# making nitric acid



## Anonymous (May 10, 2008)

hi guys i have run out of nitric i dont use very much nitric but i need some to finish a small batch of gold i been working on for several yrs. i have found some fert. its anylsis is 49-o-o nitrogen will this make nitric and if so how do i do it . any info. would be appreciated thanks J Cook


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## Platdigger (May 10, 2008)

Would that be "ammonium nitrate"?
Randy


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## Anonymous (May 10, 2008)

all it said is nitrogen


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## Irons (May 10, 2008)

That sounds like the Nitrogen content of Urea.


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## Anonymous (May 10, 2008)

will it work to make nitric if it is urea or does it have to be nitrate


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## Platdigger (May 10, 2008)

This could be interesting..........I would like to know also.....hmmmmm

Irons?


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## lazersteve (May 10, 2008)

You will need to have a nitrate to make nitric acid, or a source of NOx.

Sodium Nitrate is what you want (16-0-0), but there are other nitrates that will work also.

Steve


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## Scott2357 (May 10, 2008)

If anyone is interested (and it's allowed in the forum), I have a recipe for making potassium nitrate from organic rich soil. Which then can be used with concentrated sulfuric acid to produce nitric acid in equal volume to the KNO3 used.

Now that I think about it, is there a place here with guidlines of what is *NOT to be posted* on the forum?


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## Noxx (May 11, 2008)

I don't think there would be any problems concerning posting your technique. Unless it contains offensive language...


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## Shaul (May 11, 2008)

Also, try not to post formulas for explosives (there are other forums that deal with that kind of stuff).

Granted, there are certain chemical reactions that may end up being explosive, but they don't have to be listed as such.

Shaul


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## Harold_V (May 11, 2008)

Shaul said:


> Also, try not to post formulas for explosives (there are other forums that deal with that kind of stuff).
> 
> Granted, there are certain chemical reactions that may end up being explosive, but they don't have to be listed as such.
> 
> Shaul



I think that in such an instance, a cautionary note should be provided. Many of the readers (myself included) do not have a working knowledge of chemistry----and may not understand the ramifications of following a procedure that has the potential to be dangerous. Such a notice could well save a person from tragedy. 

What might be important is to not dwell on the hazard---but on the value of the given process. I fully agree-----this forum should not be the source of information for those intent on making explosives. 

Harold


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## Anonymous (May 22, 2008)

Ok guys I have located some sodium nitrate now I need to know how to make nitric. I have been using nitric for 25 yrs. or more A couple chemists taught me how to use it saftely and also sold it to me. I lost cont. with them . and dont have a source any more. also I dont use aqua regia either too dangerous for me . Also I have a source for furnaces and fluxes practicly anything but acids . I would be glad to swap info. with yall thanks a lot Jcook 13


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## lazersteve (May 22, 2008)

J,

The recipe is in guided tour link in my signature line. 

Here's link also:

Nitirc Acid Recipe

The link above points to a recipe which allows you to use the cheaper calcium nitrate to recycle your sodium nitrate. If you are using sodium nitrate just follow the first part of the reaction.

Steve


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## Anonymous (May 23, 2008)

I have been giving this info away for free on ebay for years

1 cup sodium nitrate to 1 quart sulfuric acid. Pre-dissolve the nitrate into 16 ounces of hot distilled water and then add it to your sulfuric acid. Once mixed, you have nitric acid that can be used as is or distilled to 70% nitric

Dr Charles
phd in chemistry


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## The Refiner49er (May 23, 2008)

DR-

Does your formula require concentrated sulphuric acid?

I have been making nitric for awhile now using concentrated sulphuric acid and a saturated solution of sodium nitrate and water. Since I use a fair amount of this acid, my recipe for volume is 2000 ml of distilled water, 3.4 kilograms of sodium nitrate, and 1120 ml of 98% sulphuric acid. Heat the water to boiling to dissolve all the sodium nitrate. Dump the solution into a clean 5 gallon bucket, let it cool just a little. Use a large stirring paddle. YOU HAVE TO PUT THE FIRST 50 TO 100 ML OF SULPHURIC ACID IN A LITTLE BIT AT A TIME!! Otherwise the stuff will boil over. Stir constantly! If it foams a lot, spray it down with a spray bottle with cold water. Once you have some of the sulphuric in, it settles down and you can pour the rest in slowly, stirring constantly. This process outgases, so be outside or ventilation! I let the solution cool in the bucket, most of the salts drop out. Then I pour the solution into beakers or glass coffee pots, and put into the freezer overnight. Then pour into containers while cold, but not the salt.

I am considering taking nitric production to the next level. The nitric produced by a saturated solution of sodium nitrate and concentrated sulphuric acid produces a theoretical 50% nitric acid. The problem I see after using this acid is there are still substantial salts in the solution, and the performance of this grade of acid is not adequate for some processes. The fix for this is purifying the nitric acid/salts is through distillation, leaving the salts behind in the evaporation flask. I don’t currently have a condenser, but would like to get set up to make full strength material. 

I welcome your advice on an effective procedure/equipment for distillation of nitric acid. I have a fume hood and a water chiller to operate a condenser.

Thank you!

John


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## Noxx (May 23, 2008)

John,
You could filter your nitric acid using a medium speed filter to get rid of the salts...


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## lazersteve (May 23, 2008)

John,

How cold is the freezer getting? 

The lower the temperature the more salts that you will get out. I recommend -5C in the recipe, but colder would be better. 


Steve


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## The Refiner49er (May 23, 2008)

Hi Steve!

I leave the solution in the freezer overnight, it is about -15 C.

I am happy with the way the nitric works for digesting base metals, usually adding a balance of water to improve the efficiency of the reaction (less brown gas). I heat it up to kick off the reaction.

I am starting to refine placer material, the bulk of what I'll be processing is from one particular client, it is around 920 with just a trace of silver. I would like to run this material in a "true AR", for I understand the dissolution power using 70% nitric is unmatched. If this isn't true, or the advantages of 70% does not justify the distillation, then I would like to know.

Tech grade nitric is expensive compared to homemade, difficult to obtain, and only reasonable in cost if you purchase a 55 gallon drum. A significant cash outlay! Not to mention the flags that go up, inviting attention from a multipicity of regulatory agencies.

Also, anybody out there have a good process for placer gold with black sands, I welcome your comments!

Thanks, guys, for your input!

John


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## crazyboy (Jun 8, 2008)

Noxx said:


> John,
> You could filter your nitric acid using a medium speed filter to get rid of the salts...



What concentration are we talking? 70% will begin to eat away at filter paper fairly fast.


To make real quality nitric acid you need a glass distillation setup with a condenser and a hotplate and even an aspirator/vacuum pump. 

Once you got that the rest is easy.


Check here for more info
http://www.sciencemadness.org/talk/viewthread.php?tid=2176


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## istari9 (Jun 8, 2008)

I have just today come across a guy i.e. refiner who uses only AR. Now this guy has told me where he get Nitric for say aprox $100.00 for five gallons. I do hope to see this supplier on Thursday. I will let you know send me a list of chemicals you may need and I will ask...


Ray


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## Lou (Jun 8, 2008)

It had better be really good for that price!

It's still not even cheap at 20 a gallon!

Nitric should cost $5-6 if purchased from Brenntag or Univar. 

It costs me about $20/gal if I get NaNO3 from the garden shop for $1.50 a pound and distill it with sulfuric. I can get a gallon of 95% sulfuric for $14.


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## The Refiner49er (Jun 8, 2008)

Hey Lou!

I would like to get set up to buy nitric acid from one of the major chemical companies. Univar is right across the river from me.

How do you get set up with them to purchase? I have gotten the runaround when inquiring the purchase of it.

"Homeland Security" and such.... I am not a terrorist!!!!

Thanks!

John


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## Lou (Jun 9, 2008)

A business license and perhaps 20 minutes talking to their account or sales manager about what you are doing with it. Don't forget the usual cordialities.


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## OMG (Jun 23, 2008)

I read that ammonia and ozone makes ammonium nitrate (and water and oxygen). 2NH3 + 4O3 -> NH4NO3 + 4O2 + H2O
so,
would ammonia and peroxide accomplish the same thing (except making more water instead of oxygen?)
or thinking further ahead...
Ammonia and caro's acid as a route to nitric (and ammonium sulfate)?


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## Lou (Jun 23, 2008)

Ozone is a ridiculously strong oxidiser. Hydrogen peroxide is made by adding ozone to water  per

O3 + H2O --> H2O2 + O2

That said, I doubt adding H2O2 to ammonia would work at all, at least in the concentrations any of us can get. I think it is more likely that we can make HNO3 from oxidation of ammonia over platinum wire or perhaps by coronal discharge to make NOx which is then bubbled into water.

Lou


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## lazersteve (Jun 23, 2008)

Lou,

I once tried making nitric using coronal discharge and it is very difficult to do. 

I used an air pump to pass the air over the Jacobs ladder and in fact it did form NOx. The discharge was then passed into distilled water. 

The problem was that the quantity of NOx formed was so little that it would take forever to make any appreciable quantity of HNO3 at a decent concentration. Perhaps if I had tried different spark gap arrangements I may have been able to make enough NOx to make it work. It may have been that more O2 was required as air is only about 20% O2.

Steve


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## Lou (Jun 23, 2008)

There have been several well-documented instances of it working. I don't have the links ready, but a simple search at sciencemadness will show some threads where people have made it in the 50mL+ range.


I think I could have a crack at the Ostwald Process, as I have 90Pt10Rh wire in abundance. I can also dig up the stainless needed to try this at 700C and 65psi. Is it worth doing though? No, it isn't...I'd rather distill it from an alkali nitrate or just buy it!


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## eagle2 (Jun 25, 2008)

Ray.

Harcross chemical is in Kansas City. I got a 30 gal drum from them 15 yrs ago. It was a few dollars a gallon, but the drum deposit is very high. 

You will need a business letterhead and some communication.

Al


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## istari9 (Jun 25, 2008)

No problem I have several business names and Lic frm Mo. 
I am in my time off so its off to research I go. 

I will keep you all posted and I can dicker with the best of them. 
Ray


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## eagle2 (Jun 25, 2008)

Small correction, its: Harcros chemical. 

You know I think we live about a hundred miles from each other. :!: 

Al


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## OMG (Jul 29, 2008)

How about making nitric as well as sulfuric from ammonium sulfate and ozone?
here's a diagram of what I would like to try.


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## OMG (Jul 29, 2008)

Anyone see issues with a set up like that? I might need to put something in there to circulate the ammonia and ozone.

And Lou, you said you had some Pt wire, would you want to sell me some?


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## lazersteve (Jul 29, 2008)

OMG,

Here's an article on ammonium sulfate decomposition by the US Atomic Energy Commission that may help you along:

Decomposing Ammonium Sulfate

Steve


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## OMG (Jul 29, 2008)

Thanks Steve, that method would allow a lower temperature, at the expense of the sulfuric acid.
I think if I can melt the ammonium sulfate and keep it at a temperature below H2SO4's boiling point, it should be okay. I might need to have some H2SO4 (not 98%) in there at the start to help absorb the H2SO4 that is being made.
If the temperature was between 280 and 290 C it should work.

I found something interesting about TiO2 as well, under UV light it will oxidize NOx's to nitrates, so maybe I could incorporate this into the design as well to keep the levels of NOx's low.
http://en.wikipedia.org/wiki/Noxer_block


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## viacin (Oct 26, 2008)

a slightly old post, but if anyone is interested in buying nitric in bulk from univar, it can be done online if you have a business.
http://www.univarusa.com/vwr-inc/partnerregistration.nsf/customer?openform

If you tell them you are making biofuels, they are less curious on the phone too.


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## Noxx (Oct 26, 2008)

Do you have an idea if they ship to Canada ?


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## viacin (Oct 26, 2008)

I'm not sure, but their headquarters is in Vancouver, here is their canadian website:
http://www.univarcanada.com/

And here is their distribution sites and contact info:
http://www.univarcanada.com/distribution.htm

Unfortunantly, I cannot find online ordering in canada? Seems odd. It was kinda buried on the USA site. They have Electronic Data Interchange (I supposed this would be online ordering) But you must call to set it up.


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## EVO-AU (Nov 4, 2008)

Dr. Charles: I just received a shipment of 70% ACS nitric acid. Can I use it as is or should I dilute it down. It will be used in A/R. Evo-au


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## Lou (Nov 4, 2008)

I don't know who Dr. Charles is, but you would be better served by diluting your nitric acid by half. So in 1 liter of solution you have 500mL of 70% nitric with 500mL of distilled water.


Lou


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## viacin (Nov 4, 2008)

"Dr Charles" Is a peddler on ebay of gold refining chemicals and whatnot. His "free" advice that he uses to push his products leaves you with more questions than answers. He provides small tidbits of facts with no "how-to" about it at all, without any warnings of the dangers. I highly doubt he is still visiting this forum.


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## markqf1 (Nov 4, 2008)

Lou,
Are you saying to make AR with 70% nitric you should dilute it with water first?
What percentage nitric in the AR does that produce?

Mark


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## Lou (Nov 4, 2008)

No Mark, not at all.

The situation for diluting nitric acid depends entirely on what you are doing with it. By diluting the nitric, you get more bang for your buck. If I am dissolving silver, the process goes more quickly and with less waste if I dilute the nitric to 30-35% because more of the nitrogen oxides are redissolved into water. Furthermore, there is less of a concentration gradient involved with the whole dissolution process, meaning that there is less stirring needed. By this I mean that there is less Ag+ per unit volume in the perimeter of a dissolving object in a 35% solution than say a 70% concentration solution. This means less stirring and heat is needed. This is also true of aqua regia in some circumstances: the aqua regia will work longer and with less waste of reagent if used at more dilute concentration.

A good example of this is the dissolution of mercury: mercury will not readily dissolve in highly concentrated nitric acid, but goes readily into nitric acid of lower concentrations. There are several factors at play, namely the passivation effect, and the concentration gradient of Hg+2 being too high, basically shielding the mercury from further dissolution.

Aqua regia need not be made from concentrated acids, in fact, you can use dilute HCl and dilute nitric and, in the proper proportions, make an aqua regia solution. Generally, it is far easier to make the aqua regia from 1 part 16M nitric acid to 4 parts 12M HCl and then dilute with distilled water to your working concentration. There are many situations where using concentrated aqua regia might not be the best option, or when using it at a certain temperature range is preferable to others.

Yes, I realize that my explanation may have done more harm than good...

Really, there are many factors involved in using acids. There are occasions when you should use them out of the bottle, and then there are times when that is too much or just plain wasteful.

Lou


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## markqf1 (Nov 6, 2008)

Lou,
So it would be safe to say that as far as pgm's are concerned, the stronger the better?
If not, it sure would save me some money on the 70% acs stuff.

Mark


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## Lou (Nov 6, 2008)

Typically, the stronger the better for the PGMs, they dissolve faster in conc. solutions. However, 35% will work well enough!!

Don't get ACS stuff if you can avoid it, technical grade will serve you just fine in this case. That isn't the case with the HCl, you should use good HCl so it isn't contaminated with iron and other metals like muriatic acid is.

Lou


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## butcher (Nov 6, 2008)

PGM's need heat and time to disolve in Aqua Regia, heating also drives of some water concentrating acids, after certain temperatures and concentrations will also evaporate more of acids.


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