looking for someone who is distilling his nitric acid

[ericrm]

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?

 

[goldenchild]

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.

 

[ericrm]

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.

 

[butcher]

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).

 

[ericrm]

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?

 

[goldenchild]

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.

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

 

[ericrm]

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.

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

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) )

 

[butcher]

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.

 

[steyr223]

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

 

[[AuCl4]-]

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............

 

[[AuCl4]-]

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.

 

[Irons2]

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.

 

[ericrm]

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

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).

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:

 

[Irons2]

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

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).

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:

Google is your friend.

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

 

[ericrm]

lol
thanks a lot :mrgreen:

 

[[AuCl4]-]

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!

 

[ericrm]

-"]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!

: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 ... :|

 

[[AuCl4]-]

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

 

[ericrm]

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.

 

[[AuCl4]-]

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.