Even if said batch processing filters through a media bed? Most I know who do batch processing as you have described filter the media out of the solution using more (or a different flavor of) media.
If filtering two dimensionally (quantitative filter paper or something of the like), I would agree that a separate definition would be appropriate. If filtering (scrubbing) media out of a solution is performed with depth filtration (3D), then it still falls under the definition of chromatography, as the filter bed will cause the solution to elute components at different speeds/times (regardless of whether all “fractions” are collected together and mixed).
Yes. It depends where the remediation process occurs.
I was dealing with simple filtration as a physical separation process.
But if some chemical separation occurs there, then it turns to chromatography.
Don’t forget this only reduces Iodine to Iodide which must be washed out aqueously.
Check for residual Iodide by dripping aqueous wash liquid into a solution of ~1ml water, and a few mg of Silver nitrate (AgNO3) or Silver sulfate (Ag2SO4).
This test is highly sensitive and will form a precipitate of slightly yellow Silver Iodide.
That is extremely helpful. I can not thank you enough for that little tip about checking with silver nitrate. What concentration of silver nitrate do you use? does 10 mM work?
I know the paper that the iodine method comes from uses thiosulfate then brine washes. This is because brine is even more polar and can catch the iodide that is created right?
Even if it were, it’s not important here. It’s aqueous, that’s what matters.
I would advise against washing with any Halides before testing for Iodide. Do you know why?
The solubility of Silver halides is so minimal, it would probably be enough to dissolve 1mg of Ag salt in 1 ml of water and use one drop of that to test your aqueous wash.
I can’t guarantee Silver won’t interact with any dissolved cannabinoids or other compounds of the reaction matrix, so take it with a of salt.
Other than that, it would probably be worth saving all the washes containing Iodide and regenerate it with Oxone, as Iodine is obscenely expensive.
It might even be possible to only use a catalytic amount of Iodine and use something else as the terminal oxidant, maybe air would suffice.
The brine will also set off the silver nitrate. That kinda defeats the purpose of using it to test for iodine though as I only want to test for it after the washes.
I have only a barebones understanding of the reaction but the I2 is abstracting the H from CBD to form CBN (4 hydrogens). Which ends with CBD +2I2-> CBN+4HI, I don’t think the HI can then further abstract hydrogen. If there were some mechanism to regenerate the HI to I that would make the process much more manageable.
Hey any experience you (or anyone) can give me about other solvents for this reaction? Toluene is a pain to work with and I’ll have to get rid of it later anyway. Has anyone tried ethanol then using a liquid liquid extraction to get the CBN into the organics then finishing it off with the thiosulfate/brine wash?
When you reflux in a solvent can you exceed that solvent’s boiling point in the reaction mixture? i.e. if I use ethanol or heptane and just put it in an oil bath at 130oC will I be able to get the mixture up to 130oC or will it just stay at the boiling point of the solvent?
Cannabinoids boils a a higher temperature than that. If you reflux is cold enough, it will bring back the solvent in the reactor, which will keep on re-evaporating…
Why don’t you try the reaction without any solvent, to see how it goes ?
Silver nitrate won’t do much harm to the cannabanoids use a .05% by volume to remove the heavy metals & then after lle also pour over a t5/silica/Alumnia/DE column to remove solids & test for ph afterwards. That should remove all worries of i2
That’s a useful tip & trick brought to me by a ochem guy from this forum.
The reason I said to check ph afterwards wasn’t for i2 it’s for the solution after passing through the filtration. Assuming there is any moisture leftover after passing alumnia.
Never said one of them removes it so now you’re just putting words in my moufffff.
Also utilizing it during lle should help bring it to the emulsion layer instead of staying in your aqueous layer.
As you saying the column and ph is what is taking care of the iodine. It was misleading.
but I also knew you meant it was just to balance the ph to ensure further isomerization wouldn’t happen during distillation but I think @roiplek wanted to make it clear that wasn’t doing anything it self for the iodine which is a completely fair reply.
Yeah sorry if that was misleading, but totally NOT for the remediation of the i2 I would never suggest that. I mean cmon my i2 sop has been known to hit high 90’s & have no residual of i2, I ensure everyone I’ve taught it to or consulted it uses a very thorough lle practice for the procedure. If someone went on the tech site & went into the non-standardized section & did this without knowing or understanding how to properly they will every time have a shit production.
of salt.
