I’m extremely curious about the steam sparge concept. You could use a diffuser glass setup that places the inflowing steam just above a stir bar extending down directly from the top of the flask. With ejection ports on it faced in every direction. A more efficient displacement by steam in this fashion may also cause less water to be required for the given procedure. My curiousity is also about testing the products after and how you then removed the water. Obviously a good nonpolar Alkane would be handy. Such as heptane.
My other question, is with this technique did you use Vacuum at all. I assume no based on the temps and based on what I expect would happen when using Vacuum while drawing in steam… but a balance may help the process happen at lower temps, thus possibly saving the boiling flasks from fracture.
Here is another way to observe steam distillation in action. I had gobs of videos on YouTube showing all this stuff but it violated their standards regarding drug videos so I took down 28 videos showing how to isolate D9 THC into absolute purity on a small scale. They all got deleted but I do not mind posting pictures. I don’t think
I can currently or my iPad is not letting it work. Just words work too so here goes;
You need a simple distillation rig. There is no steam injector at all this way. Take rubbing alcohol at 70/30 isopropyl alcohol/water and disolve your extract completely in it. Then add about 25-50% by volume water to the mix.
Begin distillation. Isopropyl alcohol forms an azeotrope with water so it boils off at the same time as the water does. Monitor the head temp in your distillation. You will begin recovering rubbbing alcohol/water well below 98C and the temperature will slowly climb as the isopropyl alcohol is depleted and the ratio of water increases.
Extract will begin to drop out of solution as the temp climbs toward 98C. Once the temp hits 98C all the isopropyl alcohol will be depleted from the boil leaving an emulsion of water and extract boiling away. Almost immediately upon the head thermometer reaching 98C you will notice an odor of pine in the condensate and it will begin to run water white with the pinene (if present). You can continue the boil and strip a lot of the volitiles this way too. I use this only for stripping lower boiling volitiles like terps. The cannabinoid stays in the boiling flask. The isopropyl serves to get the water into intimate contact with the extract which is not miscible in water alone. This technique is pretty simple and is a first step in my own current SOP to obtain D9 THC isolate. If you do not care to save the terps you can halt the boil and put the vessel in the freezer. Then pour off the chalk white water. If it is not chalk white then there is extract in it and I keep chilling it until it is a clean white color. I pour the white off and then run it again the same way until the terps are gone and the water stays clear. Then chill and pour off water. Recover extract in solvent and purge.
The second advantage to running it this way is that the water is also put into intimate contact with the chlorophylls and then they are subject to hydrolysis. So if you just strip the volitiles (I do this every run now) this way you are left with cannabinoid and waxes and chlorophylls. The waxes and chlorophyls can then be removed by running them through an aluminum oxide (220 grit abrasive grade, either brown or white from Amazon) column a few inches thick using 70/30 rubbing alcohol. Green chlorophylls and all the white wax gunk (now swollen through the denaturing effect of the alcohol and hydrolysis during the boil) gets stuck on top of the alumina when you pull it through after a boil to strip the lower volitiles, yet all the cannabinoids pull through easily.
That’s super interesting. I came across this concept a lot when doing co2 extracts. We ended up with a lot of water in our product do to not decarbing the material correctly before running it. I always heated the mixture and swirled it around to get the water in one place… then pop the bubbles and pour off.
Have you noticed issues with potency, due to the water interaction? Photon has written a lot about the interaction of water and isomer changes. And the use of MgO to counter this.
The water does not appear to impact the cannabinoid in any significant manner in these procedures that I can detect. Steam co-distillation is normally considered a good option for thermally sensitive products. I have fiddled with trying it under a vacuum but it really just added complexity to a simple process. Potency is fairly well protected so long as the THC is not exposed to atmosphere. The waxes in the extract generally slow the degredation significantly and during the boil the THC is mostly exposed to steam (water gas only) which also keeps it mostly out of contact with the air.
Once it is dewaxed and left in open air it will begin to degrade immediately. Just like a paint job on a car, without the wax to shield it then it starts to break down. This breakdown of the THC turns almost clear pale yellow isolate into ruby red couch lock wonder in sort of a pure mode in about three days when left out. When I run it without dewaxing and adjust settings to evaporate/sublimate the waxes along with the THC then I can leave the product out for weeks before the red becomes noticeable. I prefer to store it under high vacuum though and leave waxes off. I use all that I process and sell nothing. There simply is nothing like pure THC to cure what ails me lolz.
Here is my instagram page. You will see a highly purified white/very pale yellow D9 THC “biscuit” being held at ¾ of one micron pressure under a bell jar and still liquid and some other shots at various degrees of purity. Note the red sample on the mirror leaning up next to the baking soda boxes. That started out almost clear and was left out for about a week as I dabbed. it degrades fast in open air. https://www.instagram.com/redturtle984/
he did have good videos that showed every step till youtube took them down, I was watched all his videos and while not 3rd party obviously its very convincing. obviously without real analytical equipment whose to say whats actually going on or why but i believe he’s witnessing some sort of phenomena
Never used a rotovape to deodorize but the rotovaps with a feed line fed prewarmed would work pretty well I imagine. The later patents use deodorization under vacuum
The color change is not the thc but the remnants of anthrocynin and maybe not carotene if you used an alkaline anti-solvent for your crystalline. A lot of peoples 99% is like a little bit of anthrocyanin if its yellow because a little goes a long way in color. I mean at least for the majority of color change if its a still yellow concentrate. What colors CBN? I tested aqueous phase in HDPE container for like a year it only turned red with exposure lol
nope. Anthocyanins are water soluble. there is no way they would still be in extracts that have seen aqueous washes.
If the color change was residual anthocyanin, then the makers of Drobinol would not have a problem with their shit turning red, and would not have formulated in sesame oil to prevent it.
“They have a positive charge on the molecule which enables it to absorb light and thus have color. An anthocyanin has a carbohydrate (sugar, usually glucose) esterified at the 3 position. An anthocyanidin, termed the aglycone, does not have a sugar at the 3 position. Naturally occurring pigments from grapes always have a sugar bonded at the 3 position, though other compounds such as hydroxycinnamates and acetate may be involved. The presence of this sugar helps the anthocyanin maintain solubility in water. If the sugar is hydrolyzed or lost, the solubility decreases and the molecule will be destabilized and lost” Not a chemist but maybe its more complicated especially the smallest of remainder. I have some friends in vegas who get tested 102%(obviously off but closest than most to 99.9%), still not completely water clear. Myclo is remediated with magsil/c18/silica after water washes for the ppm-to-PPB remainder because tails is harder and harder to remove as it becomes small. Good point on the Synthetic version of THC! Not familiar with how they are made but your likely right that its not antho in synthetic form at least and something else. What’s weird is its only 97% so I wonder what the 3% is from synthetic form? Not saying THC can’t degrade and change color but if its not 100% it still likely has something that even in ppm could be a color. Like if you try distilling 100% alcohol without adding benzene your still going to have water. thcs is a little polar right? so even deodorization at 100c you could guess maybe isn’t piercing the thc at the ppm of oxidizable things as much as 150c+ is at any given rate of time/washes.
RE: Drobinol, that’s 97% of starting material left at 90 days, IF they add something to stop oxidation to CBN. Doesn’t really matter how they make it so long as it’s not extracted from cannabis. It’s a synthetic, so there are zero plant pigments in there.
Positing Anthocyanins requires loosing the sugar, AND the color… until color magically reappears with addition of O2. I don’t buy it. I’m also not a chemist…
I certainly agree that both anthocyanins and carotene can be co-extracted using alcohol or CO2, possibly even with hydrocarbons if they are water-logged. I don’t however accept that either are in anyway involved in the color change that takes place upon exposure of high 90’s THC distillate to oxygen.
stinky first pass distillate is not an uncommon occurrence.
yeah, that might imply you did it wrong, but the bad smell can be removed, and removing it goes a long way to salvaging the distillate. usually. unless you really messed up and ended up with 3% delta 9 THC
I’m in the market for a terpene distillation kit and came on here to do some research…
You’re the only one on the forum I could find that seems to be in discussion about this topic and your process sounds to be identical to what some of these kits claim to do. Would you happen to have any experience with any of the kits? Be able to recommend one?
All my stuff was pieced together and I have not really even looked much at kits much. I have often been asked this sort of question but I don’t know about kits or who makes the best stuff like that. My rig is obviously minimal and micro runs. I am betting that an entrepreneur who comes up with a kit for micro runs would see good business lolz because it handles quantities the average Joe might be dealing with who also needs purities that the dispensary cannot provide.
presumably you want to keep the terps.
Beaker is actively trying to loose them.
Start a new thread, and post links to the kits you’ve looked at.
my current understanding is that variations on steam distillation are the most promising route. I doubt True Terps will reveal their methodology, but my guess is steam distillation under reduced pressure with N2 sparging.
I believe true terpines are not cannabis derived, and I believe they are imported from India in mass quantity, broken down, repackaged and sold. They also sell blends of these imported terps from analying terpines profiles of strains and doing the blend for you. Nothing that any of us could learn and/or do.