Asahi LLE Project: Need help: Testing separations for the ECR

[sidco]

Looking for a quick experiment to be done to test separations.

@Future, think you could lend a hand?

Test Method

1. Use a (2) test tube, separatory funnel, or vial.
2. Measure out a specific amount of room temperature oil/solvent mixture and record the volume and temperature
3. Measure out a specific amount of room temperature water and record the volume and temperature
4. Add the water and oil to the test tube, separatory funnel, or vial.
5. While capturing video, shake the two items for a few minutes and then sit in front of the camera so we can observe the settling and separations. Record the time it takes for the separation to occur.
6. Perform the task again but this time heat the oil/solvent mixture to 60C and record the volume and temperature.
   (WARNING, DON’T START A FIRE)

After this, I think I can get your hands on one.

[sidco]

@Beaker Is this pretty much exactly what you did here?

Liquid-Liquid-Extraction

This months med run proceeds after a dewaxing process which left the compound dewaxed and disolved in Methanol. A 100 ml addition funnel used as a sep funnel was used. Starting crude concentrate before refinement and dewaxing was one ounce. I chose to start with 50 ml of hexane on the premise that about two milliliters hexane to one gram of extract would be enough to easily hold it in solution. My rule of thumb is one gram of extract equals about one milliliter of liquid. On the left is the com…

[Beaker]

Essentially yes. It took a minute to figure out what they were saying.

My advice if running a lab for a video is to avoid shaking those tubes or funnels in a way that creates an emulsion. Rocking them back and forth is how I did it in my counter current labs using test tubes.

I personally would not be interested in heating a mixture of hexane and methanol to 60C for an LLE but it is an interesting condition for a test. Are they trying to boil it out? Methanol and hexane are immiscible but they do form an azeotrope.

[sidco]

I believe the goal is to create a rudimentary evaporation time over temp curve.
Honestly, 80% of what needs to be known can be gathered from your LLE post ( Thanks for that by the way )

I don’t think people understand yet how freaking cool that is.

[Beaker]

I ran the experiment multiple times for repeatability and realized that the process could have a profound impact on distillation ops. It did on mine hands down - higher recovery and all PLUS for the first time EVER I put off running first pass distillate again because it tasted so good.

With terps removed it changes the distillation game big time. Really big. It did for me on a micro scale and it is not lost on me at all how much potential for cost savings there is doing this. Next months med I believe I can come close to even nailing down a dewax AND a de-chlorophyll pass… though my grandious ideation is kicking in. After a major PTSD episode it does that lol.

Still though my labs running counter current seperations tipped me off and this might be so simple it is a face palm moment. Imagine starting a first pass with zero waxes, zero chlorophyll, and zero terpenes. This in exchange for two LLE washes back to back (with some caveats) that take less than 15 minutes and require no winterization. Do you think you could come up with an SOP that produced pretty fine oil on first pass? hehe, I do.

We hates chlorophyll, waxes, terpenes, and Baggins.

[sidco]

@Beaker

Baggins.

Thank you beaker, let me absorb this and get back.

[CollectiveObjective]

Oh we’ve understood the importance of this tech for quite sometime and will be sharing some of our R/D in this thread, as it is a CollectiveObjective