Any updates on your success? I actually just did a post about citric acid conversion and would love your input about it? Stay stoney and sorry for your shitty gov. laws. @Gwon
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Hey, sorry for not updating yet, i’m back at uni so not much free time to experiment/post and my cheap vacuum pump crapped out on me half way into distillation. currently awaiting delivery of a good used Pfeiffer Duo so my future distillations should go much smoother.
I ran two small 10g runs. one refluxed in IPA and the other in heptane. (the fumes were nothing to worry about I was just being over-cautious, but thanks for the tip that’s good to know)
I’d say that the IPA reflux seemed better due to solubility of the phosphoric acid but it was also wasteful on solvent as it was just washed away whereas heptane is recoverable.
I ran both for 2hrs, almost full conversion via beam test around 1hr30 (ipa) and ~1hr45 (hept) and both final products were very potent (small oral dose)
I’m looking forward to doing a larger run with proper distillation in the coming weeks
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the citric acid tek was enticing to me initially but the reflux times are very long and since trying phosphoric I probably won’t go back.
I tried it in water and neat. the higher temps-neat seemed to speed things up but as @JedClampet stated in his thread, it’s rather violent so make sure everything is well clamped and clipped.
with water I didn’t see much conversion until >12 hours anything I pulled before then would crystalise on cooling, neat I seen partial conversion via beam ~8hours @ 175-180. again this seemed like a lot of wasted time compared to the many other teks but it’s a good place to get your feet wet and familiarise yourself with the techniques while working with relatively safe substances
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Totally understand. My stir plate/hot plate just died on me after like 3 days of use. What I get for buying cheapo ones off amazon x.x; Uni is a lot to good luck there mate.
Nice. Glad to hear the good results. Potent in what ways can I ask? Notice any difference? can i ask why IPA vs. ethanol?
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Times aren’t so much a concern for me long as I can hit decent yields at targeted molecules and forego any nasty solvents/acids <3
Any links you’d recommend? Can I trouble you for some more details about your citric acid tek experience? What was potency like vs sulfuric?
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Do you have access to analytics or you planning to bioassay your way through this?
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Topics tagged isomerization << read through these, tons of great info and discussion surrounding the subject
Cbd isomerization to d8 and d9 thc << Jeds tek was first mentioned here then split off into his own thread which has been linked in your citric acid post, but he quickly moved on to pTSA as it provides a much faster and more selective isomerisation (his goal being full conversion to d8)
it’s a little abstract and pretty low oral dose but ~50-75mg provided strong effects, very relaxing, heavy body stone/nice glow for around 5+ hours. No ill effects that i noticed during or in the days following.
I’ve not much to compare it too, distillate of any kind isn’t really a thing here, we have some BM carts floating around but I don’t trust them due to bad experiences with synthetic cannabinoids during the “legal high” days.
Compared to my 25% THC medicinal flower i’d say the distillate is much less “heady” and a lot more body intensive so i’d have to deduce high D8 content but still a very enjoyable experience and good for my needs (watching tv, wrapped in a blanket not wanting to move without a care in the world for hours then the sudden urge to eat all snacks in the house 
)
I just had a few bottles of 99.99% IPA lying around and ethanol is quite a bit more expensive, especially for high purity.
Sorry, i have no experience with sulphuric. Acid’s are very difficult for me to obtain, I think even acquiring 85% phosphoric has gotten me on a government list as after purchasing i found it to be on an explosive precursor watchlist at anything >35% and as of October 1st new legislation states it’s illegal to use/own/supply or import… carrying a fine and upto 2years imprisonment 
most other useful acids are covered under the dangerous weapons act due to gang/revenge related acid attacks years ago… my only options moving forward are to extract/purify from hardware supplies or synthesise although i have seen pTSA for sale on ebay in small quantities under it’s alt name tosylic acid and i found a source for Amberlyst 15h, ion exchange resin beads that ships to residential without chemical licensing requirements. so these are my two options looking forward but for now i’ll run the rest of my CBD in phosphoric
As for citric acid vs phosphoric… most of my citric acid experiments crystallised immediately upon cooling and were discarded. one stayed oily for around 24hours before small crystals started forming so safe to say the first few were mostly CBD and the longer hold out was partially converted. the small successful run i had with citric was definitely THC but not as potent as my first phosphoric run. When i weight the two reactions together, the time/energy input for citric just wasn’t worth continuing with although if you managed to work out a successful sop then ran a large batch it would still be a viable option. 2-3days for citric vs 8 hours from start to first pass distillate with phosphoric. there is a clear winner regardless of higher potency.
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sadly, this isn’t an option for me until i befriend a discreet analytical chemist willing to run some for me. my coa would arrive with handcuffs or be presented as evidence in court otherwise lol
my current plan is just to follow a successful sop, run it through a column and distil to the best of my ability. the finished product will be used for a few carts and gummies. i don’t plan on sharing or selling so the risk is solely on myself
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Learn TLC then…
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not too much accessible info for the layperson out there on TLC
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still learning sir, lol.
I’ve not much experience with TLC, but i ran plates prior to running a column to determine my fractions although i’m just kind of winging it. on my plates i get 2 leading dots relatively close (~rf 8.4 & 7.4) with the lower dot having a streaky tail to around 6. then basically nothing bar a light streak below midway and then the lower line/initial dot-streak.
Am i right in assuming these two prominent dots are d8 and d9 separating? seemed to be no or very little cbd left according to alk beam test. Assuming this I discarded my first few clear solvent fractions then kept the yellow fractions roughly 3-9(first dot, second dot to end of tail) and discarded the rest into a collection jar…
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thanks 
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so i captured d8, d9 and a bunch of isomers in the tail most likely
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Running the fractions individually on a plate before combining might be informative.
Maybe. Standards are important. You would ideally know where CBD runs, because you ran your starting material and monitored the reaction progress.
Can you access any known D9?
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not distillate, i have medical bud. 25% thc <0.1% cbd. will i just make a dilution of this and use as a test?
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Yep, that should let you know where thca and thc run (decarb an aliquot).
If you want better resolution see:Flash Chromatography vs CPC - #8 by Cannachem
Bigger plates give better separation.
No idea which fractions you should have combined. That’s where analytics come in. Getting good at TLC isnt hard if you’re determined.
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so my next plates i can run a spot for my cbd iso, a spot for my bud and then a spot for my isomerisation product and use these as references to determine my fractions.
should i have just cut the tail off? instead of running the fraction into rf6 just cut it a fraction or 2 before?
thanks guys, great help
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That will give you CBD, D9 THC (assuming full decarb), and if you’ve got good separation, you can probably call the darkest spot that isn’t one of those two “D8”.
Whether or not you’ll be able to differentiate D8 & D9 from anything else you’re making is an open question, but you should atleast make the attempt.
Sounds like you’re on the right track
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thanks for your time
this started as a way to get cheap thc and replace my irradiated bud but quickly turned into a new hobby. i’ve spent more on equipment than i could vape in a year but i just don’t care lol it’s no longer about the drug and more about the process while learning life skills and enjoying it! seriously considering changing university courses to something more aligned with this field as i have much more passion for the sciences than i do for programming
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