I have not helium tested, and need tighter connections for the probe inputs where the kangaroo thermometer and temp probe go into the mantle
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Where are you placing your mantle probe? Are you using a thermowell? Do you have any o-ring style thermometer adapters on your system?
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USA Labs 2l set
O ring style
Read my chart wrong. 10 Torr is 10 thousand microns. The boiling point of THC cannot really be practically reached in vacuum distillation this way that I know of. The breakdown of your other components would be too much.
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You need to ditch those adapters of you want any chance of getting a high vac. Get a therometer well with the correct immersion length for your flask. If you have an internal probe on the heater that’s a better choice to use.
Check this out too it’s a Great read
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The only problem with the wells are getting smashed by a stir bar that decoupled, overshoot, and lack of total immersion. You can’t distill anymore once the puddle is smaller than the probe can reach. These are the reasons I control the mantle with a direct temp reading from the heating element. Imagine sitting on a phone book on a red hot stove. You don’t know it’s hot till the book is on fire! That’s what your probe experences.
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How do you know how long of a ta you need for your application? A few last pieces i still need to source before giving it a try.
I have one of those but I do not distill that way. I was only posting up the IG post because it happened to jump up as a post on IG after @Soxhlet mentioned their use. The IG page posted is a supplier that might be able to help you.
However, as nice as these are you should be able to pull a vacuum down to below 10 Torr (10,000 microns) without anything else in terms of hardware. O rings can and do leak but I have a horizontal rig that I can use a thermometer in with an o ring adapter and it works down to ¾ of one micron.
I had a bear of a time after getting my used Edwards 28 vacuum pump pulling down to any kind of reasonable vacuum. It was not one thing but rather a whole bunch of little things. Ultimately the way I solved it was to take EVERYTHING including the foreline trap off the inlet to the pump and placing my portable vac gauge (an HVAC gauge) right on the pump inlet with only a KF 25 barb fitting.
Once that pulled down to ¾ of a micron, then I added the next item. I immediately discovered my $525 forleline trap full of fresh alumina was leaking down pressure when installed. I took it off and kept going piece by piece until I could finally pull a vacuum down to ¾ of one micron with the entire system assembled. No problems since. This might be an option since you are just gearing up too.
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Forget vacuum leaks, just wait until you get a propane leak or an ethanol spill and blow up yourself and burn your employee’s corpse to a crisp. Fucking GROSS.
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Our new mantles have a built in thermocouple so you don’t need to stick it inside the flask. It’s actually a better configuration
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I’m not sure if my regulator is reading right, I hooked up an analog gauge to read in mmHG and it says i am pulling just under -30, but I have a stronger vacuum pump I am going to hook up and do a dry pressure test and see if I can get better vac. Maybe more grease and ptfe tape until I get some good glass. I will keep you posted, and thanks to all.
Too much grease will cause leaks via channeling. You should really get yourself a pressure gauge which reads in either microns of mercury or millitorr
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Good to know, I am almost positive the pump isn’t strong enough to pull that deep vac, manual says ultimate vac is 10 mbar/ 7.5 torr. So I have a 6 cmf CPS and I will see if that gets it there.
Preach it mister! Damn those thermocouple adapters to hell!
I just pulled 10 micron on my 2L with two oring thermoadapters on the system, while messing around with some bump trap tech. Threw a little bit of vac grease around em and had no issues
I’m not saying it can’t be done, it’s just a less than ideal setup. Lots of issues come from mismatched probe size to o ring I.D. not to mention possible contamination from grease. I don’t use grease on any ground glass joints, just ptfe sleeves. All those warnings on the grease made me very wary of using it.msds krytox lvp grease artno 80005031 en.pdf (52.1 KB)
Here is the msds, the polymer fume fever caught my attention, especially as this as a smokeable product.
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Where can the sleeves be purchased?
I get them on fleabay like this.
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