This is marvelous. I’m going to shoot a video on it Very educational
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Per my trials the only time I made olivetol and cresol were with hexane
Never made it with heptane
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Just going off of what my coas from kca showed me that for my particular sop hexane worked the best.
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I did 24 hours room temp
All 4 I tested over the 24 hours popped no idea why
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I ran a 3 hour rxn. Quenched when I saw my spike normalize and begin to drop. All clear. I keep posting the same coa, but it seemed to give the cleanest. Here it is @Kingofthekush420
Clear Fraction COA.pdf (2.9 MB)
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There’s some obvious noise before the d9 peak, but kca also showed me that there were zero trash in it. So, that’s what I’ve found
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Most ppl consider those weird thc isomers bad though since we don’t know the toxicity and we can’t quantify then
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This! This is the stuff that still gets my motor turning, a well thought out piece, with comprehensive sourcing. 
great write up! Wish there was a high five and a hug button instead of just the love button.
Also great work on the guys refining their science and figuring the riddles out. This stuff is the future.
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Was that repeatable? My suspicion was that cresols may come from small amounts of plant lipids reacting with the acid catalyst but this is beyond my understanding. I assume you used a high purity input material but even high purity CBD isolate may have enough of those lipids in trace amounts that could still react and show a tiny concentration of simpler organic compounds if this is the case. I would expect similar results from heptane in either case so that is especially odd to me?
So what’s funny is the isolate that made the cresol was higher potency then the stuff I used to make the 97% stuff
The only time I’ve ever seen olivetol or cresol was in that test and they were both under 10 ppm according to kca
To be 100% fair I don’t make my isolate I only use what customers give me
Alot of the time I know I can recrash and get them a higher purity starting isolate I don’t though because no ones wanted me to
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I’ll dig up some papers this weekend. I think we should be able to gather a working idea of what conditions cause cresols or olivetol to form. My guess is still that the cresols are coming from degradation of other trace terpenoids and not the CBD itself.
This has me thinking. Forget bad catalysts or solvents, what about bad starting material? What sort of junk forms from lower quality CBD isolate?
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It’s not isolate unless it’s 99.9% cbd
So let’s try and make an effort to stop referring to this junk material as “impure isolate”
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Have you ever tested isolate with an MS?
I think you’ll find there’s always something that co crystallizes with it, even if it’s not cannabinoids
Every isolate sample I’ve ever tested by MS has always had some sort of other cannabinoid
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I see you are leaning towards the unknowns being HHCs… This does not mesh with my observations of the 3 to 6 unknowns all having a mass of 315 (314). I also can confirm they do not have the same RT as d7 or d6a or d10 standards.
This is done on lc-uv/ms… A few other labs have seen the same.
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Were you able to isolate these other compounds, perhaps with flash chromatography - so they could be run on IR and NMR? You indicated they are not the same as the standards you have - do you know if they are the same as the byproducts published by Mechoulem?
Would you please supply the additional information on the compounds that you found? We’re trying for this to be a catchall place for any known organic/inorganic byproducts, impurities, intentional co-reaction compounds, and other items that we as a community are seeing.
Sounds like you are seeing other things - which is awesome. Please share process type and the kind of things you are seeing that are not already listed. Or when they are listed - please share that you are seeing the same things.
<3 <3 <3
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Well the lc goes to a dang waste jug so can’t do IR. That would be sweet… Uv to ms to IR to nmr… Ohh the mother detector! Straight to a colony of olfactory cells all wired to some machine learning chip stack… All fn n2 cooled
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Oh but if you’re serious… No I have no IR capabilities. And I really think you’d need some seriously fancy lc method on the front of whatever IR you have because the RTs on these isomers is tight.
Is there a viable uhplc to IR solution? Because all you need is to pick up any sample out there… Gaaruunteee them byproducts are there
This is what I see in all d8 conversations coming through… All have at least 3 byproduct peaks. All byproducts hit the ms at 315 and have the same fragments when given the CID (at 30v) treatment
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Usually I use Flash Chromatography - I’ll load a column - then push solvent through it in measured bumps. Then I test those bumps until I know I’ve isolated the compound of interest. Then I test just that compound of interest.
I’m on testing the entire sample all at once at this point - but have done the separation and then I’m identifying the specifics. The tek isn’t too crazy - its literally a silica column that I’m pushing solvent through like 5 mL at a time - I collect it in screw top test tubes, then I evaporate off the solvent and have a concentrated sample left over.
Been using this method for separation and identification of unknowns for about 20 years now…first time I did this was back in 2004… I remember it was super new age back then. I’m pretty sure its standard practice now, perhaps not?
Those little peaks are far enough apart that you should be able to get that level of separation. I understand not everyone has access to all the fun tools. Most of the time I partner with a local university. I’m new to Michigan so I still need to make that connection here - but you better believe I’m already working on it. 
I’d prefer not to have to transport samples back to Boulder, you know?
Once you have things separated like I have described then you can use a benchtop IR for this. Or whatever other method for structural identification you want to use beyond MS.
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Those peaks are seconds apart on a very good uhplc column run with a very developed solvent gradient method. I will give you thousands of dollhares if you can do that separation of each peak by flash.
You would need an in-line IR system of sorts. I’ve seen some spinning disk bs but I say show me that pudddn