Very cheap and improvised still

[blindreeper]

I have been looking at light bulbs lately and they are a nice size for a small flask. But there comes the issuse of with standing heat. Then I thought they are emant to be subject to heat. I really don't want to buy a proper still ( I wouldn't mind one though) mainly for nitric acid. But then you need a condenser type thing. I started looking at flurecent tubes. I found a small fluro 15mm dia and 50 cm long. I bought it go it home and cut the ends off (with a triangular file).

Then I cleaned out the barium compound (not sure what it is) but putting some cotton ont he end of a dowel and getting it out, the barium compound is what makes it white.
After all that effort I was left with a nice cglass tube about 45 cm in length x 15mm dia. I then wanted to try and bend it. I tried with a bunser to heat it up but it wasn't hot enough. The interesting thing is that it changed the flame colour to green indicating boron present thus borosilicate glass. So I went to the propane torch and it worked good but it was my first time shaping glass so of course I stuffed it. It is bendable an I practised with it after woulds and got it perfect.

I have seen big light bulbs and I estimate they could hold about 1 L. They may be fradgile but the could work for a simple nitric acid still. To connect the tube to the bulbs just put some Al foild around it then heaps of PTFE tape (plumbers tape). Of course this type of still is only air cooled but it will work if you bend it 5 cm from the end leaving 40cm to condense.

Has anyone done this before or am I just bringing up old stuff?

[Arthis]

When shaping glass, how do you make it melt and bend, and not break because of the heat ?

That sounds like good idea, though neon tubes are pretty thin. You make your condenser by putting a small one in a bigger tube, right ?

[blindreeper]

If you just run the tube over the very outer of the flame and gradually put it in the centre. Just don't let it get red hot or it flopps over. If you heat the end of a test tube red hot you can blow it :D I am just going to use PVC over the top of for the jacket cause if you use glass you would have to melt it around the other tube which would make it crack. But then again you could just put a cork in the bigger tube and bore a hole in it, that way you can see you vapor condensing. The tubes are about 0.5 mm, thats thin but you can still work with it.

[Arthis]

Care while handling it. Normally, lab condensers are about 1.5-2 mm thick (small ones, 1 foot long), and they're very fragile. 0.5mm makes it damn annoying to handle with care.

[blindreeper]

Well I'd rather take a little more care handling it opposed to paying $50 + for a normal one and still if you drop that it'll still break :rolleyes:

[knowledgehungry]

Very good idea Blindreeper, you may be useful yet:p. Thanks again.

[Tuatara]

Before going to the effort of making a still with this glass, soak some in conc nitric to make sure it will resist the acid.

To reduce the possibilty of stress fractures as hot glass cools after forming, place it straight into a container of vermicullite. This will help to anneal the glass as it slows the cooling rate right down.

[blindreeper]

Well I am trying to be useful and worth making history in the forum :D
What is vermicullite? I 'm guessing some sort of heated solid?

[Tuatara]

Vermicullite is mineral that has been expanded into a sort of foam like structure by intense heat. It has the same sort of density as styrofoam. It is commonly used as a growing medium for hydroponics. For our purpose it acts as a very light weight, heat resistant insulator. You can buy it at horticultural supply shops.

more info on Vermiculite (http://www.epa.gov/asbestos/verm.html)

[blindreeper]

Tuatara

Before going to the effort of making a still with this glass, soak some in conc nitric to make sure it will resist the acid.

Since when does all glass not resist nitric acid?

[Tuatara]

Ordinary glass commonly contains a lot of group 1 oxides as fluxes to lower the melting point of the glass. The nitric acid, (in fact most strong acids) will happily chew these basic oxides out of the glass, so that the glass will become very brittle - not what you want when distilling acid!

Here's some basic glass info for you:

Borosilicate glass: a.k.a. Pyrex, Kimax, Duran
* very little soda or potash, no lime, about 12% boron oxide
*High chemical resistance, low expansion coeff. (33E-7 per deg C)
* softens at 820C, working at 1250C, annealing at 560C
* used in scientific glassware, kitchenware

Soft glass: a.k.a. lime glass, soda glass
* soda, potash and lime added as fluxes
* more soluble, less resistant to chemical action than borosilicate
*expansion coeff ~ 93e-7 per deg C
* difficult to anneal
*softens at 690C, working at 1000C, anneal 510C
* used in bottles, windows, common household glassware, lightbulbs

Fused quartz
* nearly pure silica
*chemically inert, very low expansion coeff (~ 11e-7 per deg C IIRC)
*softening point 1650C
* used in precision optics, special scientific glassware

Vycor (R)
*borosilicate glass which has had all the sodium and boron oxide dissolved out with acid! It is then refired.
*expansion coeff 8e-7 per deg C
* being 96% silica it has very high chemical resistance
* softens at 1500C, annealing 910C
* used in high temp lab glassware

Info taken from "Glassblowing: An introduction to artistic and scientific flameworking", 2nd Ed. by Edward Carberry.

If I had a scanner I'd up it to the FTP.

[blindreeper]

Fuck, fuck fuck. Wait one more FUCK!!! Damn that sucks oh well at least I tried to contribute. Well I should be trying this arfternoon distilling nitric so I'll post here on how the still held up.

[Arthis]

Hey don't get angry. We try to help.

Tuatuara, here it's not common lightbulbs, but the neon tubes, so maybe, as the shaping is not the same, they need to put more resistant glass.. Or maybe as it diesn't get hot, it's lower grade glass...
Definitely need to be tested.
BTW, where is it written that those glass that you present whether resist NA or not ? The fact borosilicate glass is used in labs doesn't mean other won't resist NA, but that it's higher quality (less fragile, higher *global* chemical resistance,...)

[Tuatara]

Thats why I said 'test it first'. Its the only way to be sure. Test by soaking for a day or two in conc. nitric, then compare brittleness to original glass. Maybe it will work beautifully (I certainly hope so), maybe not. The idea is to prevent Blindreeper getting covered in hot acid through equipment failure:eek: .

BTW the glass tubing used in domestic electric heaters is fused quartz. Don't bother trying to bend it unless you have an oxy/hydrogen torch. Its the only flame hot enough!

[blindreeper]

Oxy-hydrogen ay thats a new one :rolleyes:
Well I don't have any conc. NA so I'll have to find out the hard way and go ahead and try it. Oh well wish me luck.

[blindreeper]

Good news, the glass was fine! I noticed no change in it. The reason my yeild wasn't that great was that I got impatient and heated it too much causing the HNO₃ to decompose in to NO₂. The other factor is that my bend in the tube wasn't all that great which kinda bottle-necked it so that stuffed it up. Now I am using a standard halogen tube (about 1 inch dia) and 48 inches long. Also it had no cooling (except air) so my vapour didn't condense to weel. So now I am using a large diameter tube, longer and I will make a pvc water jacket over it to use as cooling, but I think I may try just air cooling with the 48 incher cause I want this to be as OTC as possible. Just a note I am using pyrex/kimax flasks atm so once I have the condenser down-pat I'll buy some bulbs and try them, which will really make this project attractive. To seal the still you use teflon tape aka plumbers tape. I think that if you can get lightbulbs at your hardware store and can find ammonium hydroxide, gelatine, sodium hypochlorite, xylene and some welding argon you should be on your way to some nasty ass shit. I know bunnings sells all that suff...OT but when mega says "1200 mL of normal sodium hypochlorite solution", what is normal ? 1M?

Edited by Zaibatsu to fix tags

[mrloud]

Most discharge / arc lamps are made out of a quartz glass capable of withstanding the enormous temperatures they generata. Perhaps you should try to get your hands on some old mercury vapour or sodium vapour street lights.
Better yet, if you happen to live near a major sports stadium, climb one of the light towers and get yourself one of these (http://203.2.75.213/filetransfer2/powerstar.jpg) .

For those who are interested, the picture is of an 3,500 watt Osram Powerstar HQI/T

[blindreeper]

Why would anyone want one of those lightbulbs for? Well now back tot he condenser I now am in the process of making a water jacket out of pvc piping around the glass tubing. I'll try and borrow a digital camera some time to take pics, but once I have them on my hard-drive I have no idea how to get it to you guys...

[Arthis]

A bulb to make a round bottom flask to heat your acid.
Still wondering if it's worth the work since flasks are not expensive, compared to those refrigerant column of Liebig.

But with one of those big light bulbs you can hope making about any glassware you would dream about.

[blindreeper]

Ok guys, I finnally got pics of the still!!!

http://www.geocities.com/blindreeper_chemistry/improvised_still.html

Ok I know it's not the best format to put pics up with and some of them are a bit dodgy but hey I am a chemist not a photographer! Enjoy :D

[Arthis]

It seems to be a great system you made here ! Is it working now ? No more nitric fumes coming off the condenser without being condensed ?

To turn the photo, even MsPaint has this functionnality. You didn't search that hard, eh ;) !

[blindreeper]

I accually havn't tried it yet. I think I may do just a simple methylated spirits distillation or somthing to see how it holds up before I go and try nitric acid. It's not a condenser really, well it's all I could think of at the time and it has a very high surface area so it should condense.... hopefully :rolleyes: Also if you notice when it is all setup the "condenser" touches the bottom of the recieving flask so it wouldn't be to hard to stuff the neck of the recieving flask with some glass wool or somthing to stop any vapours coming off after woulds. I am interested to see who accually finds this usefull and would like to see more stuff made. Any requests or ideas that I could have a go at?

[Zach]

Lime works very well for slow cooling of glass and metals. Not the fruit, but powdered lime like you find at a garden store. I do not know if lime will impart any impuritys to hot glass though, so that'd be worth looking into if you're going to be using it for nitric.

[knowledgehungry]

Very, Very nice, i must admit that i am impressed, please let me know how your distillation goes, i think i shall try to make some distillation apparatus too.

[Arthis]

With this shape, won't you lose a lot acid that remains in the condenser ? Sure that may not be a lot depending on the flask you put :rolleyes: I couldn't see any water cooling though (missed it ?).

[blindreeper]

Well there is no water collong yet. This is just a prototype. If you see all the dimples in it there is no way to HNO3 can get stuck in there as they are round. I am going to make another of these "condensers" and then get a 2 inch (dia) fluro tube and get some cork and drill a hole in it so the smaller tube fits in it and then kinda stick them into the bigger one that way you can see your stuff condensing. I hope that made sense. When I get paid next friday I'll get some more tubes and some more gas for the propane torch (we had a big barbecue yesterday thus there is no gas in the bottle :p ) and I'll make a start on a still with a vigurex column leading to the "U" shaped still head and then to the condenser described above. Then I will try to distill some acid or ethanol from methylated spirits for fuliminates of course ;) (don't worry I'll distill the product many times before using it for...err...umm...:D )

+++++++++++

It's impossible to seperate ethanol from methanol by simple distillation, or any distillation process for that matter, as they form azeotropes with each other.

That's why methylated spirits are methylated...so it's impossible to make drinkable ethanol from it.

NBK

[Begste]

You ever look into using one of those water purifyers as a still? Get a metal one. Attach copper tube to the neck part. The only part you have to modify is the screw thing which holds the top and bottom on. I think it also has a rubber seal. Remove it, no big deal. Just dont fill it over the seal line.

[blindreeper]

Using metal would limit what you distill to "boring" things. Hence why going to the trouble of using glass.

[Mendeleev]

Pretty nice still! You know they have larger light bulbs right? I have one at my house in a light fixture hanging over the dining table that is about the size of a one liter boiling flask. Not sure what it is is called, because I don't have the box. Also, copper would not let you distill anything corrosive, but you could still do anything involving organic molecules. It could be used to create and purify acetaldehyde, ethanol, etc. Furthermore the hardware store sells maleable copper so you could mold it into the shape you want, effectively making allihn or grahams condensers. You could make a very effective condenser out of a copper coil inside a metal paint can full of dry ice. A bit off topic, but, there are no hydrogen oxygen torches, Tuatara. Hydrogen combusts with more of an explosive force rather than a burning, and so you would effectively blow your torch to bits. The highest temeprature for a hydrogen oxygen combustion is about 2,000 degrees Celsius plus or minus several hundred degrees, although the explosive force is much stronger. An oxyacetylene torch can get 3,480, an oxy-MAPP torch can get 2,900, and an oxypetrol torch can also get 2,900 http://www.opetrol.com/ .