Decarbing gone wild

I was purposefully leaving some in for the previous reruns of kief. It was easier to transfer, but in the end i stopped and just leave what doesn’t come out for the next run.

transfer solvents are useful. was just concerned that somebody had taught you to add ethanol before decarbing for some bizarre reason.

as @StoneD pointed out, performing your solvent removal under vacuum will get you to the decarb step faster.

What temp are you running your ethanol extractions to generate the crude? What steps are you taking between EtOH and SPD flask?

Initially did them at -20c, overnight soak. The reruns have been at room temp between 6-20h. After I’m done with the kief its back to -20c and 10 minute soaks, just plant trim and nugs. Then ive just filtered it 2-3 times. Thought my smallest paper was 0.45 micron. Turns out it’s 1.5-3 micron. I haven’t started degumming yet. I tried cbleach once. But now it’s just filter paper. Then roto, decarb and into the spd.

Sugars from kief is a hard sell, sugars from plant matter that was within the size cutoffs to be called kief are not. Especially at room temp. I imagine that would also mean your (kief) extracts are green.

Although that definitely depends on how your kief was acquired.

It’s made through the resinator, blowing co2 through a middle bar while tumbling it. There is more plant matter in there than they thought.

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is this what you’re using?
http://www.theoriginalresinator.com/category-s/234.htm
plant matter does get pretty brittle at those temps.

using in house analyics to figure out when (time wise) potency starts decreasing (ie kief was now being diluted with ground plant material) might help figure out the best way to use that critter.

are your rm temp EtOH kief extractions green?

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Yup, that’s the thing used. The tinctures are green indeed. The entire thing looks black when in 5gl containers. So far I’m on the 4th wash and am still pulling something.

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Yuck! did you feed it fresh biomass? or cured.
Fresh would definitely explain the color you describe. and sugars crashing out, caramelizing and then carbonizing as you increase the heat.

how long are you harvesting for? are you actually able to get a weight on your yield? what happens next. I can’t bring myself to read that website. it’s just so full of gobbledegook.

if you’re not already, freeze drying your “kief” before going into alcohol would be a good idea . get as much water out a possible. you don’t care about terps, so you could even decarb at this step (so maybe just dry & skip the freeze :wink: ). don’t know. just know that if you add too much water to your alcohol, it won’t pick up all the cannabinoids. enough, and it will drop them all. see louche

Edit: when you say wash, you’ve added an aqueous (water based) wash step?

Wrong vernacular. By wash, i mean soak. I have only used 190 organic etho. I’ve not done the growing, harvesting or running of the kief. I’m just processing it. Initially did the first soak at -20c, both etho and kief in freezer before extraction. After I’d gone through everything it didn’t meet my calculations, so i went ahead and resoaked, filtered and rotoed and saw that there was more in there. Then it just takes time filtering and reclaiming the etho, so soak times are extended for the resoaks.

Edit: i tried decarbing kief in a crockpot, it worked quite well. Then i abandoned that for doing it in the oil stage.

now I’m with you. thanks. except i’m still not certain if the kief was made with fresh frozen material. if it was, and you extracted at rm temp, you may have picked up enough water to start losing cannabinoids.

you can also use louching to figure out when you’ve gotten all the cannabinoids (assuming no access to GC/TLC/HPLC etc). if you add water and you get milky ppt, you’ve still got cannabinoids in there, and need to go again.

Yeah, i haven’t looked into using water for louching purposes yet. Gonna most likely start degumming soon. So that’s gonna be my first water use.

Sooooooo. I tried decarbing in the bf, didn’t go as planned. To say the least. I was resoaking a bunch of kief and I started with throwing everything in the roto to get the most of the etho out. Started with 3l crude. To my surprise a lot of etho came out. At 2l etho recovered i stopped. Threw it in the spd and hadn’t preheated the system. When i got vac and temp going the weirdness started. As the vapor temp started rising the bf temp plummeted. Went down to 17c when vapor was around 40-50c. It never really went full muffin but was creeping up the head slowly. In the meantime etho started blasting through the condenser to the 3 way valve and hit the cold trap so hard it was spinning. Eventually the trap got full and i noticed the pump had oil coming out and i had to drain it fast. After that i had to drain the trap too.

The rest of the run was a cluster fuck. I learned a lot a valuable things… Not sure I’m gonna be decarbing in the bf. Need more research. Thanks @anon42519203 for warning me about the need for dry ice under the receiving flask. Normally i don’t need it, but now i know…

turn your vacuum down a smidge.

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Sounds like you didnt finish the ethanol recovery. The temp in the flask plummeting was probably due to the increased speed of ethanol removal cooling as it was removed. Due in the most part to the vacuum on the system. Its always good to keep a record of how much material went in before winterizationz you loose about 20% to winterization on typical bho. So if you start with 3L and end up with 3L after winterization and ethanol removal. You have 600ml of ethanol ~ roughly to remove. You can do this wtth the spd. Or the roto would be better. Time to probably upgrade your roto parts. Deeper vacuum and better cold trapping to keep it removing down to ultra low levels of ethanol. Then hot swap it into the spd. OR. Use a diaphragm pump on your setup spd and remove the rest of the material in there with a pump that can handle the vapor load and flasks you plan on changing before running. Keeping in mind your expected amount of oil and ethanol. That should make it easier to handle. The muffin was due to the ethanol fighting through the material.

Decarb wont really happen until 80C and above. Then its important to follow procedure and never turn off the vac during an in spd decarb. Turn down the stir bar or turn off the heat or both. But never stop the vac. It sometimes can energize it when its turned back on and create a muffin that cant be stopped again until its finished itself. Which could mean flooding your entire system with material and forcing you to start over

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I roto at 47-58c in the waterbath and vac at 30-50 torr. Chiller set to -21 with it getting up to around -5-0c after 5l recovery between 38-50 min. 10l roto. Spin is at 69-73 mostly.

I started leaving more etho in to aid in transfer, but after this I’ve stopped and just increase temp to 70-80c with no vac after I’m done recovering.

Edit: I’m gonna slowly try out bf decarb, but for now I’m thinking oil baths at 121 in 5l beaker with overhead stirrer. Should give good results as long as i keep stirring the edges.

Lower vac depth. Under 10 torr for roto.

You can keep the etho for the spd. Then ya, just distill it out and then start over after cleaning and letting it cool. That way you can pull a full vac. At cooler temps, which helps for overcoming decarb. Deeper the vac… better you get through decarb. Just pay attention to spin of the stir bar… it can create alot of the issues

I don’t believe his rotovap chiller will keep up with that vac level. without dropping the temp. at least until the solvent is gone.

I’m really just miffed that I said less vac, and you said more :slight_smile:

I want us both to be right.

Chiller keeping up is based on the amount of watts of cooling. Which is entirely based on what chiller hes using on. Not the vacuum depth.

You can do the same thing with higher temp and higher vac, but you approach decarb temps and whatnot which can cause issues on its own.

I’m using AIs 17l -30 chiller.

1750w at 0c
1100w at -10c
700w at -20c
300w at -30c

Edit: i have 2 poly science -60 immersion probes. They haven’t worked out that well in normal cold traps, until i put both in the laminar path cold trap. I’m gonna try and set them up chilling a coil in iso with the eg/water going to my condensers. Hoping to get more cooling power like that.