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Heidolph rotary evaporators

Gray Wolf

Gray Wolf

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Lu lu lu lu lu lu lu lu lu lu lu lu! Hee, hee, hee, snicker, snort, snort, awhoooooooooooooooooooooooooooooooooooo!!!!!!!!!
Let the fun begin!

Heidolph loaned Skunk Pharm Research a rotary evaporator system, replete with -10C process chiller and vacuum pump, iffen we promised to kiss and tell.

For an opportunity to play with such a slick system, I'll blab all and post some pictures when we have everything operating smoothly.

Its a gaugus thang and so far everything has gone slick except for a fitting leak on the spanking new chiller tank, so we temporarily set it up running ice water until we resolve the tank issue. Heidolph says we are free to R&R the tank insulation to tighten the fitting, so we will do so today.

Please feel free to pile on with questions, which Sidco Cat has agreed to field and Heidolph offers her their technical full support.

More to come:
 
A

APK47

Member
Sounds pretty slick! I've been eying the Heidolph units for a while now, most likely what I'll go with when I go bigger than my old buchi 2L.
Did they supply you with a vacuum controller/Or any automation features?
You using primarily for winterizing, or do you have any other intentions?
 
SkyHighLer

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Yep, there is a Santa Claus... laughing all the way...............

"12-06-2013, 05:29 PM
SkyHighLer

E-cigs, but it ought to work for making other BHO goodies. Kind of stuff I want to see during an extraction lab video tour. Now if Santa would just bring a x-ray machine for the Doc at the old folks home.....sorry, I meant rotavap for the geezer in chief at Skunk Pharm! ;-)"

http://www.tokecity.com/forums/show...-for-E-Juice&p=1337560&viewfull=1#post1337560

Way to go Heidolph!
 
Gray Wolf

Gray Wolf

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APK47 said:
Sounds pretty slick! I've been eying the Heidolph units for a while now, most likely what I'll go with when I go bigger than my old buchi 2L.
Did they supply you with a vacuum controller/Or any automation features?
You using primarily for winterizing, or do you have any other intentions?
Click to expand...

Yup, it came with a vacuum controller and is programmable.

We have lots of fractional distillation plans for it, starting with simple alcohol recovery until we gets our chiller leak fixed, hopefully today. I'll share as we progress.

One experiment on my own list, will be to refine some d-Limonene and extract with it. I'll share what we come up with, and if there are any other d-Limonene extractors out there willing to share, they are encouraged to jump in.
 
HG23

HG23

Member
Nice! Really excited for this thread.

So do you have a fractionating column with reflux for the rotovap itself? Never seen that.

Can you the unit withstand pressure levels low enough to achieve molecular distillation? Maybe it needs to be really thick glass for that.
 
Gray Wolf

Gray Wolf

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HG23 said:
Nice! Really excited for this thread.

So do you have a fractionating column with reflux for the rotovap itself? Never seen that.

Can you the unit withstand pressure levels low enough to achieve molecular distillation? Maybe it needs to be really thick glass for that.
Click to expand...

It is strong enough, but we need a stronger pump and both the glass taper joints and the rotary vacuum union have to be tight enough.

As is, I've seen it as low as 9 mb, and we would like to be around .001 mb.

I also question whether the Graham style cold finger will work for short path, as it would ostensibly be hard to clean.

They have a dry ice cold finger that looks like it may work, and asked the Heidolph rep to review the possibilities with factory engineers.
 
S

SquattingBull

Member
This is a super exciting thread to have start right here.

I am super curious about the d-limonene extractions as well. Thats been some voodoo with alot of mysticism on the thread for a while. It is something we have had on our list to look into as well. Do you intend to pull limonene off as an azeotrope with water as the claims go on how other folks are doing it?

We have also talked about the idea of using the roto as a short path base and using different glassware with it but have always heard what HG23 said about the roto not handing that high of a vacuum.
 
Gray Wolf

Gray Wolf

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SquattingBull said:
This is a super exciting thread to have start right here.

I am super curious about the d-limonene extractions as well. Thats been some voodoo with alot of mysticism on the thread for a while. It is something we have had on our list to look into as well. Do you intend to pull limonene off as an azeotrope with water as the claims go on how other folks are doing it?

We have also talked about the idea of using the roto as a short path base and using different glassware with it but have always heard what HG23 said about the roto not handing that high of a vacuum.
Click to expand...

Our plans with d-Limonene are to start with existing published protocol and branch out from there. As you note, it includes washing out the d-Limonene with water.

All rotary evaporators are indeed not created equal, and having a rotary union is a big disadvantage when it comes to ultra low vacuum levels, so a system that doesn't rotate 360 degrees, like a Krugelrohr, has an advantage.
 
P

Permacultuure

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These rotovaps are top notch. the precision on every variable is great.......but don't get into one thinking your going to be pumping clear out in large volumes.
 
S

SquattingBull

Member
Gray Wolf said:
Our plans with d-Limonene are to start with existing published protocol and branch out from there. As you note, it includes washing out the d-Limonene with water.

All rotary evaporators are indeed not created equal, and having a rotary union is a big disadvantage when it comes to ultra low vacuum levels, so a system that doesn't rotate 360 degrees, like a Krugelrohr, has an advantage.
Click to expand...

Very cool I have read a couple different sources talking about it but with the exception of forum talk never a reference directed specifically at cannabis. It seems like a very time intensive prospect and I look forward to seeing your personal tek for it.

Would the Heidolph not fall into that category? The short paths like the Krugelrohr seem to have a disadvantage in the volume department? Clearly they Krugelrohr can make distillate (see what I did there) but it doesnt seem like its as volume oriented as the larger rotos.

Thanks as always GW
 
A

A6 Grower

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What about running a hot solution through the coils just a tad below your hot bath temp and have the collection flask in di/iso.... So the vapor would boil out of the flask, start to condense on the coils which would be hot enough to let it drip/run off into the cold collection flask. Ive noticed when my temps and vacuum are spot on when i'm recovering ethanol it only seems like the first 3 or 4 coils are doing anything and the rest are just there for heat dispersion. Random brain fart i had the other day while using the rotavap. Might work, might not, might work a little, who know....
 
A

APK47

Member
I was taught to only "use" the bottom 2/3 - 3/4 of the condensing coils. Any more than this and you are overloading the coils and losing volatiles to the vacuum pump. Not sure how much this practice applies to what we are doing, but I've always tried to stick to this principle.
 
Gray Wolf

Gray Wolf

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APK47 said:
I was taught to only "use" the bottom 2/3 - 3/4 of the condensing coils. Any more than this and you are overloading the coils and losing volatiles to the vacuum pump. Not sure how much this practice applies to what we are doing, but I've always tried to stick to this principle.
Click to expand...

I use 50%.
 
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