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Sun Tzu
Ok, then Grobag. I been thunking. I've had a look at most of the isomerization processes for cannabis that are available and they do seem aimed squarely at chem students, people with access to labs and industrial chemicals anyway. Where would you find pure sulphuric acid? I'm groping my way towards some alternatives, and simpler processes.

I mucked around years ago with extracting DMT from phalaris and psychotria viridis, which is virtually the same process (except that the initial extraction is done in acidified water) you still have to extract into a solvent (naphtha, or rather VM&P naphtha which is the equivelant of the petroleum ether in most of the isomerization techs) seperate, de-acidify and evaporate. In my opinion most of the cannabis isomerization methods are needlessly hard-core, boiling solvent, using sulphuric acid, etc.

Here's one of the more straightforward methods: hxxp://users.lycaeum.org/~sputnik/Drugs/THC/isomerize.html (replace xx with tt), the only part that really interests us (as we're starting with BHO not alcohol extracted oil) is the isomerization part itself:

"This stage rotates all the existing lesser cannabinoids and cannabinols into THC, and all the existing THC into the most active isomer, delta-9-THC. This step involves the use of sulfuric acid, so I shouldn't have to remind you to wear long rubber gloves, don't inhale its fumes, don't treat it casually because it can eat holes in lots of things, including you.

Dissolve the extract in 10 times its own weight in ether. Slowly, add one drop of sulfuric acid for each gram of extract, stirring with a glass rod. Heat as in the initial extraction, with the jar covered by a watchglass. Cook two hours, stirring occasionally, and allow to cool.

Mix the solution with an equal volume of cold water and one-half its volume of cold ether, and repeat the shaking and separation steps. Take extract and slowly add the calcined ash from the first extraction. Stir it all in, and run the solution through filter paper to strain the ash sediment out. Check for any remaining acid by adding a small pinch of sodium bicarbonate (baking soda). If the solution fizzes, keep adding bicarb very slowly until fizzing stops.

Add fresh water and ether, shake and separate. Cook at 104F until the ether is evaporated. Voila! You now have essence of cannabis, which can contain anywhere from 85 to 99 percent THC."


I've done some investigation, and there is no need at all to use sulphuric acid. Oxalic acid will do fine, as all we have to do is lower the PH to 2.0 or slightly less. It is actually recommended as a catalyst because of how well it mixes with non-polar solvents. It just so happens that a friend of mine gave me a tub of oxalic acid for cleaning up the teak rails and decks on my boat! smile.gif The quantities will have to be higher, but it is derived from rhubarb and is food-safe. Testing the PH of the solution will help. One thing I really liked is the use of the ash from the original plant material (burnt obviously) is used to de-acidify rather than sodium hydrochloride, with a neat bicarb test and remedy if that wasn't quite enough!

So, tentatively, here is my rough outline for a (fairly) simple isomerization of BHO (for discussion only):

1) Dissolve the BHO in 10 times it's own weight of naphtha (petroleum distillates, i.e.: lighter fluid - Swann was the cleanest I found when doing the DMT).

2) Acidify to PH2.0 then heat gently for 2 hours in a pyrex beaker with a glass lid (to allow some of the pressure but little of the naphtha to escape) on a hot-plate OUTSIDE, preferably in a double boiler. Let it cool completely.

3) mix with an equal volume of water and half volume of naphtha (we should only be talking about a fairly small amount of liquid here, much less than the pints I was using for DMT) and mix.

4) Allow to settle then seperate the naphtha layer (this has the goodies in, never chuck the naphtha, always the other part).

5) Add ash from heating the plant material you extracted the BHO from (once it has totally dried off any trace of butane) until only white ash remains. Filter out ash with a coffee filter and add bicarb until it no longer fizzes.

6) add water and half volume of naphtha once more, allow to seperate and drain off naphtha layer.

7) Evaporate naphtha. This doesn't have to be done by boiling, just warming gently, maybe with the hot-bath method you use on the BHO to drive off the butane. It will obviously take a fair bit longer, but is less risky.

You should be left with isomerized Honey oil.

As I said, this is for discussion purposes only for now. Please don't anybody try it yet, until a few bods who know what they're on about have had a look and/or tried it.
Blayz'd
Very interesting. I've read about a similar way to do it before. They had to mix and seperate alot of times though. All of this is well above my head so unfortunately I can't play. I'll stick to the less dangerous things until I have an idea about what I'm doing. I'd love to try that acetate too but I don't trust myself, any experiment where I need a containment box is off limits for me. Would be good to see what someone with the knowledge and expertise could do with it all. I had a look around for discussions or people who were trying it and could find no examples. Sort of left me stuck playing with BHO like a 2 year old. Now I understand why chemistry lessons might have been a good idea smile.gif

Good luck with it.
Sun Tzu
With a few precautions I don't think it needs to be that risky. The dodgiest part of it is refluxing the acidified naptha to do the conversion from CBD to d9-THC and I found a useful bit about that on Erowid. On one of those electric hot-plates (£10 on e-bay) you have your goodies in a tallish pan with a pyrex (or oven proof) mixing bowl on top (so it fits snugly) and keep filling up the bowl with ice and removing the water. This allows a certain amount of pressure to build up, but not too much, and condenses the naphtha vapour, returning it to the liquid. Naphtha evaporates clean, so as long as you're careful about seperation it shouldn't need more than a couple of washes.

I will definitely be doing this the next time I have some oil and will do some pics, see if it can't be made a little less daunting.
Blayz'd
Definately interesting. I suppose it's the same as BHO where it can prove dangerous without the simple knowledge needed to stay safe and burn free. My problem with Isomerizing is I don't have the knowledge yet to be safe. Basically I don't understand the chemical processes which take place. My next batch of raw material I'm using for dry sift, oil and jelly hash. Might throw some of this budder stuff into the jelly hash mix aswell. So by the time I get the batch after that I think I'll know enough to attempt it safely and with the knowledge needed to do it successfully. Hopefully by then you will have explained it in pictures so I feel safe enough knowing what to do lol.gif Thanks Sun Tzu. I was starting to run out of new things to do with my trichomes smile.gif

I look forward to it. wink1.gif
Randalizer
So does anyone here remember the ISO 2 machine? I use to own one. I would pay a lot to have another one. yes.gif It did hash oil extraction and isomorization. Neat machine!
Blayz'd
Hmm, canna oil fountain? Top invention.

Sun, I just found a few text docs I saved about all of this. I think one of them is from newsgroups. Like a discussion or people giving methods. Another document I saved about hydrodistilation of mint which vaporises the oils. Not sure if that one is applicable to trichome oils. Also I found a short text doc with the following name. A Treatise on the Alchemical Method of Isomerization of Tetrahydrocannabinol, and the Extraction and Purification thereof. It's all a bit long so I won't post it. If you want it posted just ask. I think you may have read these things before though. As far as I can remember they weren't hard to find with the right search words in google.

smile.gif
scraglor
QUOTE (Sun Tzu @ Jan 30 2009, 12:04 AM) *
Where would you find pure sulphuric acid?


make friends with someone who works in industry, water treatment, metal processing plants etc, wink1.gif did find instrctions on the net for a simple method though, posted them in grobags hash thread... a fair few acids will do the job and don't have to be pure, but of course wont be as good. personally i don't see the point though? it wontget you any higher, just reduce your yield
Sun Tzu
QUOTE (scraglor @ Jan 30 2009, 10:50 PM) *
make friends with someone who works in industry, water treatment, metal processing plants etc, wink1.gif did find instrctions on the net for a simple method though, posted them in grobags hash thread... a fair few acids will do the job and don't have to be pure, but of course wont be as good. personally i don't see the point though? it wontget you any higher, just reduce your yield


Hmmm, I do have a good friend who works in steel fabrication at a pretty large place. I'll ask him. Didn't even occur to me, so thanks for that. As for yield, I was under the impression that the process of acidification and reflux actually turns the CBN & CBD in the oil (around 50% of the cannabinoids usually, apparently) into the active, or more active THC isomers (delta-9 and delta-3 I think). This wouldn't affect overall yield of material, the amount of oil would remain the same, less a small fraction that inevitably escapes with naptha seperations as you don't want to get too close to the emulsion layer, but the oil you're left with is perhaps 50% more effective. I still have some more reading to do with THC acetate, which is more psychedelic, as the Tim Leary method I read about seems remarkably similar to this one. Could be my memory though.

Blayz'd - Thanks, mate, I would be interested in the hydrodistillation thread. According to ALexander Shulgin you can synthesise THC from lichen and penny-royal oil, which I think involved that process. Future avenue perhaps? The alchemical treatise is the one I cadged the bold text from in the OP, which I got from Erowid.

This is like the good old days for me, pissing about with volatile solvents and improvised lab eqpt., sort of reminds me of the time we worked out that if you feed shrooms on DMT, they metabolise it straight into psylocin. Super shrooms! rofl.gif That was just before the plug was pulled on DMT world, so maybe I should shut up. ph34r.gif
supablu
nice gizmo,randalizer wink.gif how long would the process take and how much ice is needed approx ?
Sun Tzu
Just out of interest:

QUOTE
Dear Dr. Shulgin:

In PIHKAL you have mentioned that the chemicals obtained from lichens can easily be brought to react with certain essential oils from natural sources, to make synthetic tetrahydrocannabinol. Are there more detailed references to this process beyond what is in your book? –Tengu


Dear Tengu:

There certainly are! The tetrahydrocannabinol molecule from Cannabis can be viewed as a combination of two very different halves.

The right half (as the structure is usually drawn) resembles the nucleus of many of the substituted benzene-ring containing components found throughout the lichen world. Isolation of these products can give the raw materials that can be converted to the compound olivetol, a simple amyl-substituted resorcinol compound.

The left half is a terpene which contains ten carbon atoms, and which is substantially identical to the essential oil, pulegone. This component makes up some 80 to 90% of the Oil of Pennyroyal.

The fusion of these two materials has been shown (Claussen et al., Tetrahedron Vol. 24 p. 2879 (1968)), to produce several products, one of which is delta-3-THC. This is a close structural isomer of delta-9-THC, the principal active component of marijuana, and is known to be active in man.

-- Dr. Shulgin
Randalizer
QUOTE (supablu @ Jan 30 2009, 03:59 PM) *
nice gizmo,randalizer wink.gif how long would the process take and how much ice is needed approx ?


12 hours with isopropyl alcohol and 1/2 hour with chloroform. No ice needed, you just put water in the reservoir seen below the fins. The trick with the isopropyl is that the water would evaporate in less than 12 hours so paying attention was vital.
Sun Tzu
QUOTE (Randalizer @ Jan 31 2009, 12:14 AM) *
12 hours with isopropyl alcohol and 1/2 hour with chloroform. No ice needed, you just put water in the reservoir seen below the fins. The trick with the isopropyl is that the water would evaporate in less than 12 hours so paying attention was vital.


I completely missed that post, Randalizer! When did that machine come out, or how long ago did you own one? Had a quick look and couldn't find anything about it. Do you have a manufacturer's name at all? Oh, and one thing I picked up on last night's trawl is that chloroform can leave some bad things in the oil. I'm struggling to find the ref now, but it was quite adamant that it's not a good solvent. Naphtha would work instead though, I think.
Randalizer
hay Sun,

The ISO-2 was put out by a company called Thai Power INC. It was released during the 70s. I've not seen one in a long time. Chloroform was recommended in Michael Starks book, Marijuana Potency.
QUOTE
It extracts about 98% of the cannabinoids with 1/2 hour of shaking.


Since that time I misplaced my machine (please don ask) and have learned that chloroform is a carcinogenic. I think extracting with the BHO process is probably fine for me. yes.gif

His book has a chapter on isomerization. I'll read up on it when I get a chance and see if there is anything of value to offer this discussion.
Sun Tzu
QUOTE (Randalizer @ Jan 31 2009, 12:34 AM) *
Since that time I misplaced my machine (please don ask) and have learned that chloroform is a carcinogenic. I think extracting with the BHO process is probably fine for me. yes.gif


So how did you come to.... ? rofl.gif

I reckon I agree about the butane. 98% (according to some) of the goodies in about 5-10 mins and no nasty carcinogens. That must have been what rang the alarm bells re chloroform last night.

Right, well, you might want to get in touch with this guy. Says he has one!
hxxp://www.yahooka.com/forum/inquiring-minds/142570-iso2-isomerizer.html (xx - tt)

QUOTE
I have an ISO2 isomerizer, made by Thai Power Incorporated. It was made in 1974, and uses alcohol to extract THC and essential oils from marijuana. There were no instructions with it when I found it. I researched it and found that it creates a zero oxygen environment, which causes cannibinoids to take on a molecule of carbon, becoming THC. It also uses "isomerization', essentially adding a small amount of Sulphuric acid which converts the THC to THC-delta-9. My question is does anyone have experience with this machine? I have researched it for years, and I have the formula down in every way but the amount of acid and the time needed for isomerization. I have made hundreds of grams of hash oil, and every now and then the oil was so potent most people (including myself) essentially got so high it was unbelievable. If anyone has some info, it would be greatly appreciated!!! I hope there are some old school heads out there who can help me. Thanks in advance for any help

Randalizer
funny. When I did a google to find a picture of the ISO-2 I actually read part of that post. lol.gif
Sun Tzu
QUOTE (Randalizer @ Jan 31 2009, 12:57 AM) *
funny. When I did a google to find a picture of the ISO-2 I actually read part of that post. lol.gif


Looks like a hell of a piece of kit, and there were some posts further down in that thread that had some great info on using it. The Elric bloke also said that 2 a year come up on ebay (.com). Might be worth posting an item wanted thing he reckons. I wonder if plans/patent for it might still be available. I might have a look on the U.S. patent office website....
Sun Tzu
yahoo.gif

It seem there is a modern equivelant available for $398. Have a gander:

hxxp://www.beer-wine.com/product_info.asp?productID=1089&sectionID=5 (xx-tt)

Click to view attachment
Randalizer
it's pretty easy. The cooker is a stainless steel vessel and that sits on top of and inside of the tin body (bottom part). I believe the vessel is a resturaunt soup heater vessel. Light bulb for heat underneath with a thermostat control. The top part is the fancy end. It's a hollow steel(?) tube with those aluminum fins, The reservoir is just an upside down steel bowl. There is a carbon pellet chamber in the top part of the tube.

There is also a cage that sits under the fins and above the vessel. This holds your ground up pot. It works as a percolator. Pour in solvent over the canna, where it collects in the bottom of the vessel. Put the top on, fill the reservoir with water, turn it on. The solvent evaporates, vapors go into the cooling tower and then drip back dow through the herb. The essential oils are left behind as the solvent evaporates again.
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