Improved chlorophyll removal method

Thats exactly what I am into. :joy:

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Excellent job brother!

I wonder if inhaling the copper might become an issue?? Metal Fume Fever - an overview | ScienceDirect Topics

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Chemical CAS Number 6046-93-1 is your copper acetate? If I extract by putting dry biomass and methanol in a chest freezer thatā€™s -20F and then mixing, wait an hour or two, separate the plant material, rinse it with some more cold methanol, filter and evaporate the crude down to manageable levels, should your procedure leave my extract relatively free of fats/waxes to then SPD?

how u doing @TheMadChemist?

As I understand it, over time, that Mg ion is replaced by a hydrogen ion. Will a Cu ion replace this? Gonna try this on some crude from old, improperly stored material

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So if there is a concern of THCA conversion, what if you decarb first? Do you think it would produce Hydroxylated Delta 9?

The reason I ask is because in a separate thread I was discussing my saponification reaction of my crude prior to water washingā€¦and this crude is decarboxylated prior to my enzymatic and saponification reaction.

I tested my water washes, and my first water wash contained only about 20g (in 10L of wash) of Delta 9, some of that may be a bit of the hexane layer may have gotten pulled out. I can say that when I did my saponification reaction, there was definitely a lot more color in my water washes, so I may have been making chlorophyllin. I will have to test for that next.

I did test for anthocyanins though and Iā€™m definitely washing out quite a bit of those. Iā€™ll be doing another reaction this week and Iā€™ll submit my water washings to test for chlorophyllin this time and see what the lab says.

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Cu chlorophylls are a bit more stable than Mg ones and are actually being sold as food colorants.

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A water softening cartridge loaded with Na-rich ion exchange resin that will preferentially bind Ca2+ and Mg2+ by relinquishing 2Na+

Conceivably you could run your ethanol solution through one to process chlorophyll inā€¦some manner, at least

Hopefully itā€™s that hotfire Off-The-Shelf tek

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Very elegant - I love it, but DCM isnā€™t practical without recovery methods in place. Quick question on the terps - Iā€™m experimenting with a binary solvent to simultaneously crash out the terps and THC in their respective layers. Have you seen it? Hereā€™s the DOI: https://doi.org/10.1016/j.jclepro.2018.05.080

I had to add 100mmol of water to further polarize the polar phase; only then did the goodies crash out, developing a third phase in the sep funnel. Retail prices for isolated terps are higher than pure THC.

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Link is broken unfortunately

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Here, try this:

https://doi.org/10.1016/j.jclepro.2018.05.080

I copied that directly from the .pdf. I went to my browser, pulled up google, then pasted this DOI above. The top hit is the ā€œscience directā€ version.

Youā€™re using a molar ratio of menthol and acetic acid to extract terpenes with?

The menthol doesnā€™t change the profile?

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Happily, no. The E_f of the respective compounds appear to be just right. They used a 10krpm centrifuge, which I donā€™t have. This may be the reason why they didnā€™t crash back out of the DES, which is why I tried water, which worked. Iā€™ll post photos when I get a moment.

Also, the provocative nature of this is that Iā€™m extracting BOTH the THC and the terpenes. Iā€™d really like to crack this. I found a second paper with similar parameters - same molar ratios.

When you say crude extract, how concentrated is your extract? How much flower was used in the pictures you show here? I tried this method with a concentrated methanol extract and the good stuff did not stay dissolved, but turned in to what looks like a black/green grease after adding the saturated copper acetate/water solution.

Would copper acetate also remediate sulfur?

this entire thread seems off tracks ā€¦so to speakā€¦
I think a lot of people could spend time else whereā€¦

I dissolved sample of crude into IPA and added copper acetate. Dissolved quite well. Added water dropwise. Each drop turned milky when it hit the solution.

Dark green crumbly nasty precipitated out. Havenā€™t tried to see what it dissolves in. Anyone wanna smoke it and tell me what residual shit it taste like?

Shook solution with hexane, separated. Looked cleaner but maybe a lot of loss. Residual copper acetate from either my sloppy work or picked up with the hexane.

Must do more tests. The whole dropping green gunk is interesting.

The first time i tried this method, I was so disgusted that I almost said fuck it, cleaned everything up, (lots of nasty on lab equipment) shit can it all, put everything away for the summer and try again in the fall. But my anger didnā€™t get the best of me. From prior lab work fuck-ups I learned not to throw anything away. Save everything. If what Iā€™m seeking doesnā€™t show up when and where its suppose to, where did it go? Is it hiding somewhere because of poor instructions, or dumb assumptions on my part?

The method described in this thread is apparently one where the crude isnā€™t what I think of as crude, but one where the extract isnā€™t nearly as concentrated. I set everything aside in my garage and let it sit for weeks. Eventually the solvents and even the water evaporated. I then soaked all the filters and redissolved everything in to dry methanol. I used some more Copper Acetate (CA) saturated water. I didnā€™t add near as much water, mostly because I had figured out what was going on.

The extract was from semi-fine trim. There was was so much biomass, that I used 4 gal of MeOH (all I had). I got 3 gallons back. The mass and the MeOH had been in my chest freezer -40 degrees. I put the mass back in the freezer and the recovered MeOH when it was done. Ran 2 more gallons through. Mistake on my part. Picked up a lot of chlorophyll with the last 2 gallons. I would have done much better with 6 gal from the start. My theory was/is that because I picked up so much chlorophyll and boiled it down to what I consider ā€œcrudeā€ the amount of water I used had the canabanoids drop out of solution.

Having already replaced most, if not all the magnesium with copper the first attempt, and making the ā€œcrudeā€ less concentrated I filtered out the precipitate. A lot of the waste was trapped in filters and the 1/2 a roll of paper towels I used cleaning up the mess I made from the first try. (More or less self filtered the second attempt, there not being any water left.)

I let the redissolved extract sit for a few days in my fridge. Some crystals formed/stuck on the surface of the glass containers which I decanted. (I think it was some kind of wax, as they dissolved in water.) I then did multiple Hexane washes and a short path distillation to come up with 50 grams of beautiful amber oil.

Iā€™ll try this method again with extract from flower sometime in the future.

The link no longer works, so can you please upload the file again and edit the link.

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Original link fixed.

Yā€™all just needed to remove the spurious ā€œ:ā€ at the end (kids these daysā€¦).

Corrected link was also two posts downā€¦