Azetropic removal

Whats a good way to remove azetropes from a distillate other then water distillation or thin film

@Fadedawg @gwpharms @

Do you know what all is in this mixture you speak of? I'm assuming you've tried vacuum distillation and that has not worked for you. Your other easy options may involve the addition of another solvent or possibly some sort of inorganic
It could involve getting into some nasty things.
There is those ones that are impossible to break within reasonable means. What ideas have you had what have you tried?

There is some basic fundamental info in zubrick as always. More in depth in vogels. or whatever text books you crazy kids are using these days. i don't keep up on them all.

I tried water at first...50 ml to a 500ml solution.... Then alcohol...same ratio....then water again at at 20% ratio...then i tried thin film wipe diffuse in warm circulateing air for 3 days...it started to lokk clear but i colleted into 1 dish an it got soupy n blonde instead of clear. Yellow..still taste minutely of limone. But more so other terps im detecting

dabbindylan said:

Whats a good way to remove azetropes from a distillate other then water distillation or thin film

Click to expand...

Which azeotrope?

I lack equipment to tell u for certain...im guessing d-limo as this what i use to extract the raw oil..i then distill out terps thru multiple distallion. My mantle stirs and im pulling a 1 torr vacuum

My heads start at about 180c i range up to 200c on the boiling flask. No vacuum leaks...no vacuum grease..ptfe...im just really confused why its happened

Yeah aezreotopes can suck. It's of course impossible to save for sure what might be done without knowing all of the contents and their bp's . But my wild guess would be distillation with a metal or a solvent. like how benzene is sometimes added to ethanol to break the aezreotope. Or magnesium. Very dangerous to distill though.
Maybe less vacuum? Once you get down to 1 torr bp's sometimes get closer together again. Adding a little pressure May spread them out a little more . It's a crazy world in a reduced pressure environment. Molecules do all sorts of crazy things

Sounds like you are in the right temperature range, though a little high on pressure.

Shortpath distillation isn't my area of expertise, and much of what I do know, I learned from folks I have non-disclosure agreements with, so let's be safe and see what Pharmer Joe, our SPR short path guru, is willing to share.

He not only took organic chemistry in this century, but builds his own short path equipment, so I shot him an email running your question and 1000 microns at 180/200C parameters by him. I'll pass on what he says.

I do know that Horatio was using a rotovape for azeotrope removal, which 1000 microns would be adequate for.

The guru that I go to for rotovape processes, is Michael Bishop of Heidolph, whom is bright, knowledgeable, personable, and helpful.

He can be contacted at [email protected]. He is also intimately familiar with our industry, so I recommend you also pick his fine minds for subtle refinements.

You could of course do it with a chromatography column, but using Hexane sort of negates the advantages of using d Limonene to extract with in the first place.

No other suggestions............

Maybe just acetate or something from decarbing temp flux??? Idk ive done another its came out tasteless however its really red???? Like not amber. Red...any knowledge of how this occours. I will reach out to bishop to see if he could share some info aswell...id so like to solve this mystery..or better get it tested

Might be getting a new mantle..i feel as tho mine may be fluxing in temps. Even with all my probes it just reacts so eradicate

That makes sense. What are you using currently?

dabbindylan said:

Might be getting a new mantle..i feel as tho mine may be fluxing in temps. Even with all my probes it just reacts so eradicate

Click to expand...