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Author: Subject: DIY distillation app
postart
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[*] posted on 2-3-2011 at 12:52
DIY distillation app


hello, I have been thinking about how one might construct a distillation/reflux apparatus DIY. The apparatus would be for chemistry not brewing so it would have to be resistant to strong acids, bases, Cl, Br and so on. I'm not a glassblower or welder and am trying to figgure out something that the average DIY chemist in need could replicate. All I could find on the net was for brewing equipment. I was wondering if there is some sort of teflon spray in a can that could be used to coat steel rendering it chemical resistant. I thaught of a pot with the lid sealed on with heat resistant epoxy then use metal tubing. Im not quite shure how it would all hold up no more than aspirator pressure would be applied to the apparatus. Any ideas would be great or better yet has anyone done this before themselves?
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smaerd
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[*] posted on 2-3-2011 at 13:11


Honestly a 24/40 glass distillation set up would cost around $100 and would be sure fire. The beauty of the glass also is you can reflux, do vacuum distillations, stir through it, add on to the set up, etc. I wouldn't ever substitute a good glass set up.

I'm not to sure about your question though, so sorry if this post is irrelevant.
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Bot0nist
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[*] posted on 2-3-2011 at 13:14


For strong acids and such you'll need some Pyrex glassware with all glass tubing for a condenser. As for the joints, rubber won't work unless you don't mind eating them up and adding contaminates to the product. I think some members have had luck with Teflon tape at the joints. IMO save up a bit and get one with ground glass joints and a nice condenser. unitednuclear.com has a nice one for sale. $120 us I think for the 500ml setup. $200 for the 2000ml setup.

Search some of the HNO<sub>3</sub> distillation threads. I think it is discussed a lot there.

[Edited on 2-3-2011 by Bot0nist]
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cyanureeves
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[*] posted on 2-3-2011 at 14:04


most of your stuff will be contaminated if you use steel.epoxy will find its match eventually and escaping fumes can mess you up and your surroundings.trying to find glass that is bent and can be used for condensing or to channel distillates is almost impossible.look at the price for bent adaptors!there is almost nothing out there that can be used in its stead and acids will find cracks you cant even see on porcelain coated pots so thats ruled out.
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postart
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[*] posted on 2-3-2011 at 14:08


Thanks for the replies I think I'll start saving to save myself a headach.
BTW can a distillation condencer also be used as a reflux condencer without modification?
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Magic Muzzlet
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[*] posted on 2-3-2011 at 14:11


Don't buy the united nuclear distillation kits, they are basically useless along with the condenser that comes with it. If it was the other type of Graham condenser it might be useful to an extent but it is not good for very much at all.
I made this mistake when i bought one, better off buying from UGT or something.
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Bot0nist
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[*] posted on 3-3-2011 at 06:49


Magic Muzzlet, can I ask what problems you had with your distillation apparatus or condenser? Leaks? All the glass I have gotten from them has been acceptable.

[Edited on 3-3-2011 by Bot0nist]
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Magic Muzzlet
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[*] posted on 3-3-2011 at 08:35


The type of condenser can't be safely used for reflux and it is sometimes a pain to distill certain things with the downward configuration and all. If you get a RBF, adapter and then use the condenser it builds up pressure and is just a pain in the ass. It is better to buy a proper setup with a better condenser than to buy the odd united nuclear flask and condenser.
I feel this way because when vacuum distilling and fractional distilling you can't use the setup from united nuclear anyway, can't use the condenser really either, so I feel it is a waste.
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hissingnoise
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[*] posted on 3-3-2011 at 08:42


Quote: Originally posted by postart  

BTW can a distillation condencer also be used as a reflux condencer without modification?

Some people run coolant through condensers during reflux!
For use with high-boiling liquids they should be air-cooled to avoid undue thermal shock . . .

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[*] posted on 3-3-2011 at 08:46


@Magic Muzzlet
Thank you. So you recommend UGT. I have used U.N.'s setup, but really only for ethanol distillation. I did have trouble condensing HNO<sub>3</sub>, but I had attributed that to operator error. What you say makes sense. I will check UGT's prices out today, and thanks again for the testimonial.

[Edited on 3-3-2011 by Bot0nist]
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Magic Muzzlet
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[*] posted on 3-3-2011 at 08:50


No problem, also keep in mind that eBay often has very good deals on glassware too. There are a few sellers that often have Pyrex and chemglass items at reasonable prices and great condition, always something to keep an eye on. ;)
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hissingnoise
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[*] posted on 3-3-2011 at 08:55


I got a fritted funnel from UGT years ago---it turned out to be Wilmad!

Good supplier!

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[*] posted on 3-3-2011 at 09:01



only the inside of the condeser has to be glass..

what if you got a glass tube and ran it down the length of a peice of pvc piple with two endcaps with silicone drilled holes to let the glass tube through

i guess you whould still nead to use a rubber cork.. but there disposable.

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[*] posted on 3-3-2011 at 09:10


Quote:
The apparatus would be for chemistry not brewing so it would have to be resistant to strong acids, bases, Cl, Br and so on.

You should probably think about what you want your set up to deal with.
Even if glass is the most usual (not completely, but it should be usable for most purposes) material for chemical experiments" other materials should be fine.
If you're trying to distill e.g. organic solvents a copper distillery (DIY, or bought however) could do it.
Further usage of metal-condensers is necessary while refluxing over hazardly moisture-sensitive set ups, to prevent every failure with leakage of water into the apparatus (Drying solvents over elemental sodium)
Further if you wont waste to much water, or, how already mentioned, you're going to distill a high-boiling substance, an "air condenser" is necessary.

[Edited on 3-3-2011 by Chaoschemist]

[Edited on 3-3-2011 by Chaoschemist]
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hissingnoise
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[*] posted on 3-3-2011 at 09:31


I just cannot understand why people continue to fuck around with stoppers, teflon tape, alufoil and that shit when a simple all-glass apparatus costs a few euro . . .

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[*] posted on 3-3-2011 at 09:53


You don't need to buy a complete kit. If you have some patience, you'll save yourself a lot of money by constantly checking eBay until real bargains come up. Of course, if you don't want second hand stuff then it will be considerably more expensive.
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[*] posted on 3-3-2011 at 09:54


Fear of breaking it?
In case of a larger setup/speciality cooking (e.g.pyrolysis) it could be recommendable to use alternative compounds than glassware, but I guess nobody expects to make extreme huge apparatuses, simply due to the increasing requirements in safety issues.
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Melgar
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[*] posted on 4-3-2011 at 00:25


For temperatures below 150C or so, I've built a distillation set out of empty glass wine bottles/jugs and had it run fine without breaking. I did have to buy some rubber stoppers from the brewing store (which I glued in place with silicone caulk), and also had to buy some pyrex tubing and a digital thermometer. Granted, this glass will crack if exposed to sharp thermal gradients, so whenever I used it I always set it up cold, put the bottle I was heating in an oil bath, then slowly turned up the heat until it was the right temperature. I wouldn't move anything if I could help it until after it all cooled off either. This worked pretty well for stuff like nitric acid, ether, toluene, ethanol, etc. I even had a reflux column filled with pieces of broken glass.

I never applied a vacuum to it, but it wouldn't be impossible. Just bore a second hole in the stopper on the receiving flask, then hook a really short piece of glass tubing going from the hole to one of those brake line bleeders. Of course, I wouldn't trust this setup to withstand more than about a 5 psi drop in pressure below atmospheric, unless maybe I was distilling water and had on lots of protective gear. I liked this setup because if I cracked the "flasks", they were pretty much free to replace.

I can draw a diagram if anyone's interested.
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[*] posted on 4-3-2011 at 03:21


In some organic synth russian chemistry book champagne bottles are cited as being good for high pressure reactors (up to 20 atm), protected by a metal tube.
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[*] posted on 4-3-2011 at 06:55


o.k. i use a european gravity coffee maker to make sodium nitrate from ammonium nitrate and bubble the ammonia through water.i got a couple of coffee pots that look like erlenmeyers and will probably work as erlenmeyer flasks.there is this video on youtube of a guy making nitric acid with a stainless steel distiller.if this video is real then the acid must be condensing before it can dissolve the steel.someone wrote that s.steal forms a passivation layer that keeps it from reacting but i doubt his acid is clean.i would'nt mind having a long glass tube to attach to my glass retort spout for better condensation.
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[*] posted on 8-3-2011 at 18:06


Hay I'm looking around the web at glassware and had a question. Are distillation and reflux condencers the same thing, or do I need a distillation condencer and seperate reflux condencer? as long as everything is 24/40 the condencer should work for distillation and refluxing, right?


Thanks!
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[*] posted on 8-3-2011 at 18:47


the reflux condensor looks totally different.i bought an allihn condensors because i thought the bubbles would help more with the condensing as opposed to just a straight tube like the famous liebig condensor and i saw a picture of someone using it as a reflux condensor.the allihn has to be used in a straight down position if used as a condensor or the distillate will get trapped in the bubbles and the liebig can be used in an angled position and still work.i wanted the graham condensor but its expensive. i still havent used the allihn and was a bit disappointed at first when i saw it used as a reflux condensor because i wasnt looking for a reflux condensor.the more experienced will answer your question better and i will be feeding off it as well.
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ScienceHideout
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[*] posted on 13-3-2011 at 07:51


If you get ground glass, size 19/22 is better than 24/40. Though a bit harder to find, it is smaller and easier to work with, not to mention cheaper.



hey, if you are reading this, I can't U2U, but you are always welcome to send me an email!


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[*] posted on 13-3-2011 at 16:20


Quote: Originally posted by bquirky  

only the inside of the condeser has to be glass..

what if you got a glass tube and ran it down the length of a peice of pvc piple with two endcaps with silicone drilled holes to let the glass tube through



I did this a little while ago (before I got an actual apparatus). Just do what you said, drill two holes in the pipe, and silicone caulk two lengths of glass for icewater flow.
This setup works fine for crude distillations, and pretty easy (and cheap!) too.

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cyanureeves
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[*] posted on 13-3-2011 at 17:47


not bad redox and bquirky. by the way you do know that is the way to make a sound suppresor?with the addition of holes in the center tubing(and up to 20yrs. in the penn).but that aside what would ya'll suggest for a bent adaptor?i mean one could find a boiling vessel even if only for one time use and you just came up with that condensing tube. but how would you go about hooking them up?
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