best compared to some here. Might take me a bit to grasp concepts. But like I said in a previous post, if I have interest in something, I have a knack for learning. Fuck, I dont even really know the difference between sativa and indica. Dont really care. All I care about is if it fucks me up, its all good. This "day time high" or "wheelchair high" thingy dont matter to me. I dont buy shitty weed. I consume for the effect. Strain dont matter as long as it is heavy.

Off topic, but a funny story. I extract in a reactor. After an extraction of Cotton Candy and draining, the valve was dripping. I stuck my head under it and licked the valve a few times as it dripped, thinking I might get a buzz. I likely consumed maybe 0.5ml-1ml. Didnt get a buzz, but my tongue was numb for about 4 hrs. LOL. Great local?

"If there is a functional difference between feco and fso, I’m unaware of it."
Thanks for the confirmation. From my understanding, I had the same conclusion.

But is an extract still considered FSO or FECO if it has been winterized? I ask because a few compounds are participated/filtered out in the process, leaving the extract 'not whole'. So technically, would it no longer be considered FSO/FECO?


"If you are stripping color adequately in a slurry then by all means, keep at it."
I believe I am stripping colour adequately. Always amber to clear. But my question comes from your comment about the oil tasting like ass.

The batch I mentioned I filtered with a cake of charcoal in tandem with DE, the oil tasted spectacular. Very flavorful. Tasted like the aroma of the bud. All batches without didnt. Could that be why? I noticed any jars I winterized with charcoal present inside, the residual smelled worse than ass. So your comment had me thinking.

"You can recover the ethanol to anhydrous With this:"
1) So, Magnesium Sulphate (Epsom Salt) will do the trick. If I were to source it locally, could I just use any Epson Salt as long as it is pure? And is room temp OK to mix?
2) I am going to order the exact product you suggested. Can you give me a ballpark figure as to how much required mg/L for lets say 80%-85% ethanol? This will give me an idea as to how much to order so I have a sufficient stock.
3) So once the ethanol is anhydrous, it will extract better. But for winterization, a water emulsion is desired? So it is fine to extract with 100% ethanol, but emulsify 5%/vol water prior to winterization? As with an emulsified oilwell drilling fluid, I would love to keep water content minimal. Is it possible to remove that 5% from the extract? I can do it with hot lime in an oil based drilling fluid. Mind you these are light oils. Distillates or diesel fuel. Is there a friendly way to do it?

"For decarbing"
No offense, but this is the typical reply given. Yes, I know heat and time are required for decabarboxyltion. Regardless of flower or extract. And aware can be done with an oven or heated stirrer. But can you be specific as to times and temps for both? What works for you? This is the problem I am facing. Enough info given to make a person "dangerous", but not enough to get the job done competently. There is still so much secretcy in the cannabis world.

Thanks, The Old Guy
 
Eskander

Eskander

139
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But is an extract still considered FSO or FECO if it has been winterized? I ask because a few compounds are participated/filtered out in the process, leaving the extract 'not whole'. So technically, would it no longer be considered FSO/FECO?
I would say it still falls under the FECO/FSO umbrella. It certainly wouldn't qualify as QWET or distillate. I kinda assumed that the order of things went from RSO being extract full of garbage to FECO/FSO being as much garbage removed as possible while still being a long room temp soak.

"If you are stripping color adequately in a slurry then by all means, keep at it."
I believe I am stripping colour adequately. Always amber to clear. But my question comes from your comment about the oil tasting like ass.

The batch I mentioned I filtered with a cake of charcoal in tandem with DE, the oil tasted spectacular. Very flavorful. Tasted like the aroma of the bud. All batches without didnt. Could that be why? I noticed any jars I winterized with charcoal present inside, the residual smelled worse than ass. So your comment had me thinking.
I think it is possible that this relates back to still being cloudy after filtering. The charcoal exposure should be functional either way. Filtering through it might create an even finer filtration cake if it is finely ground though.

"You can recover the ethanol to anhydrous With this:"
1) So, Magnesium Sulphate (Epsom Salt) will do the trick. If I were to source it locally, could I just use any Epson Salt as long as it is pure? And is room temp OK to mix?
2) I am going to order the exact product you suggested. Can you give me a ballpark figure as to how much required mg/L for lets say 80%-85% ethanol? This will give me an idea as to how much to order so I have a sufficient stock.
3) So once the ethanol is anhydrous, it will extract better. But for winterization, a water emulsion is desired? So it is fine to extract with 100% ethanol, but emulsify 5%/vol water prior to winterization? As with an emulsified oilwell drilling fluid, I would love to keep water content minimal. Is it possible to remove that 5% from the extract? I can do it with hot lime in an oil based drilling fluid. Mind you these are light oils. Distillates or diesel fuel. Is there a friendly way to do it?
Epsom salt is magnesium sulfate hydrate and has essentially zero water binding capacity. you can bake that extensively and it will release the bound water to become anhydrous MgSO4 but I wouldn't really bother. The anhydrous stuff I linked isn't that different in price than epsom salt. 1g of MgSO4 will bind roughly 1g of water. If you have 1 liter of 85% you need to add roughly 150g.

Water and ethanol are a solution not an emulsion. Emulsions are usually cloudy like when you add water to Raki or Ouzo and they go from clear to cloudy called "breaking". That is the oil dissolved in the ethanol being pushed out of solution by the increased water ratio. Drilling muds as I understand them are suspensions that are under high shearing loads which keep the solids suspended while in use. True emissions are stable aqueous/organic mixtures like milk or mayonnaise.

Going from 100% to 95% helps break the solution during winterization and drops the less soluble wax into an unstable suspension. Once you are done reducing the winterized solution in a rotovap, you need to boil off the residual ethanol somehow and boiling off the water at the same time just involves slightly higher temps.

"For decarbing"
No offense, but this is the typical reply given. Yes, I know heat and time are required for decabarboxyltion. Regardless of flower or extract. And aware can be done with an oven or heated stirrer. But can you be specific as to times and temps for both? What works for you? This is the problem I am facing. Enough info given to make a person "dangerous", but not enough to get the job done competently. There is still so much secretcy in the cannabis world.
For oil I like 121C for 20 min in a hotplate and for flower 250F for an hour in an oven. You are getting to the point where the better answer is, you need to do some TLC testing and refine your method though.

Back to drying... Nothing precludes adding drying agent to the extract. I'm washing several bags of trim here that are all at 20% RH and I'm periodically drying it back out and filtering it as I process the trim. It is all going to be filtered anyway and some soluble crap from the plants will get salted out if it is anydrous upon filtering. Before the last filtration, I'll chill it to reduce the solubility of remaining salts, sugars and protein.




-Eskander
 
C

cronicoldguy

55
18
I would say it still falls under the FECO/FSO umbrella. It certainly wouldn't qualify as QWET or distillate. I kinda assumed that the order of things went from RSO being extract full of garbage to FECO/FSO being as much garbage removed as possible while still being a long room temp soak.


I think it is possible that this relates back to still being cloudy after filtering. The charcoal exposure should be functional either way. Filtering through it might create an even finer filtration cake if it is finely ground though.


Epsom salt is magnesium sulfate hydrate and has essentially zero water binding capacity. you can bake that extensively and it will release the bound water to become anhydrous MgSO4 but I wouldn't really bother. The anhydrous stuff I linked isn't that different in price than epsom salt. 1g of MgSO4 will bind roughly 1g of water. If you have 1 liter of 85% you need to add roughly 150g.

Water and ethanol are a solution not an emulsion. Emulsions are usually cloudy like when you add water to Raki or Ouzo and they go from clear to cloudy called "breaking". That is the oil dissolved in the ethanol being pushed out of solution by the increased water ratio. Drilling muds as I understand them are suspensions that are under high shearing loads which keep the solids suspended while in use. True emissions are stable aqueous/organic mixtures like milk or mayonnaise.

Going from 100% to 95% helps break the solution during winterization and drops the less soluble wax into an unstable suspension. Once you are done reducing the winterized solution in a rotovap, you need to boil off the residual ethanol somehow and boiling off the water at the same time just involves slightly higher temps.


For oil I like 121C for 20 min in a hotplate and for flower 250F for an hour in an oven. You are getting to the point where the better answer is, you need to do some TLC testing and refine your method though.

Back to drying... Nothing precludes adding drying agent to the extract. I'm washing several bags of trim here that are all at 20% RH and I'm periodically drying it back out and filtering it as I process the trim. It is all going to be filtered anyway and some soluble crap from the plants will get salted out if it is anydrous upon filtering. Before the last filtration, I'll chill it to reduce the solubility of remaining salts, sugars and protein.




-Eskander
"Water and ethanol are a solution not an emulsion."
Yes, my mistake. Two different terms. Habit I suppose. Thanks for pointing that out. I was confusing with drilling fluids. An oil based drilling fluid (Invert) is typically an oil (usually a distillate) and water emmultion. Generally in a 85:15 ratio. Chemical emulsifiers are used to bind the two. Viscosifiers added to suspend solids.

"1g of MgSO4 will bind roughly 1g of water."
Thanks. Nice to have an idea. Coincidentally, that is the same rule of thumb I use in treating out water in a 100% 'water-free' and zero solids oilmud. 1KG of Hot Lime will remove 1L water. A retort is run to establish oil/water/solids. Although this process had been used before, the company I was working for then, received a patent for using Processed Lime (Hot Lime) to maintain an anhydrous oil based oil/gas well drilling fluid. The system was called Canoil. This was our bread and butter. Super fast penetration rates.

"Once you are done reducing the winterized solution in a rotovap, you need to boil off the residual ethanol somehow and boiling off the water at the same time just involves slightly higher temps."
This I have been doing on a heated magnetic stirrer at about 100C. End point being when no more bubbles. Is that acceptable? Or should I have the higher temp for decarb and water evap?

"Back to drying... Nothing precludes adding drying agent to the extract. I'm washing several bags of trim here that are all at 20% RH and I'm periodically drying it back out and filtering it as I process the trim. It is all going to be filtered anyway and some soluble crap from the plants will get salted out if it is anydrous upon filtering. Before the last filtration, I'll chill it to reduce the solubility of remaining salts, sugars and protein."
Again, please excuse my ignorance. Could you please explain further? Adding drying agent to extract solution? So there is no chance there could be residual salt in finished oil?
 
Eskander

Eskander

139
43
"Once you are done reducing the winterized solution in a rotovap, you need to boil off the residual ethanol somehow and boiling off the water at the same time just involves slightly higher temps."
This I have been doing on a heated magnetic stirrer at about 100C. End point being when no more bubbles. Is that acceptable? Or should I have the higher temp for decarb and water evap?

If you are not intending to decarb the oil but want water gone, it should be mostly gone around 105C but decarb rate is going to be very slow You will still have tiny amounts tied up in the oil unless you purge a thin film of it in hard vacuum. Whether that amount of water makes any functional difference is application dependent. If you are going to decarb then just take the oil up to your preferred target. At 100C your decarb (which is a time and temp dependent reaction) will take at least an hour to complete and may only be at 95% or so even then.

If you google around you are bound to find this chart:
Decarb1

The decline after the peak in the higher temp decarbs is supposedly do to conversion to CBN but having tried it I would say this chart is what we in the biochemistry field call "fucking wrong". THC to CBN conversion is pretty damn slow and in an oxygen free environment is essentially zero. The peak at each temp is probably pretty close and this chart supports that:

Decarb2

For me, I like 121C for 20 min and TLC indicates that I'm getting completion at that point. I was doing it to dry in a stirrer hotplate and then using retort pouches in a pressure cooker to decarb but the difference in the result was pretty hard to detect and it required more effort. For anyone without a chemistry set, it is still a decent approach that is hard to screw up though.

"Back to drying... Nothing precludes adding drying agent to the extract. I'm washing several bags of trim here that are all at 20% RH and I'm periodically drying it back out and filtering it as I process the trim. It is all going to be filtered anyway and some soluble crap from the plants will get salted out if it is anydrous upon filtering. Before the last filtration, I'll chill it to reduce the solubility of remaining salts, sugars and protein."
Again, please excuse my ignorance. Could you please explain further? Adding drying agent to extract solution? So there is no chance there could be residual salt in finished oil?

Some residue is going to happen but it doesn't matter. MgSO4 is listed as insoluble in anhydrous ethanol but that usually means that solubility is still going to be there in the mg/L range. It doesn't matter though as you are already getting salts from the plant along with proteins, sugars and other random phytochemicals. The solubility of the MgSO4 and other salts in anhydrous EtOH or Iso is temperature dependent though and chilling the solution will force more of that out of solution. I'd wager that on balance, soaking all the water up in MgSO4 will result in significantly less salts and other crap getting into the oil in the end since sugars are also insoluble in alcohol.

Once you get to decarb, the solubility of all that crap drops to zero. You may have seen clumps of back tar or translucent sludge in decarb and that is protein and sugar being forced out of solution respectively. I've only once had any visible salt come out of the oil that was white and sand like. That was probably the result of me not adding enough MgSO4 to get all the way to anhydrous. It was easy to avoid as it was bound up in sugar sludge anyway.

-Eskander
 
C

cronicoldguy

55
18
So, having major issues with vacuum. Cant seem to get vacuum deep enough. Lowest pressure I can get is 411 Torr. Using a 1L fractional still. Has 7-8 glass joints. I greased the living shit out all joints, rotating male/female connections for clear and see-thur glass. I even used teflon tape to no avail.
Tried running 2 pumps in tandem. No go. Has got me fucked trying to figure out issue. I think either pump alone should be able to pull a deep enough vacuum.
Well, the issue was the grease I was using. I tried DuPont Molykote 55. It was the closest to vac grease I could get locally at that time. I read that it worked as a vacuum grease. DuPont being a big brand, I felt confident buying it. Later that day, I ordered the Haynes grease off Amazon. I was thinking the Molykote was a higher quality grease, so that is what I used first. It is too thin and 'greasy' to work as a vac grease. High potential for contamination. Very messy as well.

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.


This grease works very well. Food grade, non-toxic. No mess. Cleans up easy.
1669398722577

A note to those at my modest chemistry level or lower: When fitting glass joints together for say a fractional still, ensure joints are 'bottomed out'. I grease lightly approx. first 10mm of female and male connections. Rotate as pushing together. You will feel it bottom out. Joint should look clear if proper coated.

When distilling under vacuum with a fractional still. Again, my modest experience. If you have limited equipment, such as no vacuum regulator (I have a J-Kem but need a cold trap) and shitty heating mantle (me, no control below 80C), it can be done easily but must be closely monitored. This is what I do:
1) Bring solution to boiling temp, I shoot for 36C-38C. Then turn off power to heating mantle or heat source.
2) I then lower vacuum pressure to around 0.08mpa, and it begins to boil. Be very careful not to bump. Control vacuum pressure with an auxiliary valve anywhere in the loop. Preferably as close to vac source/inlet as possible.
3) Adjust vac pressure to maintain a steady boil, then leave it. When temp drops and boiling starts to slow, turn heater back on at full power until solution is steadily boiling again, then shut off. Be careful, dont get too aggressive or it will bump. Repeat cycle as required to complete the job. You can get a fairly aggressive 'boil' without it bumping.
*****Once you have initially established vacuum pressure, leave it constant. Only adjust the heat. With only one variable, it is easy to control. I was able to distill 1700ml solution in a 1L still without one bump. If you do end up bumping accross badly, it isnt the end of the world. If just lightly, then just continue on. Maybe discard the contaminated distillate. If it was a heavy bump and a considerable amount of solution is in receiving flask, start over. Pour the receiving flask back into boiling flask and start over.

This is a ghetto approach, but works. I am sure a few here will have a chuckle, but hey, it works for me.

Now cost:
The simplest way to distill the solution is in a Source Turbo. Relatively safe as well. Minimal skill level required. Cost is $700-$800CAD. But batches are limited. Great for a person that just wants to process up to an ounce or so. Any batch larger takes forever. I have one, but havent used it since I put the still together.
Now if you are half-assed competent, have bigger batches, and want to play Proffessor Kitzel, a fractional still works very well and much faster than the Source Turbo. Ideally, a rotovap would be in order. But most cant afford one or use it enough to justify the cost.
A basic 1L Fractional Still setup with a circulating vacuum pump can be sourced much cheaper than a Source Turbo.

My disclaimer: I am by no means a real chemist. Self taught. If following my advise, you are on your own. I am only suggesting what worked for me. There are others here leaps and bounds above me. If those people can see errors, criticize, or can suggest a better approach, please chime in.

My Rig:
 
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