Distillation (solventless FMCD)

[robotwithdreams]

BUMP. So did i miss it or nobody actually bought the equipment to show all the naysayers.

 

[G.O. Joe]

I have all the equipment and then some, but the experiment will have to wait, because you'd have to hate your buds to remove the tasty terpenes from it. I wonder what terpene-free pot tastes like. Probably not great. It should be pretty easy to tell whether or not the essential oil contains THC or not (without smoking it) with simple well-known chemical spot tests.

Everyone calling bullshit is spot-on, and I'll pile on: this thread smells.
THC is a somewhat big molecule, and big molecules have correspondingly big boiling points.
High-boiling molecules are simply not volatile in steam. 300C is a good general cut-off point, though not the Holy Word.
The highest b.p. figure that I can find for Indian Hemp Essential Oil is 268C. THC most certainly does not boil this low, and has never been distilled at atmospheric pressure in the literature.

I don't know of any method in the literature where anything but column chromatography was used for isolation of THC, without prior conversion to some crystallizable compound. It has been distilled, maybe first by Adams in JACS 63, 2209 (1941), where a mixture of THCs (which may well have been largely the desired isomer), from isomerization of CBD, was distilled at 157-160C at a pressure of 0.05 mm. That's 1/15200th of atmospheric pressure.

Now at really low pressures like this a nomograph and for that matter a manometer is not to be trusted, but let's look at one anyways to give you some idea:
http://www.sigmaaldrich.com/chemistry/solvents/learning-center/nomograph.html
On the right hand side at the bottom of "c", clear the box, type 0.05, and click set.
Clear the "a" box, type 160, and click set.
Now box "b" says - b.p. corrected at 1 atm (760 mm) - 432.2C
That's really freaking hot. I dare you to find something, anything, that boils that high which is steam volatile.

The 12th ed. Merck Index gives a figure of 200C/0.02 mm., and the Combined Chemical Dictionary CD-ROM says 155-157/0.05 mm. It sounds like a big difference but with small amounts, low pressure, and high temp. that's usually how it goes in this imperfect world.

Even at 150-160C in vacuo, it is said that a sizable amount of the THC decomposes.

If there is something in the essential oil which is psychoactive in some way, it isn't THC.

I'm game for argument and citation of the literature.

 

[kaputz]

You can get THC with steam provided the steam is hot enough. Too bad no one in this thread has really done it. I got proof; I have pics of them not doing it. I'll post the pics once I get them out of my space ship glove compartment.

I have done two four ounce batches of super dry super leaf popcorn bud whole without sifting, and have extracted five ml of oil. After emptying the separator I placed my ungloved finger to the spigot and took the last two drops onto my finger and then tasted the oil. I slept great that nigh and was very relaxed the whole next day! Amazing what a benefit this production does! I can't wait to process the rest of the five pounds of biomass I have! This setup of verticals glass components is fabulous! And steam distillation works. I'm going to try turning the hot plate does to a simmer to see of I get more oil out of the next batch! Sooooooo, you can see that others are doing steam distillation too!

 

[kaputz]

This has really peaked my interest. I understand the theory, I an certain it can and will work.... I would love to see a sample, DIY tutorial, just something other than all the theory on "organic chemistry"........... Anyone? Before I run off and piss away hundreds of dollars on a glass chemistry set?

More info on the fractionating column would be good as well, and maybe where to get a lab grade glass variant??? I keep finding rather larger commercial vessels when I search.

I think a fractionating column would be a lovely addition and much better at cooling off the product and thereby separating the oil from the hydrosol.

 

[kaputz]

very cool!

 

[kaputz]

then why did i get so f.....g high off of one drop of steam distilled oil!

 

[kaputz]

ok here's my take.

if the water is not dissolving the cannabloids(which it isn't) then there is no way for the cannabloids to reach the required temperature at atmospheric pressure.

That said a quick google search towards merck says that under vacuum the vaporization temperature is ~200degF, but water will also boil at room temperature under vacuum. So you would need a liquid that is pure and has a boiling point of over 200degF under full vacuum.

so basically this is bunk, it makes no sense scientifically or logically, there is no way to distill out active cannabloids using water. It works well as a medium for water hash but not as a solute or carrier.

if you want high 90's% then you're going to be doing mutiple fractionalization distillations using hexane (2 for ~94% 3-5 for 97+%). now if you're willing to go this far why not try for a THC acetate or other neat analog.

ok, im a newby and I'm distilling, with vertical glass steam, some two year old sugar leaf and popcorn, and I've done two batches at two and a half hour to process, of four ounces each, very dry and unsifted, yet packed well to the neck of the biomass glass bulb. From that process I couped two to three ml's of pure essential oil, There were two drops of oil left in the spigot of the hydrosool/oil separator after i emptied it. I touched my ungloved finger to the spigot and tasted it. my whole mouth was a-buzz for at least twenty minutes and that night was a peaceful sleep! I kept wondering why I didn't care about the little things.... whether its only terpines or what ever,... medicinally beneficial, im thinkin' its a good thing!

 

[G.O. Joe]

Everyone calling bullshit is spot-on, and I'll pile on: this thread smells.

I'm game for argument and citation of the literature.

Errr ya later on this -

https://www.icmag.com/ic/showpost.php?p=4999845

forgot to mention here. The steam part is vague, and there isn't any science saying cannabinoids come over with steam AFAIK. There are several versions of the original patent, GW Pharma keeps adding things. They claim that THC is suitably volatile at 150C, IMHO it's to be seen to be believed.

 

[bobblehead]

You guys are all a trip. I have the equipment, lab access, and a camera. See ya in a couple weeks with pics and lab results assuming the oil is worth testing.

 

[high life 45]

My bro mentioned some sort of steam hash his buddy makes in the bay. He wouldn't give it up, but I bet hes doing something along these lines.

Lets see it bobble!

 

[lifehack]

Love you guys.. sounds like ill make the venture also..

 

[SoulSynergySoil]

I've been interested in distillation of hash since the summer I spent in Yemen a few years back. Experienced Taizz tokers were distilling afghani and local hashish in crude stills made of a couple large pots, a tea glass (the collection tray), a magnet and block ice (condenser). This is of course the land where it all began. Jabir ibn Hayyan (known as Geber in the west) invented the still and founded modern chemistry back in circa 800 CE. When I got back to the states, I started researching distillation and specifically distillation of marijuana. ...most of that study was in the campus library supplemented by a couple good articles on the OG forums. Hooked on the concept, I bought a $600 chemistry set with all the necessary items to build my still. At the time my majors where in physics and chemistry but I came out of school with a finance degree. Some of these companies require educational credentials to buy but search the internet and local supply stores ...it's not hard to get the supplies. I use the steam distillation method, where steam is used to heat the hash. This is great for moderating temperatures, indirectly heating water that heats the hash rather than directly heating the hash to a vaporization temperature. ... just like compashon used a double boiler to moderate his dry distillation aka rosination. Here's the visual ....

View Image
^ the process

View Image
^what your still will look like, if you're using glass lab equipment. If you're buying a pre-made still I recommend getting a verticle one that places the water under the hash cuz it saves space.

The product you'll get from distillation is better than anything you could possibly derive thru sifting alone (with water or otherwise) because ideally your end concentrate is pure resin when sifting ... and the level beyond resin would be "essential oils" i.e. what's essential to getting you baked, or as compashon has branded - rosin*. The other benefit is this 1,200 year old method uses 0*** solvents with comparable results to butane extraction. You can use as is or solidify the essential oils into budder/glass.

And ... If you're a perfectionist who is looking for the absolute best smoke you can make, invest in a suitable vacuum (rotary for ex.). A vacuum will decrease the pressure in your system. When the pressure goes down then volume must go up. After a certain point your hash can only expand in volume by changing state from a solid/liquid to a gas (evaporation). This allows you to evaporate at much lower temperatures providing a more controlled environment. But to really get a primo product you'll want a fractionating column ...

View Image

^ This will separate the cannabinoids from contaminants with close volatilities, giving you the most precise distillation.

I'm just delving into this thread, but this is an idea that I've been exploring for the past month or so. Have you experimented with using steam distillation under vacuum pressure to lower the boiling point of essential oils, terpenes, and cannabanoids?

Much thanks, love and blessings to one and all~!

 

[Momerath]

Cannabinoids are terpenes too, guys...

 

[SoulSynergySoil]

This calculator will help provide an understanding of the temperatures at which cannabanoids boil in relation to varying degrees of vacuum pressure:

http://www.trimen.pl/witek/calculators/wrzenie.html

The temperatures needed are easily reachable via super saturated steam or possibly cooler steam. Does anyone think a honed version of the aforementioned process is what Clear Concentrates utilizes to produce their "solventless oil"? I do.

Much love and blessings from my fractal-temple-conduit-spirit-seed of divine-satchidananda evolution to yours.

 

[Pure777Extracts]

this is pretty funny reading years later