Distilling pure at 155C and less than one micron of vacuum

eugeneoregon

Active Member
This time lapse shot at 2 second intervals (60 fps) shows the second fraction being obtained. The vacuum reads less than one micron - extreme vacuum. The temp shown reveals that the fraction comes over nicely at 155C as read at the thermocouple in the heating mantel. The bulb is part of a stack of kugelrohr bulbs with a 50 ml boiling flask on its side in the heating mantel. The red tint in the video is from the red LEDs of the temp controller. The fraction is slightly yellow and clear. Potency is as high as it gets and the flavor is vague but absolutely delightful.

Now that I have slaved over hot dishes and bulbs in the lab it is time for one hell of a tasty dab!
 

MikeGanja

Well-Known Member
Thanks for posting your experiments. Whats the pros and cons with kogelrohr vs short path that most people use? Is it possible to scale it up to make it profitable?
 

eugeneoregon

Active Member
Thanks for posting your experiments. Whats the pros and cons with kogelrohr vs short path that most people use? Is it possible to scale it up to make it profitable?
My own observations using both my short path head and the bulb style method is that the short path rig is more involved to set up, there is more holdup to deal with, and the cross contamination is a bigger problem to deal with.

With the bulbs as soon as the decision is made to switch to the next fraction then the entire distillate path is removed (the bulb). I choose to slide the rig to the next bulb but could just as easily just replace it with a fresh bulb. I like the bulbs in place because I know nothing residual will be present in the next pulldown to vacuum after change over. Any contamination from the preceeding fractions in the system is completely removed from the system when a bulb is changed.

With my short path head this is not so. The distillate path becomes contaminated from the moment the most volitile fractions begin to condense as the first fraction along the distilate path. With the short path rig the entire distillate path remains in place between fractions with only the receiver flask being replaced. With the bulbs both the distillate path and the receiver are removed between fractions. I have caught pale yellow jelly like purity in between two contaminated fractions using the bulbs. With short path this is not possible when the first fraction contaminates the path. I work with gram sized quantities.

However the short path rig gives much more precise distillation data and without a doubt is much higher throughput. I have no need of throughput because of the gram size samples I use to experiment with and since I have no experience in processing ounces and pounds of this compound as a commercial operation does I honestly can't offer any evaluation about commercial possibilities. I can only assert from personal experience that I would always choose the purified form of this medicine as a purchase consideration above expense.
 

thump easy

Well-Known Member
My own observations using both my short path head and the bulb style method is that the short path rig is more involved to set up, there is more holdup to deal with, and the cross contamination is a bigger problem to deal with.

With the bulbs as soon as the decision is made to switch to the next fraction then the entire distillate path is removed (the bulb). I choose to slide the rig to the next bulb but could just as easily just replace it with a fresh bulb. I like the bulbs in place because I know nothing residual will be present in the next pulldown to vacuum after change over. Any contamination from the preceeding fractions in the system is completely removed from the system when a bulb is changed.

With my short path head this is not so. The distillate path becomes contaminated from the moment the most volitile fractions begin to condense as the first fraction along the distilate path. With the short path rig the entire distillate path remains in place between fractions with only the receiver flask being replaced. With the bulbs both the distillate path and the receiver are removed between fractions. I have caught pale yellow jelly like purity in between two contaminated fractions using the bulbs. With short path this is not possible when the first fraction contaminates the path. I work with gram sized quantities.

However the short path rig gives much more precise distillation data and without a doubt is much higher throughput. I have no need of throughput because of the gram size samples I use to experiment with and since I have no experience in processing ounces and pounds of this compound as a commercial operation does I honestly can't offer any evaluation about commercial possibilities. I can only assert from personal experience that I would always choose the purified form of this medicine as a purchase consideration above expense.
Do you think a glass blower sci of course could blow a piece that detaches at the top of the head were the condensing happens so that the cross contamination is avoided in short path also jacketed recieving flasks? It be easer to clean the head out and run a blow dryer through the head to get every last drop??
 

Jedb

Member
My own observations using both my short path head and the bulb style method is that the short path rig is more involved to set up, there is more holdup to deal with, and the cross contamination is a bigger problem to deal with.

With the bulbs as soon as the decision is made to switch to the next fraction then the entire distillate path is removed (the bulb). I choose to slide the rig to the next bulb but could just as easily just replace it with a fresh bulb. I like the bulbs in place because I know nothing residual will be present in the next pulldown to vacuum after change over. Any contamination from the preceeding fractions in the system is completely removed from the system when a bulb is changed.

With my short path head this is not so. The distillate path becomes contaminated from the moment the most volitile fractions begin to condense as the first fraction along the distilate path. With the short path rig the entire distillate path remains in place between fractions with only the receiver flask being replaced. With the bulbs both the distillate path and the receiver are removed between fractions. I have caught pale yellow jelly like purity in between two contaminated fractions using the bulbs. With short path this is not possible when the first fraction contaminates the path. I work with gram sized quantities.

However the short path rig gives much more precise distillation data and without a doubt is much higher throughput. I have no need of throughput because of the gram size samples I use to experiment with and since I have no experience in processing ounces and pounds of this compound as a commercial operation does I honestly can't offer any evaluation about commercial possibilities. I can only assert from personal experience that I would always choose the purified form of this medicine as a purchase consideration above expense.
So when you say "cross contamination", you mean because the heads and tails come through the same path as the main fraction? Are you using a single distribution adapter or a multi distribution adapter? Not that a multi distribution adapter alleviates what I think you're talking about, but it's definitely more efficient than a single adapter...
 
Top