Lol that’s true. I’ve been pretty lucky my whole life. It could also be that I listen when people tell me things and I’ve got a nack for applied theory lol.
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Distilled water. I suspended the citric acid into the distilled water then added to isolate that was warm enough to be a liquid.
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That would be my assumption. I didn’t expect it to work because I read somewhere on here that the solvent used for a reaction like this needed to have a pka of 16 or better where as water being my solvent is in the 15.3 range I believe. I believe PKA was the right term.
I guess what puzzles me Is why it’s so hard to control the double bond on the top ring. Obviously the citric acid will pull that hydrogen at the bottom and close the ring but what’s up with the double bond at the top… my theory was that I was putting to much energy in to the reaction causing that double bond to become unstable and therefore bounce around.Thats what led me to water with a lower energy input. Once again I have no chemistry education so I could be way of the mark.
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depending on weather the the compound that is created is destructive.
an idea to start with anyway
I think you may find a precipitation test in a two stage attack on the CBD
to a quinone then a hydrazone.
the hydrazone would possibly be soluble in water.
the oxime may also show to be insoluble in some solvents that THC will disolve in.
I doubt a bisulfite complex would work with the experience I have had with
the complex.
It normaly wants a rather pure compound to form and precipitate.
Polarography might help as well as one could run the sample pre oxidation to
the quinone then post oxidation and run a formular on the two results to calculate
the difference.
Polarography is used to measure some ketones in perfume though
I can see it also acting on the double bond in both THC and CBD but the difference
between an oxidised sample giving the quinone and the raw sample might
be enough to work out the CBD content.
[21910189 - Reviews in Analytical Chemistry] Determination of Phenones in a Perfume Composition.pdf (595.3 KB)
ill keep thinking on this one as the name reaction and wet chem is a passion of mine.
I am still far from a master though 
till then I think that we can probably develop at least some kind of preliminary testing
with optical and beams (which goes to quinone :)) that uses cheap as parts
but ye I thought that was the case and only chromatography was the go at the moment.
I also think raman could be tweaked to do this too and I think a diy raman would not cost much
but the code behind the fourier and logic behind the quantification would be quite
complex.
thankyou for answering it means a lot to me.
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Very cool results, I would have never thought of using water.
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to keep everything accessible in one place
AgTonik’s Cannabinoid Isomerization References
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You are the man and this is an awesome subject. I wish I could Google fast enough to keep up with the chemistry but some sort of even vaguely quantitative reactive precipitation assay would be a game changer.
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another idea for testing would be the use of nafion polymer to isomerise to Delta 9 in solvent.
the nafion would be able to be reused and easily extractable leaving no acid to be
separated from the cannabinoid solvent mix.
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thankyou for sharing this
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I am watching people do test runs in the 100 200 300 1000 gram range.
STOP IT
its stupid and waist full
why ?
get a small kit and do the reaction in the 5 gram range.
just because some dude wrote a SOP on something doesn’t mean it works even
patents and journals come up bunk at times.
every situation will be different your distillate solvent catalyst acid ect all different.
you have to tune this shit.
I am hearing of errors in SOPs that were sold ???
be wise test stuff on the small scale and then when you have results then step it up.
you don’t need a kilo to send it off to the lab.
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To be 100% honest I was disappointed with the results because I’ve be working for Non detect on the Delta 9 with no side reactions.
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understandable still but to find new information like what happens with citric in water
for isomerization is not a bad thing.
even our failures are successes if we gain information from it.
from what I can tell the route is CBD is turned into Delta 9 then the double bond moves
over to Delta 8.
maybe as suggested above its just a time thing.
use the optical rotation to follow the reaction next time you should see it move up to over 250 which is where you want it if things are going well.
it may be that at some point the rotation does not move anymore and then you know that the
path will not get to 100% delta 8 (if that’s possible)
but at least if your doing small reactions with optical rotation measurements you can do
lots of tests before having to send anything off to be analyzed
I still call it a success and thank you for the open sharing of information.
also for those going to CBN its great they don’t care if its delta 8 or 9 as they will
be dehydrogenating it anyway.
they want a food safe reaction and citric acid is used in food so there is a big win there
citric acid and water is pretty safe for human consumption.
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The citric acid was in tht case dissolved in the water. It is highly soluble in water. It buffers the solution to a low pH. The more concentrated it is, the more you will get close to pH 2.79, which is the pKa of citric acid.
Here you are limited to water boiling temp, unless you woulg go for pressurized reactor. You may just increase rate by playing with temperature and acid concentratrion, but not the yield. It may be only a question of time . If you want to check this well, you have to follow the reaction over time, and see what profile you get. From this you will be able to predict the trend over extended time, and thus the max expected yield.
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what about DMSO for the solvent ?
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Just curious, does this lab have ISO 17025 accreditation?
It’s the smallest equipment I have lol. Everything else is manufacturing/production sizes.
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I do need a way to follow that reaction over time. I feel that it could be dialed in very well. Only piece of equipment I have for analytics is a FTIR which I don’t believe will tell me concentrations. Should have never sold my Agilent 1200.
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How would you remove DMSO from the product?
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@squig is smarter than me. I had asked where to read about how to calculate how much acid is needed to catalyze a reaction. Without a Phd level understanding, the answer is optical rotation and testing small amounts with different variables.
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