Fool Proof Guide to making HNO3

[PYRO500]

Recently I have been messing with adobe acrobat 5 pdf creator and I decided to make my own file on how to make HNO3 and explain all the chemichal's and equipment necessary to create it, this is beacuse I had to scour the web when I first found out what HNO3 could do, maybee it was a good thing I didn't get my hands on any at that time but I beleve there should be a guide that will teach any dumbass how to make HNO3 and thus my first PDF was born, feel free to criticize my work so I can make it more perfect. BTW, I am temporarily putting away my M_gODLIKE powers so you can speek freely of my work. this is the link:
ftp://ewf:halfbaked@209.195.155.80/-=Uploads=-/How to make HNO3 By PYRO500.pdf

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visit my web page at:
[URL=http://www.geocities.com/pyro2000us/]

[nbk2000]

I prefer to think of it as GmODlike powers myself. http://theforum.virtualave.net/ubb/smilies/wink.gif

I did notice that in your zip file of your "lab" that you had the round bottom distilling flask sitting on a bare wire grill.

Not a good idea.

The concentration of heat in the wire could cause stress fractures in the glass from uneven heating.

Rather, get a shallow pan and set the flask in sand for even heating. A cut down coffee can would work fine.

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I've just read your PDF. You used a wire screen to set your flask on. That's OK, but sand is better.

Don't forget to mention that nitric acid liquifies rubber of any sort.

Vacuum is good, but that means you have to always check the glassware before use for any cracks, chips, or stars. Becuase once you draw down, that's where the flask will break, spewing hot acid everywhere. The glassware must be in perfect condition and clean too.

Non-vacuum distillation isn't as dangerous.

You can use a plant pot of sufficent size to make an air bath for the distilling flask. This makes for more rapid heating. Take the clay planter and cut off the very bottom. Enlarge the hole in the cut off bottom to just barely fit around the flask neck. Now cut in two.

Place your flask inside the inverted pot, hook up your shit, then slide the two bottom parts around the flask neck to enclose it.

Preheating your nitrate to 300 degrees F in an oven just before use will remove any water of crystallization it may have absorbed. It also makes it crumble into a nice powder.

Purging with dry-rite filtered air will remove water from the setup too. Not really needed though.

And there's an old saying:

Nothing is sufficiently fool proof that a sufficient fool can't fuck it up.

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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/nbk2ooo) to download the NBK2000 files and videos.

[This message has been edited by nbk2000 (edited 11-25-2001).]

[CyclonitePyro]

I read your PDF, pretty good, but how do you know when you are done distilling, read my post in "What is in Liquid Fire"

And, when I got done, I went to an msds site and read that potassum sulphate is water soluble, so I let the flask cool and then went to a sink and poured water in swished it around, poured in out and kept on doing that until it was all gone. No need to wast precious sulfuric acid getting it out.

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

[PYRO500]

I tried that once and it took a very long time. I don't think the stuff is very soulable in water, or it's slow to disolve.

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visit my web page at:
[URL=http://www.geocities.com/pyro2000us/]

[PYRO500]

I think I will add that sand in pan idea, this is the first I have herd of that idea and it sounds good, where did you learn that from?

I will mention HNO3's incompatibilities with rubber and metal and other things and I just realized that there are 2 kinds of surgical tubing, one is latex, the other is silicone, is the silicone stuff HNO3 proof? I am assuming the latex isn't. I am not sure what you mean by clean NBK, but I am assuming you mean that the still shouldn't have chemichal residues and the glass joints should be clean for good friction fit.

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visit my web page at:
[URL=http://www.geocities.com/pyro2000us/]

[PYRO500]

Recentltly I *borrowed* a spa pump I *found* and I am going to build a recirculating pump aspirator out of an old pool sand filter, the sand I have in the bag will be the heat transfer medium for my HNO3 setup, also I got a really new spa digital control center I will use as a thermostat for an electric heating mantle and a pan with some sand to hold a flask.

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visit my web page at:
[URL=http://www.geocities.com/pyro2000us/]

[rikkitikkitavi]

Only synthetic material (e g plastic) that is resistant to 100 % HNO3 is unfortunately
teflone or similar fluorcarbon polymers.

Glass and aluminium is also resistant to
100% HNO3.
/rickard

[nbk2000]

By "clean" I mean no residues or other crap, which means you can't use the setup for other purposes. All you'd need would be for some organic residue to be present while distilling hot 100% fuming nitric to start a fire or explosion.

You won't have problems with the GG joints sticking since you're distilling acid. But, you can take a small piece of teflon tape, insert the strip between the joints, and then wrap the joint tightly with more teflon tape for an airtight seal. This prevents any joint sticking. Teflon tape used for plumbing is more than adequate.

The "pan o' sand" is an ooollllddddd idea. It's in Dicks encyclopedia, Granddads Chemistry, PMJB.

The gunk in the flask, soak with vinegar. Turns it into soluble acetate. Probably wouldn't hurt to dump it out while it's still hot either, before it cools down and cakes up.

Any decent plastics store will have teflon tubing for about a $1.5/foot.

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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/nbk2ooo) to download the NBK2000 files and videos.

[Ctrl_C]

moved to

ftp://ewf:halfbaked@209.195.155.80/E&W%20Related/Texts/Chem%20Synths/

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Long

Ass

Sig

[This message has been edited by Ctrl_C (edited 11-26-2001).]

[PYRO500]

I use my still for other uses, I just clean out my still after every distillation. I have a 5 gallon bucket that I put the condenser/3 way adapter/ vac. adapter in. I have distilled ethanol (I denatured it of course : ) ) isapropanol, ethylene glycol, and other stuff, I just clean and re wrap the glassware after every use and I don't have any problems, my glasware looks just like when it was new.

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visit my web page at:
[URL=http://www.geocities.com/pyro2000us/]

[rikkitikkitavi]

When I vacuumdistilled HNO3 (68%) with H2SO4 I used a small aquarium pump to circulate the cooling water through the condenser (same setup as in pyro500´s), the cooling water was stored in a bucket with LOTS of ice, hence giving a very efficient cooling.
And also distilling slowly to maximize the yield of HNO3, I managed to get
about 90 % yield , calculated on HNO3.
(adding more ice , ice , ice next time I do it at winter ) The rest was probably gone in the aspirator.
As heating I just used a waterbath. (20C)
I found out that reconcentrating the
diluted H2SO4 under vaccum was very efficient, heated it to about 100 C.. Very little acid was lost.

I found out after a while that the ratio between H2SO4/HNO3 needs to be more than 2 , preferably 3 to give really high HNO3 %.
H2SO4 stops working as a efficient dehydrating agent when it gets below 65 % w/w (rest water).

Anybody having tried to calculate their yield , getting similar with lesser effort?Because it is a pain in the ass to keep adding ice and pyros setup seems more simple.

/rickard

[PYRO500]

I am doing a partial overhaul on my lab at the moment, I am taking an old spa pump/control unit and with a old pool sand filter ((sand removed) I am building a new water aspirator that will be adjustable, I am still working on the HNO3 file and may add how to make a variable vacuum water aspirator setup with a bypass to control backpressure.

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visit my web page at:
[URL=http://www.geocities.com/pyro2000us/]

[rikkitikkitavi]

the easiest way to regulate the pressure in your system is to have a T-connector on the vacuumtube ,between the distillationsetup and the aspirator.
Attach a tube to the T-connector and a clamp on the tube so that by changing how hard the clamp is squezeing the open tube, different amounts of air leaks into the system.

Aspirators can be sensitive to backdraft into the vaccumflask if the waterflow is to low. Preferably you will have one backdraft stopper between. (it is just a flask with one inlet and one outlet)


this trick I learned at the laboratory at my company, but the labrats even use a electronic pressure monitor (not with HNO3).
They also have a central vacuum system
(its a HUGE lab)

And for the solid left in the flask after distilling. If you use a surplus of H2SO4 you have KHSO4. Then you can just heat it until everything melts. (at about 150 C) anyway KHSO4 (NaHSO4) is more soluble than the sulfates. Otherwise use lots of hot water, preferably sprayed into the flask.
sulfates tend to cake very easily since they form different hydrates. So lots of water to break up the cake.

In the good old days when HNO3 was produced solely by H2SO4+ NaNO3 the NaHSO4 was called "niter cake" and used as a rasmaterial for making Na2SO4.

/rickard

[This message has been edited by rikkitikkitavi (edited 12-02-2001).]

[This message has been edited by rikkitikkitavi (edited 12-02-2001).]

[CyclonitePyro]

Ok, that makes sense, I use more sulfuric acid than the reaction equation calls for in moles, if I did it that way I'd be using about 50ml sulfuric acid to 200g KNO3, that would be a very thick sludge.
I was wondering what Pyro500 was talking about when he said it took a long time but that because mine is more soluble than his.
It only takes about 2 minutes to dissolve all of it.

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

[PYRO500]

I do not really need to regulate the vacuum so much as I need to regulate the flow, the pump I have is a very powerful one and has a high flow rate, you can't just keep a huge backpressure on it or they will overheat and break down. I just bough parts to set this pump up,I have gotten a 1/2" ball valve, a "T" connector, a few bulk head fittings and a ton of teflon tape (on sale) I will hook the pump to the tank through the side with the bulkhead fittings, and I will have the "T" sticking out of the top, from the top of the "T" I have a reducer to 1/2" the ball valve will go on that to the bypass pipe witch dumps directly back into the tank, the side of the "T" will go to a reducer and to 5/8" OD tubing witch will go to my water aspirator. I have a big pool sand filter tank I will use and I will possibly put some metal mesh in there so I can cool the water some to get a higher vaccume when I realy need it. I jsut happen to have an old fridge holding animal vaccines cool with nothing in the freezer so I can make blocks of ice with it.

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visit my web page at:
[URL=http://www.geocities.com/pyro2000us/]

[Bitter]

What happened to the ftp ? It doesn't seem to work anymore.

[PYRO500]

I got an email from someone claiming to know Ctrl_C he sent me this email:

Hello, I am friends with ctrl_c from the forum, He told me to email you and ask you to post that his isp cancelled his account and he should be back on the forum in a week or so. I would have posted but since I'm not a member I would have had to wait 15 days or whatever.
Thanks,
Chemsynth

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visit my web page at:
[URL=http://www.geocities.com/pyro2000us/]

[kingspaz]

hhmmm, that seems to clear things up. at least hes not blown his head off or anything. well according to the email. just hope its not a hoax from a kE\/\///\l.

[CyclonitePyro]

I finally got a big enough graduated cyclinder that is deep enough so that I can measure the density of my nitric acid I distilled with a hydrometer. It measured 1.5, so that means my acid it a bit over 97% right?

If I wanted to have a dream identicle to the one on mega's site of PETN, would the concentration of my acid suffice?
It is yellowish, it is really clear but you would call it a yellow liquid, it fumes white and I have urea. Since my acid isn't, 100% would I use a little more acid like 412 ml? How much urea would I add to that much acid since my nitric doesn't have that much nitrogen oxides because it is yellow. Is the bubbling of air through the acid neccessary?

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

[mongo blongo]

Yea that should be ok. I have read that you can use a metal nitrate to make it which means you could save your HNO3 for something else.

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AAARRRRRHHH! My beautiful eyes! It burns!
The goggles do nothing!AAARRRRRHHH!

[CyclonitePyro]

Yea, now that I think about it, I could make PETN (in my dreams) with a fairly decent yeild with H2SO4 and KNO3.
So I geuss I'll dream of RDX with my acid, my name wouldn't be justified if I don't actually dream of cyclonite.
Now, I still need to know if my acid is good enough for RDX, and do I need to add urea to my acid or/and blow air through it.
And should I use a little more nitric acid for megas recipe on RDX because I have 97%(I think) and it calls for 100% ?

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

[Madog555]

hi, the acid has to be 98-100% and 100% NOx free for RDX or the reaction will fuck up. 97% should work but just to be sure it might be a good idea to re-distill it.

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"To live is to suffer, to survive... well thats to find meaning into suffering." -DMX

[This message has been edited by Madog555 (edited 12-13-2001).]