If you are running the reaction at high temperature, using an additional solvent won’t likely make anything better.
It seems that as many other catalysts, citric acid is not specific enough, and/or cannot push the reaction to completion…
I agree 100%.I’ve run it a bunch of different ways with different solvents or no solvent and can’t seem to get it below 18% delta 9. I’ve switched over to a more widely used acid and have had better results in a far shorter period.
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Ha ! Better results ?
Of what sort ?
80% delta 8 with 10% delta 9 pretty consistently. I had a stupid math error on my part calculating percentages so I think this next run will be better due to fixing my error of excess acid.
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Which combination gave the 80/10% D8/D9? You think it was excess acid causing issues?
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Tosic. Yes I think that’s the case after talking to a few guys that have it down.
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Hey guys
I hope it’s ok if I tune in here, I’m a complete beginner but maybe my attempts can also help to shed some light on the darkness of the citric acid isomization (and if it only shows how not to do it ^^)
I have read a lot in the forum in the last few weeks and since citric acid would also be very dear to me, I also bought citric acid for the start / test / learning setup (among others).
(It may not be the best idea to start experimenting directly as a beginner instead of using a little more elaborated procedures, but whatever it is to work with citric acid just sounds too interesting to start with hcl or something.
And any method would be difficult for me anyway because I have to guess what Google Translate is trying to “tell” me about almost all threads xD
(This text is also translated with Google, sorry I just can’t speak foreign languages, no matter how hard I try to learn …).
But to get to the topic. I have now made two runs, the first one I had destroyed during washing, but before the “crash” after 12 hours of refluxing with 10% citric acid in isopropanol, at least apparently less purple could be seen in the sample with the 5% Koh test. Then I stopped to look at the result and then totally messed up while washing ^^
Then I rummaged through the forum again for 2 nights to really understand the washing despite the language barrier, it also worked and in addition I got the solution (soup?) By chance. And I also increased the citric acid concentration (20%).
I did the Koh test again after 12 hours (I thought it wasn’t worth it with citric acid beforehand) and / but a little surprised no purple saw anymore, the dried stain did not change its color at all, mixing did not change anything (as I said, I know not exactly how the KOH test is, means no purple / no reaction = no CBD?).
Then stopped and washed (this time it worked ^^) with “Benzinum medicinale” (this is a mix of alkanes, unfortunately I have not found a reasonable translation as the product is called in America, it is very clean and is obviously still used medically sometimes, -I have actually been using this for ages to oil cut residues and was very pleased that it happens to contain mainly pentane, something that can be read very often here in the forum …), then salt water washing and a few times with distilled water.
In the end, a slightly yellowish and in the consistency rather hard / viscous oil came out (a little bit harder than e.g. classic extracted wax, I would say was [cold] difficult to scrape out of the shell).
At first I thought it was see-through and was happy about Delta 8, then I noticed the slight yellow tinge.
I only took a little CBD for the first test attempts (10g each), the result will not be enough to have it tested quickly in a laboratory for fun, I thought it would take me weeks to get some kind of conversion. But I don’t think it’s Delta 8 or Delta 9, one would be like glass, the other brownish (as far as I know), but what kind of by-product have I made?
I would like to continue with this second attempt with less reflux time (since 0 purple was found after 12 hours in the test, I suspect that it was far too long …), but it would be practical to know what this slightly yellowish Oil is the one I got from (too long) reflux.
Funnily enough, the concentrate actually looks like lemon, but what is that by-product that I’ve made out of now?
(and does anyone know how exact the KOH test is?)
It would be nice to know whether the yellowish oil is a sign of something very, very bad, or if it stays within limits. Because the thought of using citric acid has of course (probably with most people interested) something to do with the hope of a little more security. And as a non-chemist you are of course much less afraid of this than of other (evil-sounding) acids ^^
Sorry if I express myself a little hard to read, and the grammar is difficult to read, as I said, I just can’t speak foreign languages. Try this since childhood, every language teacher is desperate for me …
Edit: oh it is CBN??
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I’ve sent you a DM.
Good work @jeeric thanks for sharing your experiments with us. All info is helpful. @Ennui can you help shed any light on this conversion approach for me? I’m still trying the original tek with higher concentrations to no avail. I’d like some clarification on the beam test also.
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If we’re talking about the standard citric acid in solvent reflux then it’s straightforward and there shouldn’t be much to explain. I’ve not run any trials with this citric acid/water catalyst andI don’t know anyone that has had positive results with it.
The beam test is a very limited colorimetric reagent test. It reacts with CBD by forming a quinone. It’s not a good replacement for real in house analytics. It only shows the presence of CBD and even then it’s not that accurate. For people doing at home isomerizations for shits and giggles this might be a fine way to monitor your reaction to an extent. If you’re trying to make compliant d8 on a large scale this test will not be enough. Hope that helps
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I’ve been trying with water. Maybe I’ll switch solvents and lower the concentration next time I try. Thanks @Ennui
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Yeah I can’t really speak to the water one. @JedClampet is the pioneer of this aqueous tek. Perhaps he can shed some light on the subject.
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Correct me if I’m wrong. Didn’t find it at first (I didn’t realize that I had misspelled yellow ^^), but in many places you can read that yellowish oil would be a sign of CBN.
CBN in turn arises from THC.
If I don’t think completely wrong now, it means that THC must have been present at some point in the 12 hours, which then (because it is taking too long) has further changed to CBN. So it looks very much like I actually cooked for far too long and that I boiled broke again, so to speak? (That would be my conclusion ^^)
I think I’ll do the same run again today and then test every hour with the 5% KOH test. (Does anyone know what the picture / purple looks like when you are at the point where there is little CBD available? At the time it sounds logical that you also encounter THC (I was obviously over it and unintentionally got the beautiful THC CBN overcooked ^^) I have never found a (still available) picture that shows pictures of this test … Without knowing how the test reacts, I can only differentiate between the reaction of pure CBD and no CBD Picture in the head what it looks like with medium CBD value, 3/4 CBD or 1/4 CBD content would be really nice to be able to really assess and use this test 
(you need comparison values to at least be able to imagine what saturation just exists, in the KOH test you would have to see pictures of other people in order to be able to see roughly one direction.
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I would think that would make acetic acid and ethyl chloride
https://sci-hub.tw/https://onlinelibrary.wiley.com/doi/abs/10.1002/recl.19570761004
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Please do not assume that a hue being present in your product indicates the presence or absence of any particular cannabinoid. You should have that tested.
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Does the product smell ?
After this time of reaction, you likely got a mixture of at most 50-70% d8, 2-20% d9, also a major 2-30% of another isomer (d10 is the main suspect). You can had a series of up to 20 other things to this, most far below 2% . CBN should not be much more than 2-3%.
The faint colour comes from some of the minor compound(s) formed during the synthesis. It can also develop as the product ages, but then it would rather lean toward the red/pink.
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I gave everything that I had. I’ve been trying to get this tosic sop compliant so I haven’t had anytime to recreate the citric/water reaction but maybe Friday I can re-run it from my notes again. I think the results I got were an accident because of the water boiling away over time due to the condenser being to hot.
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I wonder how much unknowns would be left if you weren’t concerned about converting past D9. It’s after all what the people want. Could you make a cleaner safer product if you weren’t reduced to selling widgets by federal drug laws? Maybe just grow good weed instead of hemp. Or maybe grow hemp and make rope.
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can ya’ll post some test results of what ya’ll achieved with the citric acid tek? I’m very interested in this because you never add poisonous chemicals… i understand it doesn’t achieve a full conversion which is fine because i plan on making a blend of cbd/cbda/cbg/cbga/d8/d9/thca in a tincture.
call it a 1:1:1:1:1:1:1??? probably need a different name for labels lol too many 1s
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