Chromatography Units for CBD Isolation

Hey guys,

Wanted to try and get a thread going about Chromtaography set ups for industrial processing of crude/distillate to CBD isolate. For my own personal application, I don’t need anything massive, but am aiming to be producing around 3-5kg per day.
I don’t know much about chromtography in general, just beginning to dive into it. Trying to come up with a realistic budget for an ICO for our hemp processing lab and learning I have no idea what machine we would even need to achieve the results we are looking for, which makes finding a cost difficult, ha.
I have also read about CPC set ups and how they are apparently more efficient than traditional HPLC, but RotaChrom’s ‘Get a Quote’ page doesn’t even work and Gilson hasn’t gotten back to me yet.
I appreciate any help anyone can lend :cowboy_hat_face:

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Ctech glass sells a great little LC tube for about $65 I have used many times these last few years. I got the ¾ diameter unit. I also own two tall form buchner style quick sep funnels for taking the ideas tested manually on the small LC tube and scaling them to preping my medicine. For me this means I scaled up to one ounce in capacity from the small.

I use the process only for prep to refine D9 but the concept generally follows the same path as for any LC chromatography seperation.

You must choose from several parameters but chiefly what your stationary phase type will be (alumina, sand, silica gel, Magnesium Silicate, ect.). Then you must decide if generally less expensive standard phase or more expensive reverse phase is needed. Standard phase chromatography to me means that more polar solvents will more easily move compound off the stationary phase as it passes, so a solvent like Ethyl Acetate (a polar solvent) will easily move cannabinoids but Hexane (a non polar solvent and hydrocarbon) will barely budge cannabinoids off the stationary phase. Reverse phase is simply the opposite relationship but as a rule the stationary phase is much more expensive then (C18 silica gel is a reverse phase gel while silica 60 is standard phase).

Once you decide standard or reverse phase then your choice is to pull the solvent through the column using gravity (standard Liquid Chromatography), push the solvent through with pressure from above (Flash Chromatography), or pull by vacuum from below (Vacuum Chromatography). Your column choice dictates this. My personal fave is Dry Column Vacuum Chromatography. Dry Column is only available in Vacuum Chromatography flavors but can process MUCH more bulk less expensively than others.

Finally you must choose whether you will run the same solvent mix during the entire run (called an isocratic mobile phase) or whether you want the flexibility but more complex method of varying the mix ratio of any solvents used during the run (called a gradient mobile phase). DCVC shines when a gradient is selected but can be run in isocratic mode too. It just does not seperate nearly as well imo.

Good luck with your efforts. I have found learning chromatography to be an intuitive process once the words are defined. Actually the biggest hurdle is just learning what the words mean and not what is actually going on - essentially you are washing a “stain” through a column that some parts of the stain need stronger solvent to wash through than other parts and the parts are collected as they leave the column (often said as “elute from the column”).

Guren Tag! :nerd_face:

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Im on the other end of the spectrum i have a 60 cm colum Jacketted chromatography stainless steel. Looking for a SOP for this bad boy maybe using biotech approach and not just simple resin affinity or reverse phase chromatography. Any suggestions ladies and gents ?


image

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Awesome! A column like that would need somebody WELL versed and educated in just how to pack a column like that. Channelling of the mobile phase must be a bear trap in a huge column like that. It is hard to imagine how much solvent would be needed to run that from start until last compound elutes but it will need many buckets for sure.

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:metal::metal: You rock. Thank you for taking the time to break this down for me. I really appreciate it. This is very, very helpful. Like I said, I’m real new to this, so breaking it down into layman’s terms makes it much easier to understand.
It sounds to me that chromatography would not be ideal for producing large amounts of isolate. Unless you are buying some massive set up… Which has got to be crazy expensive…

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Damn, that’s badass! What would one of these run me?? Just out of curiosity.

not sure to be honest its custom.

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Did you buy this for thc removal from crude or to make isolate?

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THC removal

Here is an IG short vid of my small scale efforts using standard phase DCVC running a solvent tradient over silica gel 60.
https://www.instagram.com/p/BoWNJEDFQlJ/

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Thanks for sharing this man, this is cool. I followed you on IG too.
What solvents did you use for your mobile phase, if you don’t mind me asking? And what did you start with, distillate?

I always use Ethyl Acetate and Hexane as my mobile phase. This was some first run disty if memory serves. First run without distillation first will reveal a lot of green following the red brown cannabinoid colors but the cannabinoids definately overlap into the green band as well.

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Have you tried regular phase? Ive been able to get seperation via tlc and small columns. Cheaper and can re-use if you really need to.

Obviously cannot reuse as much as reverse phase but you can reuse a bit.

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@ZizzleB These threads may also be helpful for your pursuits. I’m in a similar boat trying to find a more easily scaleable method than chromatography for removing THC from hemp extract, so anything useful I find in experimenting with these methods mentioned I’ll be happy to share.

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Ah, thank you for this! I am going to dig through these now and I will also do the same, in reporting any useful info I find. :metal:

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I can help you with developing a method to pack this! I will likely need to get a spec sheet break down, or come there to check the build of it out in person. Do you have any solvent pumps yet? Isocratic or something like that? Or vessels to mix solvent ratios in?

What are you trying to achieve here? Seperation of d9 thc from the CBD? Or just purification of a crude oil?

Dm me and I’ll shoot you over my rates and a # to call.

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You’ll need a TON of c18 media, which can be used over 100 times if cleaned between runs.

If you want a great deal on media(Si60, C18, etc) for that thing hit me up.

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Have you ever used fumed silica or precipitated silica? I have a ton of samples laying around that I don’t have any use for at the moment.

Havent used them! Idk what their benefits may be, over standard silica.