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Thca crystalline
- Thread starter BioBuddha
- Start date
H
HemperorsKnight
I can't seem to find any tutorials that explain the process thoroughly
Interesting. So you think you would have gotten crystallization? I am about to attempt a slow evaporation process myself. I thought pangea was saying to use BHO right out of blast and slight purge, but you winterized your material and redissolved. This makes sense as I would expect a cleaner recrystallization with this process. Just not sure how to move forward.
H
HemperorsKnight
Thx @Pangea
[FONT=Arial, Helvetica, sans-serif]In that article they say,
"Conventional silica gel column chromatography techniques including Flash Column Chromatography afford poor separation of amounts exceeding 10 g demanding purification of the reaction mixtures after division into several minor batches."
But, from what I read, their method is not much different from Flash Column Chromatography.
My questions are:
1. What is the difference between these two methods? Why is Dry Column Vacuum Chromatography held as better?
2. Could you not just get bigger/wider flash columns and use beakers to collect bigger fractions for Flash Column Chromatography?
3. Where/how would you implement a UV detector in the Dry Column Vacuum Chromatography set up?
Article Link:
https://erowid.org/archive/rhodium/chemistry/equipment/dry-column.vacuum.chromatography.html
All input is welcome and appreciated.
Thanks,
Woojay [/FONT]
ClandestineChem
New member
Status on Method
Status on Method
Has anyone tried the method proposed in the beginning by Summit Research? Im willing to try it but have also found additional info verified by 2 US patents. The basic water solution (pH=12-13) also contains a saline solution (9g per 1L H20). Does anyone understand why? The method (see picture below) seems legit and it looks like solvent DCM (dicholoromethane) might be used to replace the solvent IPE in the figure below.
Status on Method
Has anyone tried the method proposed in the beginning by Summit Research? Im willing to try it but have also found additional info verified by 2 US patents. The basic water solution (pH=12-13) also contains a saline solution (9g per 1L H20). Does anyone understand why? The method (see picture below) seems legit and it looks like solvent DCM (dicholoromethane) might be used to replace the solvent IPE in the figure below.
ClandestineChem
New member
Did you ever try Summit Research method?
woojay said:
ClandestineChem said:
Someone actively on these forums has mentioned some success running chromatography in his CLS column (don't know what size, quantity, time, etc)
https://www.youtube.com/watch?v=7LBGQHjgHEw
https://www.youtube.com/watch?v=B_QyhG2-VBI
^Here are some nice guides I used to check out, MIT puts out a lot of good stuff, through OpenCourseWare and other pages. You can sit on YouTube and watch entire semesters of lectures in many subjects. Shoutout to MIT for promoting real education.
I'm gonna try to read the Summit Research method you mention but I haven't been able to bare that guy's arrogance and use of English any time someone links me to his page.
Off the top of my head, the salt solution will help neutralize excess NaOH, grabbing the hydroxide ions. This process might be finicky to an at-home chemist not using molar math behind the reactions, because excess hydroxide solution might degrade or oxidize the hell out your cannabinoid acids, and lower yield significantly. Also, it takes a good quantity of alkaline water to bond the cation to the cannibanoid.
Is the saline solution he mentioned regarding acid-base extraction or column chromatography?
It might help to use a slightly weaker base than NaOH also, like sodium carbonate or bicarbonate. Weaker bases don't fully disassociate in water solution, so you might have less chance of burning your product.
Last edited:
Summit... Notice no GW this morning?
https://skunkpharmresearch.com/2017/01/13/attacks-on-instagram/
"The cyclonic drier was not designed after a mother ship, but after the numerous cyclonic systems I designed for air quality control in aerospace. It is true that you beta tested the first prototype." -Gray Wolf
That 'bout sums up all the drama in my head
Thanks for all the kind and consistent work, Sir Gray Wolf!
That 'bout sums up all the drama in my head
Thanks for all the kind and consistent work, Sir Gray Wolf!
ClandestineChem
New member
THCA Column chromatography
THCA Column chromatography
Reply:
Thank you for the links however I am not sure what solvent(s) to use to re-crystallize THCA. I also dont see the thread to a working procedure to THCA column chromatography (please send me the link or thread title).
The saline solution is used in the acid-base extraction. Thank you for explaining the reasoning behind the NaCl. So far the steps I understand from the a/b Step is:
1.) Extract the plant matter in 500mL of Hexane
4.) Filter the solution with charcoal and celite to help remove pigments
3.) Prep a solution of 500mL of saline water with a pH adjusted to 12.7-13.2 with NaOH
4.) Combine and mix the hexane solution and NaOH solution for 20-30 minutes. This (according to the patent) forms THCA sodium salt. The THCA sodium salt prefers the aqueous solution compared to the hexane solution.
5.) Separate the two layers (hexane/water) with a separator funnel.
6.) Adjust the pH of the water containing the THCA sodium salt to 3 with a solution of HCL. This will cause the THCA sodium salt to precipitate out of solution. (Unsure about statement [please correct me if im wrong])
7.) Add 50mL of hexane to dissolve the THCA crystals. (Other sources use DCM or IPE [isopropyl ether] as a solvent for this step)
8.) Separate two layers (solvent/water) in a separator funnel.
9.) Evaporate the hexane containing THCA to yield crystals.
Please let me know what you think and the flaws in this procedure.
THCA Column chromatography
Reply:
Thank you for the links however I am not sure what solvent(s) to use to re-crystallize THCA. I also dont see the thread to a working procedure to THCA column chromatography (please send me the link or thread title).
The saline solution is used in the acid-base extraction. Thank you for explaining the reasoning behind the NaCl. So far the steps I understand from the a/b Step is:
1.) Extract the plant matter in 500mL of Hexane
4.) Filter the solution with charcoal and celite to help remove pigments
3.) Prep a solution of 500mL of saline water with a pH adjusted to 12.7-13.2 with NaOH
4.) Combine and mix the hexane solution and NaOH solution for 20-30 minutes. This (according to the patent) forms THCA sodium salt. The THCA sodium salt prefers the aqueous solution compared to the hexane solution.
5.) Separate the two layers (hexane/water) with a separator funnel.
6.) Adjust the pH of the water containing the THCA sodium salt to 3 with a solution of HCL. This will cause the THCA sodium salt to precipitate out of solution. (Unsure about statement [please correct me if im wrong])
7.) Add 50mL of hexane to dissolve the THCA crystals. (Other sources use DCM or IPE [isopropyl ether] as a solvent for this step)
8.) Separate two layers (solvent/water) in a separator funnel.
9.) Evaporate the hexane containing THCA to yield crystals.
Please let me know what you think and the flaws in this procedure.
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