# looking for someone who is distilling his nitric acid



## ericrm (May 29, 2012)

i have been making my own nitric acid and lately i have a lot of probleme with it
here is what i do
i distille my nitric from 550ml of 30% sulfuric acid and 500g of sodium nitrate
that work fine it give me a weak but very usable nitric acid
BUT it disolve my gold too
at first i tough that my beaker where contaminated but that not the case ,i have tryed it with new beaker and it is the same 
nitrate is from the bag,sulfuric is from the bag,the flask and the beaker are clean ,
end at the end of each batch i try a sample on finger and no gold disolve
BUT when i put my acid on cpu + some heat magicaly it disolve gold.....(i dont realy beleive in magic....)

i know that i have sulfuric acid in my nitric acid and think this is why i got my gold to disolve

i there a way to avoid this?


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## goldenchild (May 29, 2012)

I think the concentration of your sulphuric is the problem. There is too much water at 30% concentration. Try using Rooto drain cleaner. I believe its in the lower 90s concentration. Also use a good fractionating column and preferably a graham condenser.


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## ericrm (May 29, 2012)

goldenchild
could you give a bit more detail because i dont understand how the water will make the solution disolve gold...
what is the difference between adding water before ditilling and adding water after.
or maybe i dont understand you wright and what you mean is with less water in the beggining i will have less sulfuric in my end nitric?
plz explain me if you can

i dont have a fractionating column but i do have a 30 inch graham condenser.


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## butcher (May 29, 2012)

There are chlorides involved, possibly in chlorine added to drinking water, or in the nitrate salts themselves.

It is not from plain water.

You can add some silver nitrate solution to your cooled distilled nitric acid, any chlorides involved would precipitate as silver chloride (and so the silver can be recovered), let it sit long enough for the AgCl to settle before decanting your nitric, if you add silver nitrate to the nitric and no chlorides were involved you would see no precipitant or milky cloud when you added the silver nitrate solution the silver in this solution would cement if you used the nitric on copper, or you would be able to get the little bit of silver back later, your silver nitrate solution can be made from the same batch of nitric you distilled, if you wished (it may form some silver chloride as you dissolve the silver, this would also be an indication chlorides were involved).


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## ericrm (May 29, 2012)

butcher said:


> There are chlorides involved, possibly in chlorine added to drinking water, or in the nitrate saltsthemselves.
> 
> It is not from plain water.
> 
> You can add some silver nitrate solution to your cooled distilled nitric acid, any chlorides involved would precipitate as silver chloride (and so the silver can be recovered), let it sit long enough for the AgCl to settle before decanting your nitric, if you add silver nitrate to the nitric and no chlorides were involved you would see no precipitant or milky cloud when you added the silver nitrate solution the silver in this solution would cement if you used the nitric on copper, or you would be able to get the little bit of silver back later, your silver nitrate solution can be made from the same batch of nitric you distilled, if you wished (it may form some silver chloride as you dissolve the silver, this would also be an indication chlorides were involved).



butcher i have found cottage cheese in my beaker few minute after the addition of my nitric over the cpu. my mind just slipped over it because it was making no sence to me
so your are sure theyr is chloride involved

im piss, those cpu has cost me 100$lbs just for this yield test and i have screwed it...
i will try the silver test ,your all (op) realy impressive, you make me feel small (i realy enjoy it lol)

edit : i use *fertlizer* sodium nitrate could it be that?
can i use 925 silver to test each batch? 
just moving a chain in my nitric should be enuf to make silver nitrate and if hcl is present convert it to silver chloride?


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## goldenchild (May 29, 2012)

ericrm said:


> goldenchild
> could you give a bit more detail because i dont understand how the water will make the solution disolve gold...
> what is the difference between adding water before ditilling and adding water after.
> or maybe i dont understand you wright and what you mean is with less water in the beggining i will have less sulfuric in my end nitric?
> ...



I was under the impression that you were actually distilling nitric acid via a distillation setup. But reading butcher's post and re-reading yours I now understand you are using the cold recipe to make your nitric. Pretty much everything I first posted is null and void except one point. You should still use a more concentrated sulfuric acid. The nitrate should be added to measured amounts of water and dissolved.

Here is a video to help

http://www.youtube.com/watch?v=T-UkqAs2MWE


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## ericrm (May 29, 2012)

goldenchild said:


> ericrm said:
> 
> 
> > goldenchild
> ...



no i realy use a distillation kit ,i just dont use the vigreux...
but thank for the help ( i love poeple who love helping other 8) )


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## butcher (May 29, 2012)

ericrm, 
A little chloride in your nitric may put a small amount of gold in your solution, the silver (even from what you have said in your CPU solution the cottage cheese) will help to remove chlorides in your solution as AgCl precipitate, this would also lower chloride content in nitric and the possible amount of dissolved gold, you can always get any dissolved gold back, and also deal with the little bit of silver chloride in solution as long as you are aware of it, so all and all I really would not worry about it that much and just deal with the solutions and powders accordingly.

The fertilizers or stump remover nitrates are mined and were made for fertilizer and stump remover so the little bit of chlorides involved are not a problem for their intended use, but when we make nitric acid from these products we will just have to deal with these chlorides in our homemade acids.

Sounds like you are coming right along and getting the hang of this recovery and refining, do not sweat the small stuff, just keep studying, so you can deal with them, as these little problems come along.


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## steyr223 (May 31, 2012)

Hello all
You guys are just to quick

I had this one but for a different reason
Tell me if this is right

I have read many posts where a cell is involved
with concentrated sulfuric acid
When the sulfuric is to diluted it puts the other metals
Into solution instead of the gold

Wait ..... o well it seemed to have some connection to
this in my head but now on paper it is ridiculous

yet ...i did come to the same conclusion ...wierd. :lol: 
Thanks steyr223


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## [AuCl4]- (Jun 21, 2012)

Hello, I too synthesize my own HNO3.

Get one drop of your nitric and put it on a piece of copper. Use an old penny from the 70s or earlier. They have a high percentage of copper. If you see a reaction(fizzing and bubbles) immediately, and after 30 seconds to a minute it starts to turn green, your concentration is high enough to make AR. 

Start over again with a new batch and follow the instructions on this video. This guy I'm sure is an advanced chemist.............http://www.youtube.com/watch?v=7akk5ppJjEw

Adjust quantities to your own liking but keep proportions as they are and you will get 68% HNO3. Be sure not to exceed 121 Celsius and stir often if you can. Also, you will get low concentration HNO3 until the temp reaches 121c. Collect the nitric that is low(anything that fills the flask before 121c) and keep it separate from the nitric that starts at 121c , and you will do fine............


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## [AuCl4]- (Jun 21, 2012)

Also, 30% H2SO4 may be too low a concentration as goldenchild has already stated. 

Since you live in Quebec, go to Home Hardware and buy Liquid Lightning drain opener. That is what I use and have never had a problem. 

If you dont trust the fertilizer nitrate you have, and cant find a substitute, go to Shoppers Drug Mart and get one package instant cold packs that they sell for $9.99. They have around 250-290g calcium ammonium nitrate. Make sure the cold packs contain calcium ammonium nitrate and NOT urea. 

I know it is too expensive but try it on a test batch, follow the video and you will be successful.


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## Irons2 (Jun 22, 2012)

HCl can be produced by the same process as making Nitric Acid. If you take Sulfuric Acid, Salt and Distill it, what you get is HCl in your receiving flask.
You can see the problem arising when there is Salt contamination in the Sodium Nitrate. What you end up with is distilled Aqua Regia.
Potassium Nitrate usually has a lower Chloride content due to having a lower solubility than Sodium Chloride. Sodium Nitrate can be converted to Potassium Nitrate using Potassium Chloride and taking advantage of the decreased solubility of the resulting Potassium Nitrate. This technique has been used on an industrial level for a long time. The impure Potassium Nitrate can be purified further by recrystallization and using alcohol as a wash to remove Chloride contaminants. Other Potassium salts may be used as well, as long as the resulting Sodium salt is more soluble than the Potassium Nitrate.


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## ericrm (Jun 22, 2012)

[AuCl4]-
thank for the help, i will look for for the liquid lithening ,how much does it cost?



Irons2 said:


> You can see the problem arising when there is Salt contamination in the Sodium Nitrate. What you end up with is distilled Aqua Regia.



This is my probleme ,theyr is so much salt in my sodium nitate that i make a strong aqua regia.i also have a bag of potasium nitrate (still fertilizer that i havent open thinking it would be the same probleme).



Irons2 said:


> Potassium Nitrate usually has a lower Chloride content due to having a lower solubility than Sodium Chloride. Sodium Nitrate can be converted to Potassium Nitrate using Potassium Chloride and taking advantage of the decreased solubility of the resulting Potassium Nitrate. This technique has been used on an industrial level for a long time. The impure Potassium Nitrate can be purified further by recrystallization and using alcohol as a wash to remove Chloride contaminants. Other Potassium salts may be used as well, as long as the resulting Sodium salt is more soluble than the Potassium Nitrate.



how does it work, i dont understand how to process to clean, can you explain in stupider word plz :roll: i sware it would be apreciated :mrgreen:


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## Irons2 (Jun 22, 2012)

ericrm said:


> [AuCl4]-
> thank for the help, i will look for for the liquid lithening ,how much does it cost?
> 
> 
> ...



Google is your friend.

Here's a useful link: http://www.nakka-rocketry.net/knpurify.html


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## ericrm (Jun 22, 2012)

lol
thanks a lot :mrgreen:


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## [AuCl4]- (Jun 22, 2012)

Hello, no problem friend..........I think its around 12 bucks but will last for many small batches of HNO3. 

About the nitrate fertilizer that you use...........have you tested it for nitrates?

Here is a simple test.............http://www.youtube.com/watch?v=f5M3rUqaEYs

May nitrates fill your beaker friend!


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## ericrm (Jun 22, 2012)

[AuCl4 said:


> -"]Hello, no problem friend..........I think its around 12 bucks but will last for many small batches of HNO3.
> 
> About the nitrate fertilizer that you use...........have you tested it for nitrates?
> 
> ...



:mrgreen: 
it is 2 50lbs of sodium nitrate,and potassium nitrate, no need to test it, it is wroted on the bag :lol: 
i swear maybe it was in my mind but a black car folowed me home after i got them in my truck ... :|


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## [AuCl4]- (Jun 22, 2012)

Lol..........where did you get it? It is almost impossible to get any nitrate in Ontario unless your a farmer or a huge company.


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## ericrm (Jun 22, 2012)

you said it , farmer, find somewhere very deep .i mean very very deep lol
it is fertilizer 16-0-0 ,they will ask for your driver license or your adresse to make sure they know where the nitrate are... 
you can try flower place but i havent add succes with them personaly...
but you are wright it is very hard since dudadiesel stop shipping to canada.


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## [AuCl4]- (Jun 23, 2012)

ericrm said:


> you said it , farmer, find somewhere very deep .i mean very very deep lol
> it is fertilizer 16-0-0 ,they will ask for your driver license or your adresse to make sure they know where the nitrate are...
> you can try flower place but i havent add succes with them personaly...
> but you are wright it is very hard since dudadiesel stop shipping to canada.



LOL.....my friend's father is a farmer not too far from me..........I think I'll give him a try.


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## Irons2 (Jun 23, 2012)

ericrm said:


> [AuCl4 said:
> 
> 
> > -"]Hello, no problem friend..........I think its around 12 bucks but will last for many small batches of HNO3.
> ...



Maybe it was the FLQ bumper sticker on your truck. :mrgreen: 8)


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## [AuCl4]- (Jun 23, 2012)

LOL........je me souviens :lol:


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## ericrm (Jun 23, 2012)

your getting old Iron :lol: FLQ what a bs, now it is the kitchen ware that get the attention from the cop :mrgreen: 

just to be clear ,im in shame of my poeple right now, they go in the streat for 300$/years ,but stay home when 300 children die from unger. quebec has become low in my heart


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## Irons2 (Jun 23, 2012)

ericrm said:


> your getting old Iron :lol: FLQ what a bs, now it is the kitchen ware that get the attention from the cop :mrgreen:
> 
> just to be clear ,im in shame of my poeple right now, they go in the streat for 300$/years ,but stay home when 300 children die from unger. quebec has become low in my heart



My parents were from Canuckistan. 

I hear they were going to vote to secede from Canada until people found out the PQ was going to make poutine the national dish. :mrgreen:


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## ericrm (Jul 20, 2012)

im still having trouble with hydrochloric in my nitric
now i use potassium nitrate that i dissolve and crystalise 2 time and dilute sulfuric acid,the strenght is good, very reactive ,got a nice blue rather than the turquoise i was gotten before, way less hydrochloric acid in my nitric but still have some.... when i put silver in i still got white milk....

so my question is what is my contaminent ,and how do it remove it...
at first i tough it was NaCl but now ,i think it make more sence to be potassium chloride...
im looking to find a way to remove it...
do someone have the knowledge to tell me how 2 salt react in the same solution

can i push selectively one salt out.what i try to mean is, if i saturate a solution of kno3/kcl will one of the 2 salt get out ,or *will they both get in and get out* , or *does water "love" one salt more than the other.*.... sorry for the hard explaining ,i hope you understand what im trying to ask......


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## butcher (Jul 20, 2012)

Look into distilling the nitric acid; also a silver nitrate solution can remove traces of chlorides from your nitric acid (as insoluble silver chloride).


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## ericrm (Jul 20, 2012)

butcher said:


> Look into distilling the nitric acid; also a silver nitrate solution can remove traces of chlorides from your nitric acid (as insoluble silver chloride).





butcher said:


> There are chlorides involved, possibly in chlorine added to drinking water, or in the nitrate salts themselves.
> 
> It is not from plain water.
> 
> You can add some silver nitrate solution to your cooled distilled nitric acid, any chlorides involved would precipitate as silver chloride (and so the silver can be recovered), let it sit long enough for the AgCl to settle before decanting your nitric, if you add silver nitrate to the nitric and no chlorides were involved you would see no precipitant or milky cloud when you added the silver nitrate solution the silver in this solution would cement if you used the nitric on copper, or you would be able to get the little bit of silver back later, your silver nitrate solution can be made from the same batch of nitric you distilled, if you wished (it may form some silver chloride as you dissolve the silver, this would also be an indication chlorides were involved).



i know butcher ,using your trick of silver to remove chloride is actualy what im doing ... , but if i could manage to remove all of the chloride in the beginning that would be the best way to go.it is already enuf trouble to make the nitric by hand that i wish ,if possible to not to have to deal with silver chloride after that. i think you understand


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## ericrm (Jul 20, 2012)

here the words finally got right in my mind...... at the same temperature will the most soluble salt push out of solution the less soluble salt ????? 
so will kno3 push out kcl out of solution????


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## Irons2 (Jul 20, 2012)

ericrm said:


> butcher said:
> 
> 
> > Look into distilling the nitric acid; also a silver nitrate solution can remove traces of chlorides from your nitric acid (as insoluble silver chloride).
> ...



Easy, just buy reagent grade materials, otherwise, precipitate out the chlorides with Silver Nitrate. There is no other solution other than purchasing high purity Nitric Acid.


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## ericrm (Jul 20, 2012)

im a canadian backyard ched chemist... i dont have acces to nitric due to regulation/or price...
that realy disapoint me ... thank you all for the answer, it is *realy* apreciated


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## butcher (Jul 20, 2012)

ericrm, 

I have similar trouble here and understand the frustration part.


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## Irons2 (Jul 21, 2012)

I know Silver Chloride is a pain to deal with, but It will be there, regardless. Just save it up until you have enough to convert into Silver metal. If you want to get rid of any chlorides beforehand, The Nitrate salt can be dissolved, Silver Chloride precipitated (if there is any) and recrystallized, or you can us Noxx's suggestion and use Ammonium Nitrate, but even that should be dissolved, filtered and recrystallized to remove any clay and pellet coating. The pellet coating may have an organic base, not a good idea to boil it with con Sulfuric and Nitrate together.

Ammonium Nitrate prill coatings:

http://pubs.acs.org/doi/abs/10.1021/ie00030a024


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## ericrm (Jul 21, 2012)

Irons2 said:


> The pellet coating usually has an organic base, not a good idea to boil it with con Sulfuric and Nitrate together.


 :shock: woops

what would be the difference with Ammonium Nitrate? does ammonium nitrate fertilizer free of any chloride?


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## Irons2 (Jul 21, 2012)

ericrm said:


> Irons2 said:
> 
> 
> > The pellet coating usually has an organic base, not a good idea to boil it with con Sulfuric and Nitrate together.
> ...



Ammonium Nitrate is produced by reacting Nitric Acid with Ammonia, but anti-caking agents are added, so it's good to check to be sure there's no Chloride contamination.


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## Irons2 (Jul 21, 2012)

ericrm said:


> im a canadian backyard ched chemist... i dont have acces to nitric due to regulation/or price...
> that realy disapoint me ... thank you all for the answer, it is *realy* apreciated



http://goldrefiningforum.com/phpBB3/viewtopic.php?f=58&t=14970


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## ericrm (Jul 21, 2012)

yep i just saw it :mrgreen: im waiting for the details 8) .if the price is right that will be an excellent news


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## ericrm (Sep 4, 2012)

im a bit scared of amonia because of the explosive possibility and my miss of knowledge...is ammonium nitrate safe to use to distillate nitric acid?


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## Irons2 (Sep 4, 2012)

ericrm said:


> im a bit scared of amonia because of the explosive possibility and my miss of knowledge...is ammonium nitrate safe to use to distillate nitric acid?



I wouldn't worry too much. If you want to get rid of the Ammonia, just add NaOH or KOH. The result will be Sodium Nitrate or Potassium Nitrate with the Ammonia driven of as a gas. You can bubble the Ammonia into water to make Ammonium Hydroxide, which you can use to wash your precipitated Gold with.

I edited in red changed the word was, to the word wash what I believe Irons meant to type) Butcher


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## lazersteve (Sep 4, 2012)

Don't forget, ammonia gas is very hard on the lungs and sinuses. If you have any sources of HCl (ie beakers/buckets of muriatic solutions) near the ammonia gas source, the work area will quickly begin to fill with a white ammonium chloride gas. If the sources of ammonia and HCl are plentiful enough. you'll have a tough time breathing anywhere near the reaction. Proper ventilation and containment is a must when working with ammonia gas near muriatic sources. 

You won't realize how much HCl is in the air around you until the ammonium chloride starts to form.

Steve


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