vacuum refluxing

[pickler]

PLease don't try to tell swim what temp his safrole comes over at. Believe swim when he's says 70-72c. Swim really doesn't care what you think.
We'll soon find out if I'm a chemist or not!

[wyndowlicker]

sorry but Swiw doesnt think his does this good.Didnt mean to offend.
I will choke untill I swallow!Who are you to judge or strike me down!

[Rhodium]

What is a micron? Microbar? In that case the temperature is fully reasonable. A perfect vacuum does not exist in real life, and if there was such a thing all liquids would boil below room temperature.

[wyndowlicker]

How if a 15 micron mbarr torr whatever what is the propper terms to use here.It says factory micron rating 15 that makes this pump pull safrole at 114c no better.H20 distills at 24c
I will choke untill I swallow!Who are you to judge or strike me down!

[Chromic]

A vacuum of 15 microns is 15 mtorr is 0.015 torr = 0.015 mmHg, which could easily pull safrole in the 70 degree range, probably even lower... I too doubt he's getting that good of a vacuum without a liquid nitrogen trap and new pump oil, but he's likely getting something close to 15 microns if his sassy is coming over at 70 degrees.

[Vibrating_Lights]

The pump he has does pull safrole at the temps he mentions. With the OEM oil without any special apparatus
VL_

[Chromic]

RB: your iso is awesome. The glycol made from the isosafrole as prepared in your procedure gave a thick slightly yellow glycol (made by peracetic in DCM). After H2SO4 reflux it turned to a light tan brown oil. 200µL of the crude ketone in 5mL of sat. sodium metabisulfate filled the test tube with tons of white crystals. Keep up the good work dude, now it's definitely safe to say that everyone can lose the continuous use of a vacuum throughout the KOH isomerization.  

[riobard]

Wyndowlicker, his 6 CFM pump is definitely able to pull that, considering that a 6CFM flowrate is total overkill for his setup.  The things that make inefficient vacuum for the rest of the smaller pumps are less considerable considering such a volumnous flowrate(things like using nonmetallic vac hose or using any hose with a flexible nature, things like waiting for the vacuum to equilibrate forever, etc. etc.).

Pickler, i hope you use cold traps.

[pickler]

Never used a cold trap riobard, just changed the oil a lot. But alas, the pump finally broke and swim had to get a new one.
We'll soon find out if I'm a chemist or not!

[sYnThOmAtIc]

If you don't know what the fuck your talking about then shut up and quit giving people a hard time(i have(finally) and only speak when I have a question or something to add). You obviously know nothing of these pumps. Their sole purpose is removing water from refridgeration units. These units can be inside outside in florida or alaska. The point is they need to be able to remove water at almost any normal enviromental temp. Do the math wiht the vacuum calculator on rhodiums. Safrole 234c boils now 55c water 100c well you figure it out.

I have the same ritchie (almost) pump but it's 3cfm and rated at 5micron. It refluxes safrole at 50c and distills it at 55c. Iso is collected from 65-80c range.

They only reason you would ever need and dry ice or ln2 encapsualted flasks or traps is to collect someting that is not to be collected. Like water or anythign else below 200c. With the gas ballast open you can save your oils purity. Like I stated in my isomerization thread I unscrewed the ballast after distillation started to get it to flow quickly. And I GOT FUCKING FALMED about it but it doesn't even change the vacuum that much and the separations had already been conducted this was jsut done to isolate the last fraction quicker like raising the bath temp 3c and that little differnece will not distill the resin left over. I have a friend that has a newer ritchie vacuum pump with regular ritchie vacuum oil that boils safrole at 38c. Now that is too low in my opinion 55c-70c is perfect. Though if your distilling liters of goods at a time then you would want the recieving flask in an ice bath to prevent too much evaporation.

Ever heard "Don't knock it till you try it"?

My opinion is these are the best pumps cause their cheap. Fuck em up ohwell. Get another only $200. Go find a robinair on labx that pulls the same vacuum and see what you pay. I've distilled acids and all kinds of nasty shit with mine and it still hasn't affected it. Though I change the oil after doing an acid distillation withthe ballast open. THough I have used the same oil for regualr distillations for months now with no ill affects (yet) some the solvents flushes and sealers used in refridgeration are much harder on gaskets and seals than any sassy derivative so change after every use is not nessecary but is worht not having to buy another pump.