ILL NYE CBD-D8 Conversion Master SOP

@Miles-Beyond

He mentions stir speed 1 time during homogenizing the heptane and CBD but nothing past that.

Am I safe to assume it stays there (kinda goes against everything I’ve ran) or do you go full tilt on her?

I used a sep funnel until rotovap. once in the spd I stir about 400-500 while ramping up tp distillation parameters.

1 Like

Thanks for the support @Torgull im excited to get closer to shaving that unicorns ass

1 Like

What about during the actual RXN? I know you are using a BF and I’m using a reactor, just was curious.

Heads coming now

3 Likes

For those who wanna follow along from start to finish

7 Likes

I think the size of reaction vessel/volume/stir speed relationship is an important variable in the rate of reaction that is often overlooked. I think it was @Roguelab that mentioned stir speed early on.

On another note, how are you guys purging your heptane? I have customers looking to distill themselves to save and need to fully pull the hept beforehand. Currently recovering as much as possible then bump the temps and vac on the roto then redisolve in 5/1 etho to crude/recover X2 and sometimes X3. Just wanted to see if a thin layer in oven with vac was faster or another method utilized etc.

Keep on keepin on.

1 Like

This is what I do roto off solvent place flask in mantel at 140C and a hose from the flask to a coldtrap with large catch flask vac purge with spinbar in place for 2 hours
Under hard vac 2 stage 8cfm Edwards

13 Likes

@Roguelab as always thank you :raised_hands:

Nice @Roguelab !!

4 Likes

Fckin brilliant man. That’s a good way to keep the volatiles out of the trap/good pump oil

2 Likes

Of course MLC, level up together! :call_me_hand:t4::handshake:

Yeah, totally can do solvent recovery in a reactor. Actually did it today cuz our Roto was being utilized. Usually a slower recovery because the condensing coil on my reactors are much smaller than that on our roto’s. But yeah, it works. I’d still prefer to use a roto, but you can absolutely do “most” of the solvent recovery in the reactor.

2 Likes

Nice! Should have our 1220 running next week! Can’t wait!

Of course, level up together :call_me_hand:t4::handshake: The data from this weeks experiments… should be pretty awesome. Will definitely post up everything on here in a few weeks.

4 Likes

This is what its all about! Thanks so much @iLLnyeTheShatterGuy

2 Likes

The wife just picked up a 500ml kit so we can do 100g runs and try every goddamn perimeter (and scenario) we can (temp, time, argon with and without, etc.).

TLC plates should give us a base analysis to help us dial in the process a lot more quickly (since we are lacking in in house analytics, correct? Just a quick way to say “yeah… continue with this route” or “nope…scrap it”!

14 Likes

Another great initiative on your part (thank you to your wife too). Runs of 100gr of CBD may seem ridiculous to some, but there are many countries including Europe, where the prices of CBD are still prohibitive, 2000 € / KG of CBD if it is found by the kilo (if it comes from UK + 20% tax)! Besides, we mainly find only CBD and CBG!
The note goes up quickly, to experiment.

I know that it takes time, energy and money, you show altruhism which is rather rare these days! :pray:
For my part, I learned a lot with you and the others, is it continuous every day, thank you all, for your sharing, which I am sure will help many people around the world, at different levels.
Continue like this, do not change anything, you are perfect! :clap:

6 Likes

I’d give ya a like but I used em all up! Lol

Thank you for the kind words! More going up this week

1 Like

My run yield very bright pink (red) color. Could you let me know how to do color correction? Thanks.

There’s too many variables to just say what could’ve caused it.

If you’re already at a finished distillate and have a short path… just re-run it with 1% activated carbon or bentonite clay (T5) in the boiling flask. Then fraction as normal for any clay additions.

The better, safer, cleaner way to do color remediation of distillate is to do a carbon scrub.

  • Heat up the distillate and pour into a large Erlenmeyer flask.
  • Dilute it 2:1 (warm ethanol:distillate)
  • Add 1-2% activated carbon into the Erlenmeyer flask containing the Δ⁸:ethanol solution.
  • Heat solution to 80c for 30mins while homogenizing the solution in a vented hood or C1D1-2 room, after 30 mins… turn the stir hot plate down to 50c.
  • Once the temp has stabilized… filter solution through a Büchner funnel with appropriate filter paper to catch all residual carbon.
  • Roto that down to a relatively solvent free “crude”.
  • Distill again.

I personally prefer short path, but that’s just cuz it’s what I’m most comfortable fractioning on. If you’re a badass wiper technician… then by all means… (first, absolutely make sure you have no more residual carbon in your crude, death to your blades and evaporator) get good fraction separation, and minimize oxidation as much as possible.

PSA: You’ll always end up with a pink or red ring at the top of your liter due to oxidation. You can nitrogen back fill the jar while adding your disty… but when you open the jar… you’ll still get a pink or light red top layer.

Also… any of these post distillation runs, scrubs, etc… will diminish your Δ⁸ potencies. And increase 9, in my experience. Hence why I focus so heavily on my washes and tight distillation parameters. Instead of targeting a water clear finished product… I aim for a very pale yellow distillate. And can hit that color every time once I’ve dialed in my washes and distillation.

  1. First let’s start with your pH in your washes. Did you monitor and take pH readings of the aqueous layer each wash? End up neutral on the last aqueous collection?

  2. Distillation: Short Path or Wiper? Did you take a good heads fraction? Or get good separation on the wiper?

If I were to guess where your color came from just by dealing with this for so long… it probably came from your washing (LLE) pH or residual compounds, or during distillation by not fractioning tight enough. That’s normally where my pinks come in.

11 Likes

You’ve probably never been more wrong actually. What an embarassing attitude for someone of such a poor educational background. Dunning Kruger much?