Holy Crap, I think Im on to something

Discussion in 'Harvesting and Processing Marijuana' started by bioguy, Dec 6, 2013.

  1. #1 bioguy, Dec 6, 2013
    Last edited by a moderator: Dec 11, 2013
    EDIT 12/10/1213. This turned out to be a failure. If you can figure it out, more power to you.
     
    I was cleaning some low quality hash with solvents the other day and I had "what alcoholics call a moment of clarity". I had 10 grams of hash dissolved in 100 ml of Isopropanol that I needed to evaporate. I thought that I would try something new. I figured if I poured the iso into water, then the solubility would be reduced and the solution would purge its solutes.
     
    I tried it with +/- 5 ml of the hash/iso solution and 80 ml of ice water. I poured the iso on top very slowly and it floated. It immediately started to separate into a film as the iso and water began to mix. A amber/red/brown layer remained onto while a cloudy precipitate formed. I could not resist the urge to shake it but nothing changed.
     
    This was when it hit me. How do I know that the precipitate is not the THC. I thought back to chem lab experiments where a change in solubility causes the formation of a precipitate (ph shift causing precipitate is a standard chem 101 experiment). My understanding has always been that thc was an essential oil. If this is true (absolutely true) then the precipitate is garbage. But I suspect THC maybe actually be a compound within the essential oil. A good analogy would be the way azadirachtin is a part of neem oil. I have seen this cloud many times when I accidentally spilled butane or alcohol in water but I never thought about it till now. When I saw the precipitate I remembered how confused I was when I learned the trichomes sink (essential oils float).
     
    My initial thought was the water would get rid of any crap not form a collectible precipitate. But the crap looks good. I smoked the precipitate and it tasted like hash, smelled like hash and I'm pretty stoned....but I've been smoking all day. Its white when its in the cloud but it looks like hash when it dries. 
     
    It does not matter in the end because both the film and the precipitate are collectible. This will allow for the separation of the hash without the long evaporation time. It will also probably help wash the final traces of alcohol from the hash. Regardless of whether or not the THC is precipitating out or floating (or both) it can be harvested. But I am willing to bet one of the two (sinker or floater) is much stronger. This will reduce solvent removal time to nothing but the water alcohol solution will still probably have some THC since the solubility of THC in alcohol water mix "must be" higher than just water. (must be is an assumption). 
     
    You can see the precipitate in the left corner (I settled it on an angle) and the oil/wax/hash stuff smeared around the top.  IMG_2697.JPG
     
    Sample of the hash/iso solution with the undissolved hash settled.  IMG_2700.JPG
     
    This is plain water for reference so you can see the cloudy effect  IMG_2699.JPG
     
    Some solution floats and the cloud begins. IMG_2701.JPG
    The iso layer and the cloud growing. IMG_2703.JPG
     
    This one shows it after shaking. If you look carefully, the oil is beginning to float and attach to the glass at the top. IMG_2706.JPG
     
    This is what it usually looks like when I evaporate the iso like normal. Its black unless you put the light on it...then its amber gold. IMG_2707.JPG
     
    If I knew the density of THC it might help determine if the precipitate could be THC. I know its molar mass is 314 vs 18 for water but without a volume I can't do a density conversion. My gut tells me something that heavy should be sinking but chemistry is not really my area. 

     
  2. I can't speak to the facts of this experiment but it was a good read. That being said, you said you smoked the precipitate and got high from it? A risky move man but it apparently worked out for you  :bongin:  :eek:
     
  3. #3 bioguy, Dec 6, 2013
    Last edited by a moderator: Dec 6, 2013
    Thanks
     
    The mix was just iso and hash. Therefore the removed solid is something I have smoke before (it could have been a wax but if so it would be a wax we have all smoked). I don't think it was risky. 
     
  4. As long as you could tell it wasnt loaded with booze still i think youre fine!

    I'm currently too stoned to really comprehend all of this, but good work. :p
     
  5.  
    Yeah what risk? I don't see one either. So its like a shake-N-bake method? for reclaim iso? lbs? right?
     
  6. I've heard of people using water to blast into, except they used warm water to accelerate the evaporation of the butane.  It seems like that would work much better than cold water.
     
  7. I should have slept on this before I posted. After a little more thought about it and an attempt to replicate the results I think I have figured this out
     
    In order to take the photos I redid the experiment. The first photo is the results of the original try, the next 5 are the duplicate attempt. The duplicate was done with a little of the iso/hash mix but I added the oil that floated in the first try. When I was finished almost no oil floated up (even though the solution had more oil in it). This is when I realized the 2 solids (floater and sinker) maybe the same thing. I suspect the floaters are just the larger pieces. When I did it the second time I was much more careful to float the iso on the water. Then I left it sit for 30 mins without shaking or stiring. The iso continued to float while the cloud formed slowly. After it was eventually shaken virtually no floater was formed. 
     
    I am almost certain that by floating the iso and allowing the precipitate to form slowly the hash formed very small particles of precipitate. Whereas the first try, the iso went in faster and large pieces were formed immediately. Then they stuck to the glass giving the illusion they were floaters.
     
    I am going to do a full sized batch with iso and shake. My real goal is to create an easier way to remove the solvent and chlorophyll from THC containing solutions. The only thing that prevents alcohol from producing BHO quality is its propensity for chlorophyll. I am hoping this still work with high levels of cholophyll....the chlorophyll should stay in the water.  
     
    The bottle in the last photo above was settled overnight and yielded a precipitate like before but virtually nothing on top. 
     
  8. so you want the purest of the pure eyyy? lol sounds stressful. gl, be safe.
     
  9. Yeah I saw that on you tube once and it makes sense. In this case, evaporation is not the goal. I kept the water cold so the particles could form without sticking to each other.  I'm just starting so I should try hot too at some point. If you see my update about "floaters and sinkers" you will see that this may be an option. The hot water may force the particles to stick. Then it could be removed as a blob instead of a million tiny particles. 
     
  10. Yeah that's how I saw it I'm pretty sure, the extract ends up as a film which he scoops up.  It would probably be a good idea to get a vacuum purge if you blast into water, or you'll have some still in the final product.
     
  11. Yep. 
     
    I think it could also be used to wash the final traces of butane from BHO. 
     
    My concern is that THC must be partially soluble in the alcohol water mix. But If this allows for the washing of lbs of crappy product with cheap solvent then that loss might be considered acceptable. 
     
  12. What confuses me is that BHO floats, trich's sink and this stuff has done both (looks like it sinks when done right). Terpenes should always float - should. Although once a terpene is bonded to another substance is density changes. THC is terpene bonded to a phenol and in this case a carboxyl group (I did not decarb this stuff). I found the density of THC last night and it 1 g/ml +/- .1 (same as water but it has a +/- .1 g/ml) this may explain why some float and some sink.
     
    As for a vacuum...I wish, maybe someday! Currently I have my eye on a boiling flask condenser set up. For now I use an ethanol wash to dilute the original solvent. I have heard you can just use water for this (I saw three rinses recommended somewhere). With the current tech, the particles are tiny. This leads me to believe the water would be very effective. If this was done with ethanol instead of iso, the trace ethanol would be well within the bodies ability to cope.   
     
  13.  
    Ahhhhh. :hide:  I see....
     
    yeah may be some trace amounts...but like you say, an acceptable loss (I am sure of).
     
  14. Yes and no. I like to play. I was on track to be a real scientist when the economy collapsed, my job prospects went to hell and I started growing again. Now the lid is off in Colorado and I'd like to make some kind of contribution. Colorado has tons (literally) of low grade hash but an oil craze has swept the scene. I can't imagine how much butane is being used daily. Its dangerous, an environmental atrocity, the butane does not come all the way out....its less than an ideal method. BUT BHO ROCKS!
     
    I just think their is another way. Can I find it? IDK. Maybe I can't. Maybe someone else will be inspired by my method.  
     
  15. I've heard that some people use hexane, I'm not sure if it would be safer but I think it might be a little more volatile and therefore more likely to evaporate.
     
  16. #16 bioguy, Dec 6, 2013
    Last edited by a moderator: Dec 6, 2013
    I think Hexane and ether are the two best but both are comparatively expensive. Ether has the benefit that it is not miscible (floats) with water so the chlorophyll can migrate out of the mix (thats standard old school methodology) and the THC stays in the ether. Thats part of where the idea came from and why I was so confused about the precipitate (it does not happen in the ether water separation) 
     
    I also think the any petroleum solvent is gonna stay behind in trace quantities unless vacuum's are used. Even then I have read the butane will never come out completely. I'm using iso for the experiments but I think this should be an ethanol tech. That way if the water does not get rid of completely its not a big deal.
     
  17. you could evaporate the alcohol in your concentrate in a 20 dollar rice cooker then finish the process with a couple teaspoons of water to continue the boil til the alcohol is gone this is pretty much how you make Rick Simpson Oil.
     
  18. #18 bioguy, Dec 11, 2013
    Last edited by a moderator: Dec 11, 2013
    I tried to scale this up and it was an utter failure. FAILURE.
     
    I did it with an ounce of trim. When I poured it into a gallon of ice water everything went as planned. Some beautiful oil condensed on a knife I was using to stir the water. I poured it into another 3 gallons of water and then through a 25 micron bag and got NOTHING. I let it settle overnight and got NOTHING. IDK why it worked with a small amount nd not a lot but thats the end of my experimenting for now. From now on I will dissolve the bubble hash in butane and winterize with everclear. 
     
     
     
    I am updating the OP to include this. I will leave this up for posterity.
     

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