How lame, but easy!

[SantasL.Helper]

Ey, i lately discovered the most lamest thing.
My parents where using these little rubber stoppers on wine bottles and this handpump that fitted on the stoppers with which you can vacuumpump wine bottles to preservate it.

Now i'd never really thought of using it, but yesterday i tried them on my setup and these things actually work. They fit perfectly on my 1L 3neck distilling flask so i just use that one as receiver and put such a stopper in and closed the other neck. I mixed 222 ml nitric with 444 ml sulfuric, closed the setup and started pumping it with the wine bottle pump. When i figured i created a nice vacuum, i started heating it to 140/130 degrees celsius, as i also do without vacuum when distilling nitric.

I just regulated my pumping, just everynow and then to compensate for the gasses and heating. I noticed that the nitric acid started to distill WAY faster (lower bp) then normally, so i lowered the temperature of my bath. I've not been so happy in my little science life seeing drop after drop nitric and without a single tint of yellow, not even in the gasses in my setup. Everything was just clear!

When i measured 43 ml of the gained nitric, I found out it had a concentration of about 98%, though i can't fully conclude it was THAT high due to me weighing such a small amount of nitric with a not very precise (1gr) scale. Anyhow, I'm pretty sure the concentration was somewhere up in the 90.

So to everyone with a vacuumless setup, go to the store and get yourself these winebottle stoppers and handpumps. Works like :eek:

Oh, btw can anyone tell me at what gas temperature (thermometer located above the exit of my distilling flask) i should distill the nitric under vacuum and at what temperature i should set my frying pan? thanks

Ps, frying pans work great for (amaturistic) heating!

[hereno]

Check your pump, it will dissolve pretty fast if it isnt made for nitric (which it obviously isnt!). Your mummy wont be pleased.

[tmp]

SantaL.Helper, there are numerous threads on nitric acid production all over this
forum. Personally, I like my hydroaspirator, cost about $9(USD), and does a
great job of providing vacuum as well as washing those noxious fumes down the
drain in the process. I wouldn't risk using my vacuum pump due to the corrosive
nature of HNO3. Look around on this forum. You'll find plenty of information on
making HNO3 with or without vacuum. IIRC, Brainfever had a vacuum-less
method that did a good job.

[SantasL.Helper]

yea but vacuumless synths very often end in a pretty NO2 rich mix. Which yield crappy in producing RDX.

Anyhoo, i don't get how it works... When i distill nitric under vacuum with a gasstemperature of 80 degrees, i get a just as pure nitric acid as when i heat the gas temp up to just 60 degrees celsius. I'd expected a lot of water to be distilled over when i heated till 80 degrees but that didn't happen... Anyone has an explanation?

[Dave Angel]

Certainly this could have been posted in an existing HNO3 topic, but the results are still interesting. If you can make a litre of it Santas, then please do so; as you know, your measurements will be less affected by error.

I'm currently distilling w/o vacuum, (hoping to eventually get very pure HNO3 via the DCM/dry ice method), but these handpumps are not all that expensive and I have a scale accurate to 0.1g, so I'll see what I can do about trying this out myself. Is it 19/26 joints they fit? It looks that way from the wine bottle neck, and I have a suitable three-neck. I can see that large batches might be quite tedious/tiring to produce with a manually operated vacuum though.

I think the reason you don't get water coming over with a vacuum is that the effect of the H2SO4 on water is a chemical one, and you are only altering physical properties by applying a vacuum.

[SantasL.Helper]

yup, they are 19/26 necks the stoppers fit in. I got 100 ml now of (calculated again) 94% nitric i guess. I'd like to create a litre of the stuff, but at my current rate, that will take 20 distillations :p as my bigest flask is a 1000ml one. Bummer...

The stoppers however cost €4 per 2 if not mistaken. The pumps are a bit more expensive (€10) but i guess you can get them a lot cheaper cause the one i saw in the shop looked pretty stylish and shit, we got like an ugly one, gotta be cheaper.

here's a picture of the pump + stoppers (our pump looks exactly the same but is coloured white though, details details... lol):

http://www.winestuff.com/acatalog/W1116full.jpg

[thelasttrueone]

I am thinking of making an apparatus out of a mason jar, a martini glass, a beaker, that pump and a copper valve. Could I have a picture of your apparatus for comparison?

[festergrump]

SantasL.Helper hasn't been back here since June 12th, 2005 08:44 AM.

Always a good idea to pay close attention to when posts were made. This thread is 3 years old and by dredging it back to the top of a section to ask a question of someone who doesn't stop in anymore and not really have anything of value to offer yourself... that's called necromancy (a bannable offense, I'm afraid). :eek:

[thelasttrueone]

Thanks well I'll look out for that in the future (or past?). *goes to read rules again*

[megalomania]

Reigniting an old thread is good, asking questions of the long dead, necromancy, is not good...