Distilling condenser types

[CyclonitePyro]

I've made up my mind, instead of using H2SO4 and KNO3 as a nitration mixture to make certain goodies and getting crappy yields, I'm going to buy or make myself a nice vacuum distillation setup and distill my own HNO3. I plan to distill a mix of H2SO4 and KNO3 and if neccesary distil the product with some H2SO4 so I'll have 98-100% anyhydrous white nitric acid.
Now my question, which type of condenser do I want? Leibig, Allihn, Graham, the Graham looks the best with those cool swirlies, but should I really spent a lot more if a nice Leibig works fine, even if all the vapor doesn't condense, if the reciever is in an ice bath then the vapor will condense there right?

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"Friends don't let friends play with
Nitrogen Triiodide"

[EventHorizon]

I think it all depends on the other glassware you have and connectors. I've used the Graham, Leibig, and Freidricks and like the Graham and Freidricks the best.

I'm interested in what the other members like/worked best in their distillations.

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"Chance favors a prepared mind" - Louis Pasteur
"Happiness is a large pile of links." - Me
PGP ID 0x147CEF54

[Microtek]

Well I've used a simple aluminium tube, no vacuum and gotten excellent ( 70-80% ) yields with distilling a 62%HNO3/96%H2SO4 mix. After a single distillation the product was red fuming and was capable of almost stochiometric yields of HDN to RDX nitration ( after NOx purging ).

[nbk2000]

Since nitric boils at a fairly high temperature, there's no need for the maximum cooling capacity of a grahm condenser.

Either a liebig, or allen bulb will work. I'd use an allen because it has more cooling surface for the same length as compared to a liebig. It's also a straight tube, making it easier to clean.

http://server3001.freeyellow.com/nbk2000/condenser.gif

This shows a coil type made from vinyl tubing wrapped around a wood dowel. You'd want to use teflon tubing ($1/foot) for nitric. You can also use a straight length of glass tubing instead for a liebig type.

Cost for either style is less than $15 and can be disassembled for easy cleaning or hiding.

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"I have begun evil, I shall end evil. That is the end that awaits me."

Go here (http://briefcase.yahoo.com/nbk2k) to download the NBK2000 files and videos.

[10fingers]

Have you checked out www.unitedglasstech.com? (http://www.unitedglasstech.com?) You can get a complete vacuum distillation setup with 24/40 joints for about $135.00.

[EventHorizon]

Very nice company, and fairly cheap. Kimble is another nice one. www.kontes.com (http://www.kontes.com) is their cheaper stuff.

I plan on resumeing my nitric acid endeavours now that it is cooler and I can work in my shed in relative comfort...plus it tends to make my wife a 'little' less mad. http://theforum.virtualave.net/ubb/smilies/wink.gif

I'll even get pics of my coolant circulator which works excellently!

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"Chance favors a prepared mind" - Louis Pasteur
"Happiness is a large pile of links." - Me
PGP ID 0x147CEF54

[CyclonitePyro]

Thanks for the info, this morning before school I used "buy it now on ebay" to buy a complete United Glass Tech distilling setup, with a Leibig condenser. I would have gotten an allihn condenser but there weren't any on ebay with ground glass ends. Here's the URL to see it: http://cgi.ebay.com/aw-cgi/eBayISAPI.dll?ViewItem&item=1653036092&ed=1003833771

on ebay also I just bid on one of 3 submergable water pumps for just 8 dollars: http://cgi.ebay.com/aw-cgi/eBayISAPI.dll?ViewItem&item=1287716550

and I might just buy this vacuum/pressure pump, but I won't have enough money left on my paypal account for it: http://cgi.ebay.com/aw-cgi/eBayISAPI.dll?ViewItem&item=1652287325

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"Friends don't let friends play with
Nitrogen Triiodide"

[Anthony]

I'll have to resume my still construction soon.

CyclonitePyro aka; "sarahgirl4"http://theforum.virtualave.net/ubb/smilies/smile.gif

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"It's important for us to explain to our nation that life is important. It's not only life of babies, but it's life of children living in, you know, the dark dungeons of the Internet." - George W Bush - Arlington Heights, Ill., Oct. 24, 2000

[EventHorizon]

Hahahah, I just checked that too. http://theforum.virtualave.net/ubb/smilies/biggrin.gif

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"Chance favors a prepared mind" - Louis Pasteur
"Happiness is a large pile of links." - Me
PGP ID 0x147CEF54

[PYRO500]

I got one of those 24/40 vac distillation setups a while back, I still got to get a recirculationg spa pump for a friend to power my water aspirator to max vac. I also want to get 2 refrigerant compressors and wash bottles so I can draw a very high vac. that and distill things with very high boiling points.

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"Death may come from above, but terror most certainly comes from below."

[PYRO500]

And another thing,instead of teflon tubing you could use poly propylene tubing avalable at most hardware stores, it is nirtic acid proof as far as I know, and is ridgid enough to withstand a fairly powerful vac.

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"Death may come from above, but terror most certainly comes from below."

[Anthony]

If you mean the translucent tubing (same stuff as used for aquariums) then it is HNO3 proof as you say.

However when I drew some super saturated, very hot NH4NO4 solution through some 3mm bore stuff, it collapsed into a figure of eight (8) cross section and actually welded itself together!

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"It's important for us to explain to our nation that life is important. It's not only life of babies, but it's life of children living in, you know, the dark dungeons of the Internet." - George W Bush - Arlington Heights, Ill., Oct. 24, 2000

[PYRO500]

No, not the stuff that they use for acquariums, this ts a whitish color to it and is used for water supply tubing in homes, I got mine that way, it is the same stuff my aspirator is made of, I beleve the acquarium tubing is viynl, I used a piece of transparent viynl tubing to join the pieces and it got discolored and sticky with a yellow substanceafter just 2 distillations.

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"Death may come from above, but terror most certainly comes from below."

[CyclonitePyro]

No, no I did not think up Sarahgirl4 for my own use, my mom registered on ebay and made up that name for herself but she never bought anything. If I had my own username it would be... you guessed it, CyclonitePyro, but I don't have a credit card to verify myself, and I don't want to lose the # next to Sarahgirl4 which is how much feedback I got, and people are more confident to buy from and sell to me. But it must look wierd having a fem sounding name bidding on labware and all the stuff I've got in the past.

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"Friends don't let friends play with
Nitrogen Triiodide"