HNO3 your way

[crazyboy25]

well the best and cheapest place i found that will ship to individuas (not companies) is this place http://www.artchemicals.com/Nitric-Acid-70...2-P371C528.aspx

 

if you have a place that will ship 70% nitric acid to personal addresses cheaper than that i would love to hear it

[FrankRizzo]

Keep in mine that *truck freight* charges apply to nitric acid orders from ArtChemicals.

[weknowpyro]

Tried concentrating 68% HNO3 to 100%, using sulphuric acid. So I added 30ml 91% H2SO4 to 15ml HNO3. I then used the brainfever set up as shown before.

I applied heat for about 3 hours keeping them temp at about 50 degrees centigrade. I then removed the reaction vessels and then observed my yield was around about 5.8ml.

 

I knew from previous knowledge that density of 100% HNO3 is about 1.58gcm3. So I weighed the nitric I had extracted and then worked out the density using: mass/volume.

 

- 6.2g/5.8cm3 ---------------> 1.068gcm3?!!

 

That worried me; 1.068gcm3 is about 40% HNO3 which doesn't make sense to me as I was using 68% HNO3 with a density of around about 1.37gcm3.

So, this would mean that I have condensed and collected HNO3 which is less concentrated than before.

Anyone have a guess at what might have happened?

[hst45]

I knew from previous knowledge that density of 100% HNO3 is about 1.58gcm3.

Not to quibble, but I think it is 1.51 gm/cm3. I've produced small quantities of HNO3 at 1.39 gm/cm3 using Brainfevers method, distilled over a VERY long time, as in a whole afternoon. The yield was pretty crappy for the amount of KNO3/H2SO4 used, but I thought that the concentration was pretty good for such a ghetto-easy method. (pickle jar/ shower curtain)

 

I've never tried to concentrate my 70% HNO3 for just this reason; that I thought I might yield LESS than I started with. Not really confident with the process, and I didn't want to piss-away 100 ml.store-bought 70% to yield 45 ml. of home-made-less-than-70%, so I'm sorry, but I don't know the problem.

[John Hinckley]

Would Teflon tape work?

 

It's found in the plumbing section of the hardware store and is used as a sealant for threaded pipe. It comes in a small roll like tape.

 

For threaded pipe, you wrap it around the threads of your pipe in a clockwise motion then screw the pipe into the threaded fitting and the Teflon will fill any gaps and seal the pipe. Maybe it'll work the same in your application? Don't know.

Tephlon tape works great if you use a few layers. I don't trust the plastic screw in piece (for the thermometer) on my 3-way adapter, so I cover it in tephlon tape.

 

Works like a charm.

[Picric acid DOES taste bitter!]

Well, my first comment in this forum . Finally a place to discuss theories and experiments with the equal-minded...without intervention from pesky security-facist admins .

 

Anyway... I use the boiled battery-acid and NaNO3 with a hot water bath to produce the (H)NO(3)2 an usually put my nitratable compound directly into this mix. Hardly yields pure compounds, but i dont make any larger ammounts anyway.

 

Tips for how to extract the HNO3 without complex equipment?

[TheSidewinder]

As long as you obey the rules here and act in a mature, adult, manner you'll never have to worry about "security-fascist Admins".

 

TheSidewinder

[Arthur]

I plan to make a significant quantity of strong Nitric acid. I have sulphuric acid and can evaporate it to 98%. I have potasium nitrate in sufficient quantity. I can easily get good quickfit glassware.

 

Do I need a vacuum pump to distil under reduced pressure? Can I use the tap mounted one -What is it called? Is there a market sector that uses these and supplies tham cheaper than the four figures of pounds I have been finding for real vacuum pumps that would produce too much vacuum anyway?

 

Is there a chart available of %HNO3 vs SG so that I can check what I produce?

[tentacles]

Anyway... I use the boiled battery-acid and NaNO3 with a hot water bath to produce the (H)NO(3)2 an usually put my nitratable compound directly into this mix. Hardly yields pure compounds, but i dont make any larger ammounts anyway.

 

Use a cold water bath; the reaction between the salt and the acid will be exothermic enough as it is! Unless all you want is a huge red cloud of NO2.

 

What you want for the vacuum supply is called a vacuum aspirator. They are generally faucet mounted and should feature a check valve to prevent suck-back if the water pressure drops. I think I got my from Best Science and Surplus or something. It was like $15 - see a few pages back in this thread.

 

I suggest using a 50/50 mix of calcium nitrate and sodium or potassium nitrate. The calcium nitrate will get you a significantly higher yield from the same quantity of H2SO4, and the Na/K nitrate will help prevent too much caking in your glassware.

 

My last run of HNO3 came out at like 1.51 SG, pretty strong stuff. It was probably at like 7-15C though. I only made up a little over 100ml as I'm not making any more lead nitrate right now. I ran out of Ca(NO3)2 so it costs me more in sulphuric acid until I can get more.

 

http://www.efma.org/publications/NitricAcid/Section15.asp

[Picric acid DOES taste bitter!]

Well, i dont concentrate all the way down to 98% to risk boiling the sulphuric instead. Did that once in my youth and it quick-cleaned the citchen-fan . quite nasty fumes if you know what i mean.

 

I also have had a problem with the battery acid not reacting to the nitrate, even if i boiled the heck out of it. It varies from individual batteries (i nick the acid from a recycling container), so i figured it is some kind of replacement for the sulphuric. Also, this crappy acid leaves white crystals in my pyrex when i concentrate it (i can tell when the sulphuric starts to evapourate, and its only when the water is boiling off). Doesent really belong here, but does anyone have a clue to what that could be?

[Arthur]

Acid from failed batteries will likely be so impure and weak that it may not concentrate to 98%

[Mumbles]

I agree, rather off topic, but the crystals are probably lead sulfate, or some lead salt at the very least.

 

I should probably clarify something here. When people say they concentrate battery acid, they usually don't mean they crack open batteries and boil that. It's wasteful, impure, and by the time the batteries are laid out where they can be tapped they are more or less useless. All the "sulfuric-ness" is tied up in the badly corroded lead sulfate on the plates. Concentrations well below 5% free acid would not suprise me in the least. When they say they boil down battery acid, they get replacement battery acid from an autoparts store. This comes at ~30%, and is actually relatively pure.

[Picric acid DOES taste bitter!]

Thanks, i figured that was whats happened. I do charge the batteries before pouring the acid out to extract the sulphur-part from the sulphide, but it doesent always work. Also, thanks for the replacment-acid tip.

 

Well, back to topic.

 

Any idea on how to easily extract the HNO3 in a cheap and simple way? Got a bit of an economic problem right now besides the lack of proper equipment... it sucks that the nearest large town is 55 km away...

[asilentbob]

Many viable ways have been proposed in this thread... DCM extraction, ghetto double beaker still, etc... You did read it didn't you?

[Arthur]

Having found a UK licensed factory at which to rent a hut, I rang some gen suppliers and can get most things delivered to there.

 

There is a HUGE advantage in having a factory or a club membership at a manufacturers.

[superman1451]

What would the best lubricant for the joints?

[Mumbles]

Probably teflon sleeves or rings. I've heard accounts of it dissolving and oxidizing most petroleum and silicone based greases, and even one about it reacting with the other stuff in teflon grease. I believe it is also a silicone base.

[tentacles]

I've been using a very small amount of silicone grease on my joints. Haven't had any problems or even discoloration, but I do wipe it clean with ethanol after a run. I just make sure it's all in the joint surfaces and not globbed inside the apparatus. I buy my grease as dielelectric grease because it's cheap and easy to get. Edited August 14, 2008 by tentacles

[Mumbles]

I've never seen the 20/4 notation before. I would think that it would be one or the other. 20C is normally room temp, and 4C is when water is the most dense. It is when it has a perfect density of 1.000. Either would make sense, but not both.

 

Any idea where the image came from, source-wise? There may be additional information on the accompanying pages.

[al93535]

I just thought I would add pictures of my latest distillation. I have here 125 mls of 98% to 99% of white fuming nitric acid. I need to do a density test, which I will do soon enough. It is so clear, I just like to look at it. I have another 450 mls to distill the second time. But I wanted to share my pics with you guys, here they are...

[superman1451]

What type of bottle is that?

[al93535]

Its a pyrex glass reagent bottle with ground glass mouth and stopper.

[Mumbles]

Are you using a vacuum distillation? Thats the only way I was ever able to get white acid like that. It seemed like if I ever got it over 40 or 45 degrees, it would turn slightly yellow.

[al93535]

Nope, its at atmospheric pressure. I am also using brainfevers method, and on a coffee hot plate.

 

I will get pics the next time I do a run. I am however getting an entire set of glassware here really quick.

[Swede]

Nice - that looks exceptionally clean.