im a gang member and im also here in the forum (but very quiet ) while i was collecting all needed parts for my short path destilation setup. but i just completed it i think.
any recommendations please? and i would have some questions maybe some experienced users
can give me some answers please…
inventar:
all glassware ( from destilation head to coldtrap)
goldleaf heating mantle
huber chiller -40 to 200 degree celsius
vaccubrand vacuum pump + cvc 3000 controller
edwards nxds vacuum pump
and all chemicals ( clays, mag sil, cole and so on )
it took me some time to collect all things but now i want to start to destill my ethanol and / or hydrocarbon extracted crude oil.
-any recommendations for this prouducts in this setup or is something missing?
-i have some short path SOPs including the glg one and https://www.grmlabs.com/post/short-path-distillation-standard-operation-procedure-sop and another one but i would need some more informations about the temperature in the condensor when its about to pop. is it 45 degree celsius?
and what vac level is it then? i mean to which temperatur i set the chiller for the condensor?
-on the vac controller i dont get below 12 mbar is this enough ? are the edwards nxds pump and the vaccubrand strong enough ?
-any more tips , recommendations or anything ?
thank you for reading and would be super nice if anybody with experience can give some help.
(there might be a reward too)
Vac as deep as possible. Deeper vac, less mantle temp. There are a few of us who have detailed spd threads on here. Read thru a few of those for more pointers.
Seems like you spent quite a lot of money on some of your gear, and not enough on other pieces.
The step down transformer suggests you got a 110V mantle, yet 220V are easy to find, and often cheaper. You purchased glass with gl-14 connections, which are prone to leaks, and make it harder on your vacuum pump.
The vacuum controller is nice, but absolutely not a necessity, and for the price of that dry scroll pump you could have purchased two more capable rotary vane pumps.
There are folks paying less for their entire production rigs than that pump…
Throwing a little more money at the problem and having a local glass blower (If you’ve got access to one) upgrade those gl-14 connections to 24/40 ground glass & getting a kf-25 SS bellows would seem appropriate.
the task that huber is performing does not require a unit capable of refrigeration. a simple heating circulator is sufficient. I’ve used a bucket heater and a $15 aquarium pump.
this is correct. is not equally spent but what to do there were some opportunity and life is a journey im not yet arrived but on the way.
the heating mantle was a mistake it came in 110v but needed 220v but i like the goldleaf heating mantle with this heated top thing for the flask. it was not cheaper.
yes the glass parts, especially the destilation head could be better.
and this gl14 connection on top of the destilation head you mean?
the vacuum pump you have, while a very nice pump, is not really the correct tool for the job. ideal would be a dual stage rotary vane pump. see: Oil-Free Vacuum and Dry Vacuum Pumps
an Edwards E2M28 is the “gold standard” on this sized rig, and a used Alcatel 2021i is the budget approach.
I’ve posted pictures around here somewhere of an Agilent dry scroll that pulled rotovap & Buchner duty and died early from the liquor it was forced to inhale.
I would suggest a new head with fatter column and 20° angle. Then a swing arm or pistol receiver and wide bore trap. What size setup is that? A 1L or 2L?
We can alter your cold trap and throw on some ground joints on there for full bore. You might want to throw another trap on there for extra protection for the pump. That should do the trick.
All the above should get better results and a faster distillation. That pump is rated to pull down to like 5 micron but in my experience they usually stop at about 50 micron which is a little high but low enough to use. If you pair it with a diffusion pump, then that sucker will rip.
Shoot me a pm if interested and I’ll send you a quote for the repair and new head.
Dry scroll can survive as long as you are absolutely anal about cold trapping the shit out of your rig (probably want a second trap). A super ghetto way to keep it healthier is to heat the vapor after the trap so that it doesn’t condense while being compressed in the pump. This is safer on a water cooled pump (like the multistage roots style) because there’s no risk of overheating the pump, but it works nontheless. Maybe consider only running the heater for devol./heads, after which there shouldn’t be substantial condensable vapor anyways. I use a hot water heater element directly in the piping but then again I have big pipes (insert joke as necessary).
