Hey G_Boe or anyone else - quick question regarding filtration for winterization processes.
I currently utilize the Whatman 1 (qualitative) filters stacked in triplicate and then inside coffee filters as well. Do you feel these filters would be sufficient to create a bed of CLite, bentonite, and/or AC for filtering? It states these are 11micron filters, although they are not ashless, I have plenty of them on hand.
CeliteÂź 545 has a particle size of 0.02-0.1 mm, or 20-100 micrometers (micron) so yes your filter paper should be sufficient.
Ok great!
I will be finding out by Friday if the sediment in question is in fact a water soluble or not. I assume this should help identify whether the issue I am seeing is due to water solubles where a bentonite would be needed to remove this issue, or if I should stick with a Celite and AC scrub.
Thanks Scooby
You could try to add a dessicant to the solution to see if you can get the compounds that are causing the murkiness to redissolve back into solution once the water is gone. If they did dissolve back into the solution then that shows you its an excess of water causing that murkiness. The same thing happens when people add water to alcohol in a procedure called louching.
I recommend MgSO4 since its cheap and easily available at any grocery store as epsom salt, although when you buy it its in its hydrated form and must be baked to remove the water.
From what you described it sounded like water must have collected in the solvent when you let it sit overnight in the bucket. Did you have a lid on your bucket?
Make sure after Degumming You wash with Brine and plain water to get all citric acid and Carbonic acid out
Very true, its interesting because its extremely cloudy in the alcohol solution and then when sitting overnight it settles into a mass of build up at the bottom, causing me to stir up everytime I refill the receiving flask on the rotovap.
We have a lid on the reaction buckets that contain the solvent, but leave them cracked open since the solution is still slightly bubbling (i assume from the CO2 generation of the ethanol and dry ice).
Sounds like the cloudiness is just small crystals precipitating that if left alone will settle, this is a good thing because it means what youre seeing isnt some kind of emulsion happening. This is an example of âantisolvent crystallizationâ.
The water is acting as the antisolvent to reduce the affinity of the waxy compounds to the ethanolic solution and thus causing them to no longer be soluble in the solution.
Also if dry ice is still bubbling from the solution the there is no question what happened, water vapor from the air condensed in the cold alcohol. Easy fix.
Yust remember to reproof that ethanol Well before Reusing iT s probably not at 190 proof Any more 
So yes ? You can set up the degumming step , sep funnel, heptane, 4:1 hep to crude. Then add water to a 1:1 of that total amount. Mix shake and apply Citric and BS appropriately. Check the ph before and after adding until its at 7. Check ph while in the sep funnel after drainging water ? Just trying to understand the little things and also the main concept ha.
Phcan only be read in the présence of water so not sure If measuring the heptane Will work
But You can deffenatly read the rinse water
And dissolve Some pure crude in ethanol or Any alcohol
Degumming in a sep might not work so Nice for sometimes the fats floculate and might clogg your sep funnel
Damn, I need to investigate this if thatâs the case. Itâs a newer container of ethanol however we uniquely identify every jug of alcohol used in an extraction to understand our recovery and use in each process.
Scooby, the solution after extraction will definitely continue bubbling after extraction so we crack the lids overnight until its near room temp to introduce to the rotovap so we dont stress any glassware. In the morning the bubbling has stopped, but I have observed this for several hours after an extraction, possibly because there could be small particles of dry ice left that we could not remove. With that said, youre saying that its absorbing water from the atmosphere in the process - whats the best method of remediation on this? Bentonite filtration prior to introducing to the rotovap or something more complex?
THanks!
Just so everyone can see, and hopefully learn from any of this as they get started in these processes, here is some photos this morning of a reaction bucket.
You can see the color leaves much to be desired, but the settling of particulate is at the bottom of the bucket, the liquid is fairly clear all things considered.
Give it a little stir up, and look how cloudy it becomes which in turns becomes part of the rotovap process, and ends up in the final products a bitâŠalso explains our very high byproduct weights after buchner filtration and winterizing.
What is the plant material like that you extract from? The more ground up it is the more particulate you will have to remove from your ethanol. DE, Celite, or bentonite (t-5) will all work as a filter to remove that particulate.
Bentonite will also provide the added benefit of removing water soluble components, further improving the potency of your crude, and vastly reducing or removing burnt on particulate when decarbing.
If you are only leaving a small opening (leaving the lid cracked open) I donât believe you would have an appreciable amount of water absorbed over night.
Ideally, I believe you should be removing all plant particulate, then fully winterizing, then continue on to any other steps you want to pursue (degumming, brine wash with LLE).
In my lab, we are limited to using only ethanol as a solvent. I can tell you that it is possible to create a high quality crude using only ethanol. Cryo wash 10 minutes -->filter all plant matter outâ> filter through bentonite to remove fines and water solublesâ> winterize if you arent sure if you pulled any fat/waxes -->roto down to loose syrup -->decarb 250 C in a vacuum oven, under vacuum.
Thats basic process that has works for us. Makes Short path crude that is clean and odor free. Normally tests around 75-80% delta9
Try going a bit longer on your soak. I do up to a 40 min with the same color results as my previous 25min soaks. All cryo temp.
Edit
Filtered only with fritted disc buchner funnel and celite 545.
I may look into the bentonite as its cheap
Have you compared yields/potency at all when doing longer soaks? In my experience, all readily available cannabinoids are dissolved in the ethanol quite quickly. I have compared yields in 10 min to 1 hour soaks (all kept below -60C) and had only about 2% less oil in the 10 min wash, as well as having higher potency.
The color was pretty similar, but color is only one way to view potency, which is what I assume everyone is striving for. Not all undesirables are colorful molecules. The longer the soak, the more undesireables, even if it is kept cold.
I make distillate out of crude
So a clean etoh wash is a must for me. I have my sop down to a T. It works for me, but may not for others. And i do it all by myself, no helper. So speed, and efficiency are key.
I can bang out a 25 gallons etoh used, 25lb trim, drained, and filtered in 9 hrs.
What you make out of the crude doesnât matter too much, if you had a (even slightly) cleaner crude, your distillation would be better/easier, and you could achieve a higher end distillate potency.
I feel you when it comes to doing things alone, I can understand why a longer soak would work for you in that regard.
Definitely pick up some bentonite (i would recommend carbon chemistry), removing the water solubles will help improve your starting crude potency as well as help keep stuff from crusting onto the inside of your boiling flask.
G - hope you dont mind me asking this. I plan on picking up some T5 so I can start using it in this process as long as the R&D process gets approved, which I dont see why not as the cost is pretty minimal in the changes I want to implement.
Using T5, is it OK to use immediately after pulling the alcohol and filtering it cold from the extraction? When I look at LS or Carbons recommendations they are saying to do hot scrubs on them basically, which means Id need to let the solution warm up to room temp overnight, warm up more, then filter thru the T5/AC before anything else?
Thanks again
