Sciencemadness Discussion Board - A GOOD distilling setup?

A GOOD distilling setup?

Duster - 14-7-2004 at 19:21

So I was looking around eBay and my VWR catalog (by the way, do they sell to individuals?) and I decided I needed a good quality distilling setup... Id say I have ~$200 to spend...

I decided eBay would be my best bet, and while prices were a bit higher than I wanted, I think I will be getting all my supplies from here: http://stores.ebay.com/UNITED-GLASS-TECHNOLOGIES

I want the following:

1000ml Round Bottomed Boiling Flask
500ml Round Bottomed Boiling Flask
Liebig Condenser
Distilling Adapter
Vacum Adapter

Yes I know I need the stopper too, but thats not really a big part haha

In any case, what do you guys think? Did I miss anything? Main think I want to distill is HNO3, though I am sure some other things will run through that as well...

How much HNO3 you think I could get using conc. H2SO4 and KNO3 in the 1000ml flask? I dont think the full 500ml, but how much less? Would it be worth the saved money to buy a 250ml flask?

Thanks for the help guys, hope to get this running soon!

Duster

PS: Before someone points out the obvious, yes I know I need a stand and heat source

EDIT: I was thinking to, to save money, to replace the distilling adapter and vacuum adapter with this:

http://cgi.ebay.com/ws/eBayISAPI.dll?ViewItem&category=2...

Only thing is, that would leave no way for expanding gases to escape... This a huge worry or can the glass take it? Or should I stick with my first combonation?

[Edited on 15-7-2004 by Duster]

Cyrus - 14-7-2004 at 22:12

Well a thermometer might be useful. And if you are going to be distilling HNO3, you might want a glass stopper with a hole for the thermometer. Just a thought.

I like homebrew distillation apparati better though. And I save about $185.

The distilling parallel adapter you linked to looks like
1- a very efficient way to destroy your flasks or get boiling hot acids on you
2 - a very inefficient way to distill, there is no cooling or water jacket on that tube at all. (except for air)

(IMVHO-I'm no distillation expert)
I may be wrong, as I have never used a piece that looked like that, someone who has might want to correct me if I'm wrong.

The_Davster - 14-7-2004 at 22:35

I too am planning on purchasing my first ground glass distilling aparatus. I will probally just get one from UGT. But I want the opinions from the people here on what the best size is (24/40, etc,etc..).

Duster - 14-7-2004 at 22:38

Well, I was still planning to use my condenser on it, just further below it (further displaying I need a (tall) stand).

After I edited that though, I found another device that is similar, but has the added joint for a stopper...

And what kind of apparatus did you make? Note: If thats too off topic, then would you kindly U2U me? I am curious about that... And it doesnt use lightbulbs does it(not that it seems like a bad idea, but I just think I would break the thin glass enough times to warrant just buying jonted glassware)? At least for flasks...

Duster

S.C. Wack - 14-7-2004 at 23:10

You can put a vacuum adapter between it and the receiver to act as a vent, and vacuum is a good idea if you're distilling nitric anyways. But you will want a three way adapter eventually. If not for a thermometer adapter, an addition funnel. Or fractional distillation if you buy another condenser and want to do something that requires it. Chemistry is addictive. I don't see a need for that piece personally. If you want less glassware, think retort.

If you want to add, distill, and take the temp all at the same time, you will also need a Claisen adapter, and obviously an addition funnel.

If you buy a thermometer adapter from them, of course buy the nylon one with the bad picture, not the useless rubber one. Not sure if a carved plastic champagne cork will stand HNO3 or not, but its always nice to know what temp this or that is distilling at.

If you had more money, I would suggest buying two of everything, except just one mag stirrer/hotplate combo and one Claisen. You will be surprised that you ever thought of doing just one distillation at once, when you have a number of electrical outlets and hotplates are cheap at walmart.

Can't say anything about different sizes, just that 24/40 is plenty big. On the subject of big, you will also soon find a need for 2 and 3 L flasks.

You may want to hang out on ebay awhile before buying from anyone, to get a good feel for what costs what at closing.

Duster - 14-7-2004 at 23:47

Closing? I use buy it now

Hehe... Yea I guess I will stick with the three way adapter and vacuum adapter, I suppose if I dont get it now I will end up with it later on...]

I was thinking of getting a 1000ml retort to tie me over till I could maybe save up a bit more money for more/larger glassware... The only thing that throws me off about the retort is the lack of water cooling, I dont know if this is a big deal or not though, what do you guys say? Supposedly they were made (or at least are often used for) nitric acid distilling, but nevertheless, its just a class tube... I dont like the idea of exposed nitric fumes hanging around my lab... Thats the main reason I am getting jointed labware in the first place, that and so I have the ability to vacuum distill...

Well, thank you much and sorry for the lengthy reply

Duster

Lab glass

MadHatter - 15-7-2004 at 08:01

Duster, whether or not to use a retort really depends on what concentration
of HNO3 you want. As for cooling the sidearm of the retort, you
could fashion some plastic pipe and 2 carved out rubber stoppers
to make a cooling jacket. As for VWR, years ago I purchased some
labware from them. I don't know what their current policy is.

Johnny - 17-7-2004 at 08:37

As unique as it sounds I found that all I needed was a Cliesen and some TEFLON stoppers and built my own. It came out great and is acid resistent. I saved a bundle! But if you were to buy one I suggest that you also invest in additional teflon (or similar acid resistent) stoppers. If any "wear & tear" exists on a distilltion rig that where it would be.

Cyrus - 18-7-2004 at 12:19

My distillation setup is pretty small, I usually don't make or use very large amounts of chemicals. If I were to make liter upon liter of HNO3 this is not the exact setup I would use, it is too small IMO. I would just scale the thing up to whatever size I need.

Attached is an image. You get the general idea. The water jacket is copper straight from a hardware store, joints are sweated then sanded. The glass tube goes through a 1 hole stopper, the stopper goes into the copper jacket. I attach some polyvinyl pipes to the jacket, one of which go to a hose spigot.
The tube is 7mm flint glass, if this was really homebrew I would have to use Cu or Al pipes instead.

They would work almost as well. The copper water jacket is polished and coated with polyurethane to keep it nice and shiny. It works fine.

The round boiling flask is just there for looks, I would use an erlenmeyer flask or a test tube. And there should be ice in the large beaker.

The image was made with blender-anyone else a blender fan? Sorry for the large pixels, I scaled the quality way down to keep size down.

[Edited on 18-7-2004 by Cyrus]

condenser.jpg - 13kB

Magpie - 18-7-2004 at 17:43

That is a beautiful graphic! How long did it take you to do that? Where do you get "blender'?

The_Davster - 18-7-2004 at 20:57

I made one of those too.

However it still has a few unfinished parts. What are the names(as in what a hardware store would use) of the copper connectors you used to attach the coolant hose.
What is the diameter of the copper pipe you used? I used 1/2 inch.
Finally, I did not use rubber stoppers for the ends of the condenser, I used copper endcaps with a 5mm hole drilled in it. I am wondering what I should use to attach the glass tubing to the copper endcaps. I was thinking hot glue, but am worried that it might melt. Suggestions?

Btw, how did you polish your copper pipe? Mine is all green from the soldering and looks ugly.

Beautiful graphic.

Duster - 18-7-2004 at 21:04

I love that homemade setup you got there... I think I may just do that instead

And I know a bit about copper (just finished an ethanol still a week or so ago), and personaly I would use barb adapters... Doesnt matter what size I would imagine, and since it wont be under pressure, I think just screwing it in the side of the pipe would be fine, or you could use silicone, or hot gue (since its on the pipe, which is water cooled, it should be fine).

And for your end caps, I think I would go with hi-temp silicone or RTV, epoxy at best but that may be excessive... If you can find the correct size, a rubber groumet would work I think, or cut down a cork to fit (i was originally thinking of using cork for sealing the jacket on a retort I WAS going to get, since I think cork stands heat better than rubber)...

Edit: Sorry, while I said barbs would work, and they would, thats not what he used on his cooling jacket... His look like T-fittings with a rubber stopper in one (possibly two ends to seal to the glass), and then barbs in those...

[Edited on 19-7-2004 by Duster]

ahhh.... Blender

Polverone - 18-7-2004 at 23:00

Off-topic discussion:
http://www.blender3d.org

Blender is an open source 3D modeling, animation, and rendering program that runs under Windows and most Unix-like systems. It was first developed in the mid 1990s by a company called Neogeo in the Netherlands. They used it in-house for animation work. Neogeo eventually gave up on the animation business, but one of their people got permission to distribute the software and use it as the basis of a business venture. I first used Blender when it was version 1.30, I believe, one of the very first releases for Linux (it was developed for SGI, and for a long time ran best on that platform). It was slow (especially on a Pentium 133 with no hardware 3D acceleration!), quirky, and it crashed a lot, but I could tell that it was way ahead of the other free animation software I'd seen.

Blender was initially released completely for free, but no source code was available. As it grew more popular, more developers were hired to work on it, some venture capital was raised, and it was turned into a semi-commercial product of a company called Not a Number. There was a printed manual for sale (to supplement the very sparse electronic documentation), and there were extra features added that were available only to people who purchased "C-keys" to unlock the extra functionality. I ended up buying the manual and a C-key.

Blender was not in the end a commercial success. When the money ran out, another idea was proposed: this apparently commercially-unviable program would be bought from the people who had backed Not a Number and developed as open source. Thanks to the contributions of many people, myself included, the money was raised and Blender was freed. Nowadays, Blender has better electronic documentation than when it was a commercial product, and its functionality is the best it's ever been.

I used to play around with Blender a lot and I even made a 3 minute music video with it for one multimedia class I took a couple of years ago. Blender's greatest strength is in animation. It has traditionally been weak in modeling and its built in renderer is so-so (but fast). It is by far the most advanced and complete all-in-one free 3D package. The interface is very fast and efficient to work with once you learn it, but does not attempt to follow anyone's UI guidelines and takes a while to pick up.

Duster - 18-7-2004 at 23:04

Damn... A documentery on a free program... Thats a first... Hah...

Though you have inspiried me to download for myself now...

Cyrus - 19-7-2004 at 12:23

It took me a while to make that pic, maybe an hour or two, (all of the dimensions are pretty accurate) but I was doing it to practice blender skills, now I have found a better use for the picture.

My blender skills are pretty lousy and limited. I was interested in the interactive "game" part, but that is one area where blender stinks. My "games" ran at about 4 fps. :mad:

I have not done much animation, just images.

Polverone, do you have a link to some of your images? I would love to see them.
Good to see another blender user.

rogue chemist- I would not permanantly attach the water jacket to the glass tube, if the glass tube breaks, all I have to do is bend another one and slip it in. Stoppers work great, no leaks, aestheticly pleasing, easy to disassemble, cheap, and no worries about cracks because of the different expansion rates of glass and copper. (a very minor concern, but still

)
Cork might work better, but I doubt it withstands water for long periods as well.

The connections to the coolant pipe from the jacket are called "tube"

- I believe they are for refridgerators. Let me get out a ruler. Ah, the coolant pipe connecters are 3/16 in. ID Cu pipe, and the main pipe is 5/8 ID Cu pipe. I doubt dimensions are too critical. The connecters are attached to the main jacket tube by a tee with rubber stoppers.

I filed off the tin knobs from soldering, sanded the pipe down, and then used steel wool to get it all shiny, then painted it with polyurethane. Shiny Good.

The setup looks professional if you do it well. Edit- but the image doesn't do the real thing justice.

Duster, hose barbs aren't necessary. The coolant pipe connecters fit snugly with the correct "standard" size of latex or vinyl tubing, (they fit better with the latex though) and because there is barely any pressure, there are no leaks at all.

[Edited on 19-7-2004 by Cyrus]

David Marx - 20-8-2004 at 04:18

I have one of Corning's Organic Chemistry kits. It is all 24/40 Pyrex and comes in a padded plastic case. It is very similar to what you see in sophomore organic labs, except those are usually 19/22. I have been very happy with it so far. It works wonderfully for cleaning up solvents and other large scale work. I also have a few assorted pieces from Ace Glass which I am very happy with. Ace Glass is a respected company in the chemistry world and any of their products you might see second hand on eBay are well worth the price.

Next, I'd like to get one of Ace's microscale kits to better work my coordination chemistry.

Centimeter - 11-9-2004 at 19:07

200USD for that? I hope you didn't actually buy that. I just bought a 24/40 distillation setup composed of a 1000ml RBBF, 500mlRBBF, bent adaptor, 200mm liebig condensor, and a vacuum take off adaptor for 65USD + 20USD shipping. The kit is made out of second quality parts but it is more than good enough for low vacuum distillations. If anybody wants I can post the guys email and ebay-store link. I was wondering what is a good lubricant to use on the joints for HNO3 distillation. Preferably cheap and easily available.

Duster - 11-9-2004 at 19:14

I didnt buy it lol

And for a lubricant, I hear teflon is good... The sleevs (expensive) or the tape work...

neutrino - 12-9-2004 at 16:38

If you use a grease, use as little as possible, because even teflon-bases greases are attacked by HNO3 (the grease part, not the teflon part).

Cm: I'd like a link to the guy's ebay store.

Centimeter - 12-9-2004 at 16:54

If you want a simmilar kit, you will have to email him and ask for the kit containing second quality parts. This is of course unless he has one for sale already. Perhaps you could even mention my name; centimeter5426. He will probably know what you are talking about from that.

http://stores.ebay.com/kantu200-scientific-store_W0QQcolZ2QQ...

Centimeter - 18-9-2004 at 16:07

I know I am not sapost to double post but this deserves it! I just got the distillation kit in. I am speachless. Everything is perfect except for one minor flaw in the elbow joint. This was definately the most outstanding deal I have ever come across. I am seriously considering building a shrine to this guy!

rift valley - 19-9-2004 at 06:15

I don't know anything thing about distilling but I am trying to educate myself. What would a three knecked flask be needed for?

Quantum - 19-9-2004 at 08:30

I hope that setup never explodes on you. Would you trust anything coming out of china?

rift valley: A 3 neck flask lets you say add a liquid, inject a gas, and have a route to the condenser. Its just giving you more options to speed setup time and preform complex reactions.

Hermes_Trismegistus - 19-9-2004 at 09:04

it also allows for the use of a mechanical stirrer and/or a thermometer.

paccman278 - 30-5-2005 at 00:01

Quote:

Originally posted by Magpie
That is a beautiful graphic! How long did it take you to do that? Where do you get "blender'?

docberto - 31-5-2005 at 17:45

I love my 19/22 Kimble Kontes organic chemistry kit that I picked up on eBay for less than $200. Here's one with two days left in bidding: http://cgi.ebay.com/ws/eBayISAPI.dll?ViewItem&item=75195...
Instead of the regular RBFs that are in my kit, this one has a triple-necked 500mL and a 250mL with a temperature sidearm.
Cyrus, I never knew those were called hose barbs. My friends and I always called those nipples. Nipple flask, nipple adapter, etc. Now I know what to tell custom glass people.
There should also be perfluorinated lubricants that you could use on joints. Fomblin is the brand name of one that came up when I searched. They are perfluorinated polyethers, so I doubt they will react with much.

glass joint grease

expInfi - 3-3-2012 at 12:21

I have a vacuum distillation apparatus I bought.I am a newbie to practical chemistry.But I did pretty well in my graduation.So recently I developed a lot of interest in practial chemistry and trying to do some safe things...I was trying to figure out a good glass joint grease .Inertness is the highest priority.I see some brands online..But wanted to check with people who really use them and can give a good practical advise !

Thanks in advance !

entropy51 - 3-3-2012 at 18:09

Quote: Originally posted by expInfi

I have a vacuum distillation apparatus I bought.I am a newbie to practical chemistry.But I did pretty well in my graduation.So recently I developed a lot of interest in practial chemistry and trying to do some safe things...I was trying to figure out a good glass joint grease .Inertness is the highest priority.I see some brands online..But wanted to check with people who really use them and can give a good practical advise !

Thanks in advance !

Click on the Search icon in the upper left hand corner. Enter "grease" as the search line, select "Subject", and "All forums". You will get about ten hits. There, wasn't that easy?

Exactly where was this graduation that you did pretty well in? Did the school have computers? Did they have practical laboratory exercises in the chemistry courses that you did pretty well in? Most people who have taken chemistry at the university level can function considerably above the newbie level.

expInfi - 3-3-2012 at 19:33

Quote: Originally posted by entropy51

Quote: Originally posted by expInfi

1.I searched vacuum grease ,not grease.I will try grease alone now.
2.About the questions on my graduation.Your sarcasm does not deserve a reply.So that is ignored.

entropy51 - 3-3-2012 at 20:45

Quote: Originally posted by expInfi

2.About the questions on my graduation.Your sarcasm does not deserve a reply.So that is ignored.

No sarcasm intended. I just wondered why someone who claims some educational achievement cannot figure out what to grease joints with, for Gawd's sake. I suspect you don't have any chemicals and I certainly hope that you are not able to make cyanide.

[Edited on 4-3-2012 by entropy51]

expInfi - 3-3-2012 at 21:51

Quote: Originally posted by entropy51

Quote: Originally posted by expInfi

2.About the questions on my graduation.Your sarcasm does not deserve a reply.So that is ignored.

You are simply becoming unreasonably fearful.Google can tell you all sort of possible greases in this world.I asked precisely in my previous post that I wanted an opinion of someone who did it because only experience can teach you certain things.And it is just accidental that I refined the search with vacuum grease all the time that I didnt get the results.
I referred to my graduation because in the cyanide thread someone claimed that I do not have any clue on acid base reaction.I did not know that such revelations can come out from experts and just took an advanced bail for asking this simple question.
Anyway your interests about how my experiment should come out does not influence me anyway.So you are free to wish whatever you feel to.

[Edited on 4-3-2012 by expInfi]

[Edited on 4-3-2012 by expInfi]

expInfi - 3-3-2012 at 21:55

Anyway , grease search gives me some good links.Thanks for that.

Funkerman23 - 3-3-2012 at 22:51

Unless I am wrong( and doing it wrong as well) the Teflon plumbers tape should be strong enough to both "lube" the joints AND still prevent contamination of the batch. Teflon joints sleeves work as well.

expInfi - 3-3-2012 at 23:29

Quote: Originally posted by Funkerman23

Unless I am wrong( and doing it wrong as well) the Teflon plumbers tape should be strong enough to both "lube" the joints AND still prevent contamination of the batch. Teflon joints sleeves work as well.

Thank you! What temp range have you worked that with ? Is that inert even when strong acids are involved ?

Endimion17 - 4-3-2012 at 04:02

Quote: Originally posted by Funkerman23

AND they can easily snap the joints. Proven fact...

cyanureeves - 4-3-2012 at 06:34

i got a boiling flask and an adaptor arm siezed pretty tight right now after using teflon, pisses me off. i will try to heat it with a propane torch around the joint later today.i forgot i had keck clips but will use grease next time for sure.all in all i got the stoutest nitric i ever made and that made me run and buy new clamps and am looking for flasks and adaptors with thermometer ports on cr scientific that are affordable.grease is the word is the word! just now i freed the joints,all i did was hit it a couple of times with a rock and pulled it straight out.if i had twisted it off it would've broke for sure. yipee! oh! and it had a factory crack on the joint that withstood the heat,which is probably why it seized.

[Edited on 4-3-2012 by cyanureeves]

Bot0nist - 4-3-2012 at 06:53

Quote: Originally posted by Endimion17

Quote: Originally posted by Funkerman23

AND they can easily snap the joints. Proven fact...

Yeah, I just broke my 14/20 claisen because of Teflon tape, at 100°C too!. Its thermal expansion is to blame, IIRC. See the "Bad days in the lab" thread for a pic of my ill fated claisen. ( I miss it so much

)

Ohh, and for HNO3 distillation, conc. H2SO4 works great as joint grease, as long as minor sulfuric contamination is not a problem.

[Edited on 4-3-2012 by Bot0nist]

Funkerman23 - 4-3-2012 at 07:35

Quote: Originally posted by Endimion17

Quote: Originally posted by Funkerman23

AND they can easily snap the joints. Proven fact...

Well..crap( so much for avoiding the expense of the DOW grease...). I am guessing this applies to the joint sleeves as well as the tape?

Pulverulescent - 4-3-2012 at 08:20

Quote:

Yeah, I just broke my 14/20 claisen because of Teflon tape, at 100°C too!.

I've not had any problems with teflon tape!
It should be wound carefully so that it doesn't build into a lump around the joint.
No more than six turns should be used.
And the joints shouldn't be rammed together with too much force . . .

Funkerman23 - 4-3-2012 at 12:02

say what you will but given that Nitric acid is being distilled wouldn't Teflon joint sleeves be preferable? fluorinated greases are an option but for acid work I just don't see grease being the best option... But as I often ask; correct me if I am wrong.
Edit: found a thread( from 2009) regarding ptfe but there HAS to be some lubricant that won't contaminate HNO3 when distilling it...aside from the tape or sleeves that is.

[Edited on 5-3-2012 by Funkerman23]

entropy51 - 4-3-2012 at 14:33

Quote: Originally posted by cyanureeves

just now i freed the joints,all i did was hit it a couple of times with a rock and pulled it straight out.

With a rock? Why not a crowbar or sledge hammer?

Hint: A piece of soft wood is less likely to break the glass.