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Short Path Distillation

O

Old Gold

Active member
Pnw_guy said:
What are you guys doing to clean your glassware? Finding a brush skinny enough to fit in 24/40 joint in my boiling flask, but able to scrub all the walls has been a challenge. I can never get it spotless like want it.
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Soak a shop-rag in alcohol or acetone, put it inside the flask, and blow into it with an air compressor :dance013:
Maybe toss in some steel wool?

Otherwise, I usually soak things in acetone, and reuse that same dirty jar over and over until it's damn near the point of saturation (which means it's ready to be tossed into the clear machine!
 
T

thegreenman91

Member
Pnw_guy said:
What are you guys doing to clean your glassware? Finding a brush skinny enough to fit in 24/40 joint in my boiling flask, but able to scrub all the walls has been a challenge. I can never get it spotless like want it.
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Usually at the end of the run I leave the boiling flask to cool overnight, warm it back up in the morning, pour out the residue and immediately pour in ISO, swish it around and the iso it heats up. Never get it spotless though, always some burnt residue, I've learned to live with it.
 
G.O. Joe

G.O. Joe

Well-known member
Veteran
pictureguy said:
Wouldn't this work for short path distillation?
http://www.labdepotinc.com/p-59710-24-40-flat-bottom-distilling-kit.php?c=534
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NO!!! It might work for flying glass shards.

Also, that's a standard distillation kit, except that the FBF's are useless for vacuum applications. Some are calling this setup - with RBF's - short path distillation, and maybe posting sorry howto videos, when there is no type of short path head.

Pnw_guy said:
Finding a brush skinny enough to fit in 24/40 joint in my boiling flask, but able to scrub all the walls has been a challenge. I can never get it spotless like want it.
Click to expand...

The item you're looking for is called a flask brush. They come in different sizes with nylon or hog bristle and either is fine.
 
Daub Marley

Daub Marley

Member
Old Gold said:
How are you guys greasing ground glass joints (or are you)?
Dow high vacuum grease. Make sure every joint is as clean as can be before greasing them. You must grease every joint. Glass joints in general aren't meant to together unless they have grease. They're liable to get stuck otherwise.
Hose selection? I was going for high temperature silicone hosing with hose clamps.
No need for the high temp stuff. The terpenes will dissolve most plastics so use rubber. Keep the section that goes from the cow to the cold trap short and replace often
I've been unable to pull the system too deep. The pump (Alcatel 2021i) pulls down to 15 mTorr or less on its own. I have Polyspring hosing connecting it to a vacuum regulator, and likewise to the cold trap and distribution adapter (which I'll probably remove soon).
You're a couple orders of magnitude away from where your pump should be. The welch 1400 is what is commonly used and it gets to 0.1 mTorr
I can pull on the regulator down to 450 mTorr, and my glassware only to 22 Torr. This is closer to atmosphere than my tiny beat-to-shit 3cfm pulls vacuum ovens down to.
I also noticed that water gets sucked through two of the three 24/40 joints between distribution adapter and collection flasks.

Glassware is from Xtractor Depot...Summit Research head with Chemglass everywhere else. Up to 285°C and still not at THC. I need a significantly deeper vacuum pull.
The vacuum regulator is overkill. Just run it as deep as it will go. Get rid of any thermometer adapter.
What do you mean water gets sucked in the joints? How would water get in there? Like water is getting sucked into the system from the joint?
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in blue
 
O

Old Gold

Active member
Daub Marley said:
in blue
Click to expand...

I've wanted that Welch for a long time now, and have a friend with a couple of them. The Alcatel Adixen 2021i is rated to an ultimate pressure of 1.5 mTorr, which is certainly good enough for some level of distillation.

I didn't think the regulator was too necessary. The thermometer adapter seems like a big place for leak. I was just interested in verifying my heating Mantle's digital temperature setting.

As for water being sucked in, I applied a small amount to the exterior of the joints. Two of the joints hhadhowed the water sucked in immediately and entirely. Tells me the joints may not be the best fit..
 
Daub Marley

Daub Marley

Member
Old Gold said:
I've wanted that Welch for a long time now, and have a friend with a couple of them. The Alcatel Adixen 2021i is rated to an ultimate pressure of 1.5 mTorr, which is certainly good enough for some level of distillation.
Yeah that should be good enough for some action

As for water being sucked in, I applied a small amount to the exterior of the joints. Two of the joints hhadhowed the water sucked in immediately and entirely. Tells me the joints may not be the best fit..
With vacuum grease the joint willl change from transparent to completely clear when you work it into the joint. Any spots that don't change aren't meeting together all the way, and is a good indication that the joints in general aren't fitting together correctly. All glassware has variation and the joints are often where the less skilled glassblowers mess up.
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Blue
 
oneshot

oneshot

Active member
Old Gold said:
Fats/lipids present in the boiling mixture surely increases the need to raise temperature, no?
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Yes. I just experienced this. I had an unwinterized batch of RSO and my THC wasn't coming over till 193C in the head. The aftermath material was absolutely disgusting.
 
S

shortwave360

Member
Vacuum Pump Questions

Vacuum Pump Questions

I want to create a universal vacuum pump system in my lab. Is it possible to tie in a huge pump with manifolds that pull ovens, distillation station, extractor etc...

Been looking at putting this catch pot inline before this pump.

Am I crazy or would this be possible using regulators and other vacuum goodies? I would love to get insight and guidance for my vacuum system from a distillation expert. :thank you:
 
T

thegreenman91

Member
shortwave360 said:
I want to create a universal vacuum pump system in my lab. Is it possible to tie in a huge pump with manifolds that pull ovens, distillation station, extractor etc...

Been looking at putting this catch pot inline before this pump.

Am I crazy or would this be possible using regulators and other vacuum goodies? I would love to get insight and guidance for my vacuum system from a distillation expert. :thank you:
Click to expand...
check out http://www.vacuu-lan.com/ they do whole lab vacuum systems but I am sure you could imagine up your own and order parts through them.
 
K

KDT

Member
Daub Marley said:
in blue
Click to expand...

Im also using the alcatel, and have consistently good results (tho it's the only pump i've used for distillation). Usually my winterized oil will begin to distill THC between 205-215, depending on material... Is it safe to assume however that implementing the Welch with a lower micron pull will allow me to achieve the same results at a lower temp? Or, being that my CBN % on tests are lower than 1%, would it even be necessary? What other advantages might I see with a change in pumps?

thx
 
K

KDT

Member
Gray Wolf said:
Our best short path distillation results have been after winterization, with both the Kugelrohr and the Pharmgold Trommel molecular still test sled.

For de-coloring we use a chromatography column, with a proprietary mixture of random sized chromatography beads and rare earths, that we get from oregonmedicalgrowers.com. It comes out close to transparent, with THC typically in the high 90's.

I'll take a picture next run to demonstrate.
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Slightly older post I see, but am curious as to if anyone can recommend another source for the chromatography beads and rare earth GW spoke of to achieve ultra transparency? Anyone have any opinions and result info on this?

thx
 
A

AppleBrookFarm

New member
shortwave360 said:
I want to create a universal vacuum pump system in my lab. Is it possible to tie in a huge pump with manifolds that pull ovens, distillation station, extractor etc...

Been looking at putting this catch pot inline before this pump.

Am I crazy or would this be possible using regulators and other vacuum goodies? I would love to get insight and guidance for my vacuum system from a distillation expert. :thank you:
Click to expand...


We're doing this in our lab. They make big professional setups but I'm just going to plumb the lab with vacuum line and setup ports. You'll want a nice cold trap. I'm going to get a pump that will pull deep enough for distillation and get a controller to pull my ovens to -29.91.
 
mobin

mobin

Member
fuck paying people.

grow a pair and realize that there's enough shit available to you already that you don't have to pay someone to learn.

242y8hu.jpg
 
1

1labs

New member
Hello everyone

Hello everyone

So much good info, on this forum.
If anyone is interested in a complete lab setup from multiple distillers, co2 extraction, pumps filters and two short path distillers message me.
I will not sell it seperatly. Much to offer not cheap but a super good deal.
 
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