BHO + ethanol Solvent "Glass" Concentrate

[mrcryce]

Had 1/2 lb of popcorn laying around, trying to get something smokeable out of it. First ground it up with a coffee grinder, then placed ground up flowers into a stainless steel thermos, frozen in a container of ice, and put liquid butane into it. The butane maintains its liquid state because butane boils at -1 C while the ice surrounding the thermos is 0 c. Ambient temp outdoors is around 20 C.

0.25 lb of the ground up flowers in thermos


Poured it into here to be evaporated off. The butane dissolves THC and some other substances, leaving behind most of the plant matter in the coffee filter.



After the butane fully evaporates off, the sides of the container look like this:


The problem is, waxes and fatty lipids remain (which gives it the gooey texture). To solve this problem, we wash it in high concentration ethanol, a solvent which dissolves substances we want (like THC)

After putting in 300 mL ethanol, the glass looks like this



Notice all the fatty lipids floating inside the ethanol solution



Then this solution is spread over a pan and evaporated:


Then all scraped together with a razor blade. The consistency while cool is actually glassy, it will snap if you bend it. Once it gets to room temperature it bends though.


Darker area is where it bent over itself.



Then scraped together to condensed into a small block (5.5 grams, first run)




I am currently working on a batch of second run concentrate. First time I did not freeze the ethanol, this time I am freezing it for 2 days, before evaporating ethanol. Hopefully will be of even higher purity. I am also harvesting soon which will give me an opportunity to try this process out with fresh trim, which is supposed to be higher in THCa, which I have read contributes to the glassy quality of concentrates.

Pictures to come when I finish.

Comments and questions welcome.

 

[dc4]

Awesome.

.

 

[mrcryce]

Pictures from today's batch:

This is the coffee filter after the ethanol solution frozen overnight was poured into it. At this point, the solution had already been filtered through a coffee filter once as a butane solution.



Here is the final filter. The ethanol solution is taken from the freezer and put through this contraption, where it drips onto the collection tray. The thing underneath is a cooker used for double boiling the ethanol solution. Depending on how impatient I am this time, I may try to let the ethanol evaporate naturally, because I read it might increase the glassy characteristics of the final product. Also, trying to avoid any kind of unnecessary degradation of the final product through heat.

 

[cycleogic]

shouldnt have ground it up

 

[mrcryce]

shouldnt have ground it up

Going to try a run a run soon with some unground flowers, and also some unground fresh frozen trim.

Do u know if grinding it up yields more quantity of THC? I was thinking of maybe doing first run with unground, then after the first run, grind up the flowers/trim for second run.

 

[mrcryce]

Today's batch was made from unground Banana Kush flowers. I used a contaminated razor to collect it, otherwise it would have been much more pure looking. The impurities are actually visible as specs. Unfortunately this stuff still won't shatter at room temperature, but it will shatter when cold.

Rigged up a new collection system (16" diameter round metal sheet)





Ethanol while evaporating. Notice the whiteish looking pools vs the spots that dried yellow. I suspect the white pools color is caused by waxy substances floating on the surface of the puddle of ethanol. This means my filtration process needs work. Next time will try freezing the entire apparatus, and using smaller micron paper lab filters.




This stuff maintains shape at room temp, but u can see so many impurities in it.




Smokes GREAT. Smells fragrant like banana kush and tastes the same as it smells. The effect is exactly as expected from a heavy indica.

 

[sine143]

what was the input weight on the BK flowers? what was final yeild. do you think you could use an open blast tube that has been frozen alongside freezer cooled butane (just frozen cans of vector) straight into an ethanol transfer solvent and then proceed to evap from there? what benifits do you find from adding the extra ethanol step in your method?

 

[mrcryce]

what was the input weight on the BK flowers? what was final yeild. do you think you could use an open blast tube that has been frozen alongside freezer cooled butane (just frozen cans of vector) straight into an ethanol transfer solvent and then proceed to evap from there? what benifits do you find from adding the extra ethanol step in your method?

Input weight approx 7g, final yield about 0.8g. Not a great return, but this was just first run.

I have done frozen blast tube with frozen butane, but I used ground up flowers. I was just playing with a different method this time. Whats annoying about the blast tube method to me is constantly reloading the tube. With a thermos full of liquid butane, I can process almost 1/2 lb of ground flowers simultaneously. (But quality won't be able to get to "glass" level) I haven't tried to see how much un-ground flowers I can simultaneously process, but will be working on that in the upcoming week.

I am not a chemist so I don't know what interactions putting the butane straight into ethanol will cause, so I do it in two separate steps.

The ethanol step allows for higher thc content in the final product by removing more waxes and lipids (which give regular BHO its characteristic gooey/stickiness). Butane dissolves these substances while the ethanol does not. However my final product is still stickier than it should be, because some of those undesirable substances still can pass through a coffee filter. I am hoping using qualitative filter paper rated at low microns will result in a higher purity final product.

I know the ethanol step is having an effect because if u look above at the pictures, u see precipitate in the ethanol solution. Also, the ethanol solution passing through the same grade coffee filter miraculously yields a lot of crap filters out. (Also in above picture)

I forgot to upload earlier, but this is what the flowers look like sitting in a thermos of liquid butane:

 

[sine143]

i'm at about 1.1-1.35 on 7 gr flowers with a single vac purge (lab grade vacuum). consistency varies unfortunatly from wax to goo to glass.

 

[mrcryce]

i'm at about 1.1-1.35 on 7 gr flowers with a single vac purge (lab grade vacuum). consistency varies unfortunatly from wax to goo to glass.

Do you know what causes the variations? First run/subsequent runs? Flowers/trim? Ground/Unground, Fresh/Dried, etc?

My results so far indicate not grinding helps a lot to achieve more glassy consistency. I also read using fresh-frozen trim yields glassier product, which I will try soon.

I also read that THCa is the glassy form of THC, so weed with higher THCa content will be more likely to yield glassy extract. THCa turns into THC with time and heat I believe, hence the recommendation to use fresh frozen trim. I believe that generally plants grown in a colder environment will have higher THCa content, so I do not have high expectations for my trim extraction run (my temps are quite high, often in the 90s).

 

[sine143]

I actually had the chance to run this strain (sweet tooth) twice with a very long time period of time seperating the runs. First run was the day I got it, single 7 gram nugget in the turkey baster. yeilded 1.44 (20%). I ran some nug from the SAME hp, 6 months later (saved a half o in a mason jar for later date), and and I pulled 1.05. First run was crumbly/ opaque , later run was golden clear gum.

I dont know what alters the consistency honestly. If heat purging I think that significantly messes with the consistency based on heat and duration of exposure

Your hypothesis about THCa interests me. I found I almost always got an opaque wax if I heat purged, this MAY in fact be due to the THCa in my oil deoxycarbolizing into delta 9 thc. If this is true I would find it very interesting indeed. I think Terpine content also has an influence on the outcome too.

 

[mrcryce]

I actually had the chance to run this strain (sweet tooth) twice with a very long time period of time seperating the runs. First run was the day I got it, single 7 gram nugget in the turkey baster. yeilded 1.44 (20%). I ran some nug from the SAME hp, 6 months later (saved a half o in a mason jar for later date), and and I pulled 1.05. First run was crumbly/ opaque , later run was golden clear gum.

I dont know what alters the consistency honestly. If heat purging I think that significantly messes with the consistency based on heat and duration of exposure

Your hypothesis about THCa interests me. I found I almost always got an opaque wax if I heat purged, this MAY in fact be due to the THCa in my oil deoxycarbolizing into delta 9 thc. If this is true I would find it very interesting indeed. I think Terpine content also has an influence on the outcome too.

Your nug total yielded 35% of its 7g dry weight in concentrate? I think that is a clear indication that the process is picking up a lot more than just THC or THCa. Did u notice any difference in potency between your first run crumbly stuff vs the golden goo?

My "glassiest" products yet are the result of keeping the temperature as low as possible. Its too hard for me to judge the potency though. If high THCa content actually is the determinant factor in making shatter, the product may actually be weaker then because it is not all properly decarboxylated to THC. For me though, there is a certain appeal in creating the glassy look. (Watched too much breaking bad maybe ) Especially when considering the temperature that BHO concentrates are often consumed (vaporized at much higher than decarboxylation temperature), high THCa content concentrate may just be a gimmick with less potency. Looks so damn cool though.

 

[sine143]

I think you misunderstood. it was a first run product, on seperate A grade quarters that came from the exact same half pound. the only difference was the latter product had been stored long term for 6 months. Fresh batch was a 20 % yeild. 6 month old batch was around a 15%.

 

[cycleogic]

The point behind not grinding the bud is to decrease the extraction of chlorophyll so you have a cleaner product. Looks good though man

 

[mrcryce]

I think you misunderstood. it was a first run product, on seperate A grade quarters that came from the exact same half pound. the only difference was the latter product had been stored long term for 6 months. Fresh batch was a 20 % yeild. 6 month old batch was around a 15%.

Aaah, I see. Do you have any ideas on why fresh product yields more extract than product that has been in storage for a while? I just made concentrate from the sticky stuff on my fingers while trimming 500g wet, it was insane. I yielded 0.6grams of concentrate. (Just washing my fingers with ethanol and then filter + evaporate). Makes me sad to know I was throwing away so much before. The ethanol was a bright green color I'd never seen before.

 

[mrcryce]

The point behind not grinding the bud is to decrease the extraction of chlorophyll so you have a cleaner product. Looks good though man

Thank you for your kind words. I'm still learning too. For some reason though with this process, the resulting concentrate is always the same color for me. Even when I use fresh bud that has been unground! Is grinding the bud supposed to increase extraction rate while sacrificing purity of final product?

 

[sine143]

I always clean all my trimming tools by submerging in 91% iso and evaping. while the cannabis is wet the chlorophyll gets juiced out of it and ends up in the final hash product.

I think thc just degrades over time, even in jars imo. that being said some people cure for 6 months +

 

[mrcryce]

Did an extraction run with trim and popcorn buds (frozen for 24 hours right after trimming)



Submerged all into liquid butane


900 mL of liquid butane boiling off at ~70F. I sped it up by placing this container into a pot of hot water (if you want to try this at home do it outside)



After dissolving the BHO into ethanol which is then frozen for 24 hours and filtered...the final product.


FINALLY GLASS! The final product from this run was much purer, and MUCH more solid at room temperature. However, with the heat of my fingers, I can leave finger prints on it. It will shatter at a much higher temperature than my previous attempts.


I think using fresh materials, plus freezing it, was a big factor in the glasslike consistency of this product. It smells very aromatic like flowers (the subcool ripped x bubba raw material that it was extracted from). Also I believe with the butane + ethanol process, see-through purity like this will only be possible on first or second run.

 

[sine143]

looks tasty

 

[Bhobuddy]

I don't want to sound like a no it all but
i get different consistancys only when I don't clean my extractor
you have to clean it with iso every third time you run or the plant break matter gets into the oil
i hope that helps