DIY Nitric Acid

[usapyro]

Now this guy knows how to synth his nitric...

 

http://www.youtube.com/watch?v=AXoJYbkOd3s

[madmandotcom]

There isn't anything lazy about spelling it sulfur, it's the correct way. It's the accepted spelling by the International Union of Pure and Applied Chemistry (IUPAC) since 1990. It's also accepted by the Royal Society of Chemistry, so you guys have no wiggle room with your claims of British English.

britian was settled before america so therefor there spelling is correct, you lazy americans are always abbreviating things such as jeep just because you though it was easier to say than GPV-general purpose vechile.

[WSM]

Now this guy knows how to synth his nitric...

 

http://www.youtube.c...h?v=AXoJYbkOd3s

 

It's obviously not his first effort; did you notice the scorched earth on the spot he's working on?!!

 

Wow!!!

 

WSM

[anapogeetoofar]

Wow, this thread went straight to hell. Just one step away from a "U.S vs the "rest of the world"" flame war. A classic, and completely stupid internet argument. And, funnily, one that NEVER seems to come up in person. The internet seems to compel people to be rude and obnoxious.

 

 

Oldguy; using sulfuric and a nitrate salt, I made quite large batches of very nice nitrocellulose by letting the mixture sit over night. You could try a small batch using that method, but even them it will not be terribly safe or economical, hots spots will be a major problem. Is there any particular reason you need MCNC? I got very finely powdered NC by dissolving smokeless powder in acetone and then crashing into cool water, you get something that resembles solidified egg drop soup which can then be broken up and carefully crushed into a powder or tiny flakes which press very nicely. Could that work?

[dagabu]

britian was settled before america so therefor there spelling is correct, you lazy americans are always abbreviating things such as jeep just because you though it was easier to say than GPV-general purpose vechile.

 

Brittan lost the war to a bunch of Patriots using hunting rifles to kill the invading Red Coated Hoard from England. Apparently, we won the war and are still rather scrappy.

 

Thank you for making the above foolish and misinformed statement, My grandfather was the first person to ever drive the first JEEP made by Minneapolis Moline.

 

Several companies claim credit for inventing the Jeep, especially the American Bantam Car Co. of Butler, Pa., which claims it introduced a jeep in February 1940.

 

However, Minneapolis-Moline Power Implement Co. maintains it invented the Jeep at Camp Ripley, Minn., in 1938, while developing the Minneapolis-Moline Model UDLX Comfortractor.

 

A 1944 booklet entitled A Wartime Report: Food, too, Fights for Freedom, carries a section called 'The Original jeep is a Product of Minneapolis-Moline.'

 

'Current national publicity has obscured the fact that the first war machine named 'JEEP' was born at Minneapolis-Moline and christened at Camp Ripley, Minn.,' the pamphlet reads.

 

'Back in 1938, Minneapolis-Moline engineers were already experimenting with the conversion of a farm tractor to an artillery prime mover. And in 1940, collaborating with Adjutant Gen. E. Al Walsh, commander of the Minnesota National Guard, models were tested in maneuvers at Camp Ripley.

 

'This new Minneapolis-Moline army vehicle wasn't yet a crawler tractor, truck, nor tank, and yet it could do almost anything and it knew all the answers. Because of this, it brought to mind the Popeye cartoon figure called 'Jeep' which was neither fowl nor beast, but knew all the answers and could do most anything. The National Guardsmen therefore named the Minneapolis-Moline vehicle the 'Jeep.' The 'Jeep' name, there fore, isn't a contraction of the term General Purpose (GP).

 

'Since the original Minneapolis-Moline Jeep, Minneapolis-Moline has designed several additional models of military tractors in cooperation with Army and Navy officials. Several models of Minneapolis-Moline Jeeps are now being produced in quantity for the Armed Forces of the United States, and in use throughout the world.'

 

Sgt. James T. O'Brien is credited with first naming the machine 'Jeep.'

 

I may be lazy, but you are still a pain in the ass and a fool of epic proportions.

 

-dag

[Mumbles]

britian was settled before america so therefor there spelling is correct, you lazy americans are always abbreviating things such as jeep just because you though it was easier to say than GPV-general purpose vechile.

 

Seriously? You saying anything regarding correct spelling makes me keel over with laughter

 

I have no idea why you continue to argue things that are so easily disputed. Did you even bother to look it up? Even Wikipedia says that Sulfur is correct. I guess you are mildly correct because even the Royal Society of Chemistry (a British organization) changed their official spelling to s-u-l-f-u-r. Anyway, if you really want to argue, the word sulfur (spelled as is) is actually Latin for brimstone, which was known and used well before English was created. Perhaps the British should stop making words overly complicated

 

Let's play a game. Every time you post something blatantly false or idiotic, you're banned for 2 weeks.

 

There will be some serious trimming in the coming days, perhaps movement and or lockage. I'm still trying to decide what to do. I was just trying to tease Ralph a little bit, but this got significantly out of control.

[stckmndn]

He doesn't stand a chance.

 

 

[usapyro]

It's obviously not his first effort; did you notice the scorched earth on the spot he's working on?!!

 

Wow!!!

 

WSM

 

Sorry to disappoint but I think he usually has a big charcoal furnace setup in that location.

[asilentbob]

I feel like an old fart.

 

Nitric acid distillation has been discussed to death on most every pyro forum.

Most every chemistry forum.

(HINT: Sciencemadness alone could probably fill a 100+pg thread with nothing but nitric acid preparation related posts pulled from its various threads. A few hours of searching is all it takes and you will learn so much more than you will ever learn in a single thread like this. Someone could probably compile and print a veritable novel from their discussion alone.)

In many chemistry books.

In many explosive related chemistry books.

Newsgroups like Rec.pyrotechnics, alt.engr.explosives, sci.chem, etc...

(which google has archived MANY MANY YEARS back)

Patents. Patents. Patents.

Pyroguide, and similar pyrotechnic and chemistry related wikis.

Many personal pyro and chemistry sites.

Wikipedia's Nitric acid page even has a laboratory preparation section.

Youtube and other video sites.

And even less reputable sources like the ACB have a hard time messing it up too badly.

 

 

1) So you go to wikipedia and youtube and get some info on how to set up a proper distillation apparatus or how jerry rig something up.

2) You go to wikipedia's nitric acid, sulfuric acid, and nitrogen oxide pages and read them well for hazard info and chemical/physical properties. If your wise you read several first hand experiences from various mentioned sources and get a good "feel" for what to expect. You can probably even find some really professional nitric acid distillation videos on youtube.

3) You set up and distill.

4) Your done. You store it in a good container, at a good temperature and in a good place.

(You already do this with pyro chemicals. I hope.)

5) Easy. Now you apply this mentality any time you need to synth something else.

 

I'd say move this thread to the HE section where it will die. For it to be suppressing information... there would need to be a lack of information out there, which is not in any way whatsoever the case.

[Ralph]

I was just trying to tease Ralph a little bit, but this got significantly out of control.

 

Mumbles and I and a few other guys have a bit of fun every now and again, When I make a goke at the expense of "you Americans" I mean no malice just as they don't when gokeing about my spelling/ grammer and general inability to shut up

[dagabu]

Man, I have been gokeing on my breakfast burrito now for the last two minutes since you posted that, Ralph!

 

Aussies, geez....

 

-dag

[SolarSeeker]

WTH ! Where did the conversation slip away from the post topic ?

 

So I'll just answer several questions I noticed while reading through the thread.

 

#1 the initial post's recipe is very viable for 60% and lower concentration nitric. (laser Steve's recipe)

#2 nitric need not be more than $100/gallon within the US http://www.dudadiesel.com/all_chemicals.php

#3 battery acid can be boiled down into 90% sulfuric acid if you work out of doors with glass equipment because sulfuric acid boils at 3 times the temperature of water.

You'll know when the acid gets to the desired concentration because it will have much smaller bubbles and the steam switches from water vapor (no smell) to sulfuric acid vapor which is quite toxic and very acrid.

#4 Note that #3 is the dangerous and expensive method especially considering that drain cleaner (the kind in the plastic bagged bottles) is 90+% and is only $22 a gallon at most US hardware stores. This price is less than 1/3 that of battery acid.

#5 For nitration purposes straight sulfuric acid mixed with a powdered nitrate (preferably ammonium nitrate) will usually suffice.

#6 Do not use the nitrate/HCl/ copper (poor man's aqua regia) gas chamber method. It doesn't produce any usable concentrations of nitric acid but it does make a lot of toxic NO2 gas.

[r1dermon]

WTH ! Where did the conversation slip away from the post topic ?

 

So I'll just answer several questions I noticed while reading through the thread.

 

#1 the initial post's recipe is very viable for 60% and lower concentration nitric. (laser Steve's recipe)

#2 nitric need not be more than $100/gallon within the US http://www.dudadiese...l_chemicals.php

#3 battery acid can be boiled down into 90% sulfuric acid if you work out of doors with glass equipment because sulfuric acid boils at 3 times the temperature of water.

You'll know when the acid gets to the desired concentration because it will have much smaller bubbles and the steam switches from water vapor (no smell) to sulfuric acid vapor which is quite toxic and very acrid.

#4 Note that #3 is the dangerous and expensive method especially considering that drain cleaner (the kind in the plastic bagged bottles) is 90+% and is only $22 a gallon at most US hardware stores. This price is less than 1/3 that of battery acid.

#5 For nitration purposes straight sulfuric acid mixed with a powdered nitrate (preferably ammonium nitrate) will usually suffice.

#6 Do not use the nitrate/HCl/ copper (poor man's aqua regia) gas chamber method. It doesn't produce any usable concentrations of nitric acid but it does make a lot of toxic NO2 gas.

 

the nitric acid on that website is more expensive per mL and less concentrated than the nitric acid from chemical supermarket, and by a fairly large margin. reagent grade "fuming" nitric acid is very hard and costly to produce, which is why it is expensive. it is delivered with a lot analysis outlining dissolved impurities in ppt and ppb levels and are ultra low in those levels as well as detailed in content. technical grade chemicals are suitable for generic synthesis, however, if you're looking for a lab reagent an ultra pure "GR" grade is what you're looking for, and will cost many times the price.

[jimbo]

does anyone know what I can use for boiling chips while distilling nitric acid from nitrate salts,I've been reading up on the subject but can't find a definetive answer,I've read glass beads for jewellery making are used for distillations and should be acid resistant I don't have any broken boro-silicate but have read that broken glass from car windows works,any thoughts. cheers

[Mumbles]

Are you planning to do an atmospheric pressure distillation, or one under vacuum? Honestly, a stir bar has treated me well 95% of the time to prevent bumping.

[jimbo]

I was planning on doing it under vacuum,I've got one of those humbolt aspirators so whatever vacuum those pull if anyones used one. I don't have a magnetic stir bar set up it's too risky to get lab supplies or do you mean just using a stir bar as an anti bumping media Edited July 27, 2011 by jimbo

[Mumbles]

No, I meant a real magnetic stir bar that is stirring. I guess it could be mechanical too, but the typical sealants/lubricants are going to be attacked by nitric acid. The issue here is that several anti-bumping aids like porcelain chips do not work under vacuum. Broken glass is just a ghetto form of boiling chips, and will likely behave similarly. You could try a capillary tube I suppose.

[oldguy]

[oldmanbeefjerky]

I soon plan on making lead and copper nitrate, and at the moment, the Nitrate/HCl/copper method seems to be the only reasonable one in terms of money, though ill be directly nitrating the lead which will be inside the peroxide solution where the nitrogen dioxide will be bubbling through.

I cant buy sulfuric acid, i cant buy nitric acid from anywhere other than a national Australian lab chemical inventory stockist(which by chance is a 45 minute bike ride away form my house), but, the only way i can make sulfuric acid is by electrolysis of copper sulfate, but now ive realised that it only takes maybe 100ml of 100% sulfuric acid to make 1kg of copper sulfate, so sulfuric acid from there is pointless.

 

 

I just wanted to ask, which one of leads oxides (PbO, PbO2 or Pb3O4), is most reactive with nitric acid or is lead the most reactive and most likely to react with the acid the fastest?

Once i have a lead dioxide electrode, which i can use to make sulfuric acid to make nitric acid, i can promise i wont ever try this method again, since its so wasteful, but being in australia, i dont really have acces to cheap, or even reasonably priced sulfuric acid for what its worth, so im not exactly left with allot of choices here.

[Mumbles]

The nitrate salt/HCl method of dissolving copper and/or lead doesn't make the nitrates, it makes the chlorides or probably more specifically the tetrachloro complex ions.

[oldmanbeefjerky]

oh no, i meant i was going to put a chilled lead/ peroxide mush in the secind flask in which the nitrogen dioxide was bubbling, rather than make the acid, then put lead into it.

My aim is to just filter out the remaining solids, such as left over lead or lead chloride, so im left with the itrate which i can boil down.

[jimbo]

oldman,sulphuric acid's pretty easy to get where I'm from but it's $40 a litre,lead nitrate is also available pretty easily if you need it pure,I found a 98%clear sulphuric acid drain cleaner manufactured in nsw called maximum power,I also have mo-flo drain cleaner which is about 96% but its dark amber colour but still works good,mitre10 stocks mo-flo where I'm from just ring up your closest one.

mumbles how would you go about a capillary tube in a distilation set up,could you modify a thermometer pocket with a glass tube that bleeds a gas into the reaction vessel,because I only have a single neck rbf.

[Ralph]

oldman,sulphuric acid's pretty easy to get where I'm from but it's $40 a litre,lead nitrate is also available pretty easily if you need it pure,I found a 98%clear sulphuric acid drain cleaner manufactured in nsw called maximum power,I also have mo-flo drain cleaner which is about 96% but its dark amber colour but still works good,mitre10 stocks mo-flo where I'm from just ring up your closest one.

mumbles how would you go about a capillary tube in a distilation set up,could you modify a thermometer pocket with a glass tube that bleeds a gas into the reaction vessel,because I only have a single neck rbf.

 

Jimbo I wouldn't help this skid mark with any useful info, ive killed more inteligeant things with my foot and an old dog is more open to learning how to do pyro safety

[oldmanbeefjerky]

Thanks, but i just discovered that i CAN buy nitric acid, and 70% lab grade too, at a reasonable price. thanks for your help though.

i am though rather surprised that mitre 10 would stock something as hazardous as that, but then again ive not been to a mitre 10 shop in over 2 years, and the last time i was there, it wasn't because my dad said i could buy some sulfuric acid.

 

 

ill have a look next time im at bunnings, the nearest mite 10 is 80km from where i live

[Mumbles]

oh no, i meant i was going to put a chilled lead/ peroxide mush in the secind flask in which the nitrogen dioxide was bubbling, rather than make the acid, then put lead into it.

My aim is to just filter out the remaining solids, such as left over lead or lead chloride, so im left with the itrate which i can boil down.

 

I'm a little confused as to what you're doing. Are you really going to try to attempt that ghetto NurdRage POS prep of nitric acid to make lead nitrate? Good luck with that.

 

 

Jimbo I wouldn't help this skid mark with any useful info, ive killed more inteligeant things with my foot and an old dog is more open to learning how to do pyro safety

 

I may not be leading by example lately, but be nice Ralph. You don't have the clout here to get away with saying stuff like that. It also doesn't really make a big point trying to insult his intelligence while spelling intelligent incorrectly and using next to no punctuation. An insult from a 3rd grader may still be an insult, but it doesn't really cut that deep.