Problem with making nitric for silver refining

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Dragnfly1

Member
Joined
Jun 23, 2019
Messages
11
Ok. I've been using the the cold process for homemade nitric and havd had different reactions each time I changed an ingredient. Meaning instated using drain cleaner for sulfuric and sodium nitrate at first. Which the sodium nitrate came from synthesis involving ammonia nitrate and sodium hydroxide. Then I changed over to battery acid for sulfuric. Which changed the reaction, then I changed the way I was drying my converted sodium nitrate and once again. I got a different reaction. Well now I've went to potassium nitrate
 
Ok. I've been using the the cold process for homemade nitric and havd had different reactions each time I changed an ingredient. Meaning instated using drain cleaner for sulfuric and sodium nitrate at first. Which the sodium nitrate came from synthesis involving ammonia nitrate and sodium hydroxide. Then I changed over to battery acid for sulfuric. Which changed the reaction, then I changed the way I was drying my converted sodium nitrate and once again. I got a different reaction. Well now I've went to potassium nitrate
This has recently been discussed here.
Calcium Nitrate is a prime candidate, since if forms Calcium Sulfate which is not soluble.
So then it is just a matter of proper filtering after.
It is slow but that should not matter much.
After you have a crystal clear liquid, it might be wise to add a bit Silver Nitrate to it to precipitate any Chlorides as Silver Chloride,
that might effect your process later.
 
Which I am buying and not using and conversion. Anyways from reading in the forum, the cold process is not good enough to use for silver nitrate which I am trying to make for my silver cell because apparently there are sulphates or sulphides that carry over in the cold process that interfere with the silver refining. So I tried to distill my cold process nitric and distilled it untill it got to 120° C. Then I stopped the reaction and was going to go to bed for the night. Well when I went to pour the remaining nitric back into the bottle I use for storage, some type of salt precipitated out of it.... Did my nitric decompose?
 
This has recently been discussed here.
Calcium Nitrate is a prime candidate, since if forms Calcium Sulfate which is not soluble.
So then it is just a matter of proper filtering after.
It is slow but that should not matter much.
After you have a crystal clear liquid, it might be wise to add a bit Silver Nitrate to it to precipitate any Chlorides as Silver Chloride,
that might effect your process later.
Wow that was a quick reply. Thank you. I will have to see if I can get some calcium nitrate. Any idea what I should do with the 7lbs of potassium nitrate I have left?
 
Which I am buying and not using and conversion. Anyways from reading in the forum, the cold process is not good enough to use for silver nitrate which I am trying to make for my silver cell because apparently there are sulphates or sulphides that carry over in the cold process that interfere with the silver refining. So I tried to distill my cold process nitric and distilled it untill it got to 120° C. Then I stopped the reaction and was going to go to bed for the night. Well when I went to pour the remaining nitric back into the bottle I use for storage, some type of salt precipitated out of it.... Did my nitric decompose?
How is your setup?
I haven't heard much about Sulfates and Sulfides, but the Nitrates used as fertilizers seem to always have some chlorides in it.
That is why it might be wise to add a small amount of Silver Nitrate or a small Silver button to remove the Chlorides as Silver Chloride.
 
How is your setup?
I haven't heard much about Sulfates and Sulfides, but the Nitrates used as fertilizers seem to always have some chlorides in it.
That is why it might be wise to add a small amount of Silver Nitrate or a small Silver button to remove the Chlorides as Silver Chloride.
My distillation set up or my silver cell? I don't have the 12" tube for fractional distillation yet so I just have the standard setup with a snake and such but I have a vacuum container Incase of suck back and then a hose run into ice Water to collect the NOx gasses(as much as possible).... As far as my silver cell, I was building it like sreetips instructed.
There was definitely silver chloride or something in my attempt at making silver nitrate. I guess. I should have purified the potassium nitrate like I used to do with the ammonia nitrate?
 
My distillation set up or my silver cell? I don't have the 12" tube for fractional distillation yet so I just have the standard setup with a snake and such but I have a vacuum container Incase of suck back and then a hose run into ice Water to collect the NOx gasses(as much as possible).... As far as my silver cell, I was building it like sreetips instructed.
There was definitely silver chloride or something in my attempt at making silver nitrate. I guess. I should have purified the potassium nitrate like I used to do with the ammonia nitrate?
It was your distillation setup I was thinking about.
For chlorides in the Nitric the easiest may be to filter your Silver Nitrate after you make it.
I was thinking a bit too complicated in my last post ;)
 
... I tried to distill my cold process nitric and distilled it untill it got to 120° C. Then I stopped the reaction and was going to go to bed for the night. Well when I went to pour the remaining nitric back into the bottle I use for storage, some type of salt precipitated out of it.... Did my nitric decompose?
When I make nitric by distillation, I normally get some sodium hydrogen sulfate salt precipitate in the boiling flask, since both the water and nitrate have been distilled off.

My standard operating procedure for making nitric calls for adding about 10 mL of water to the boiling flask after doing the distillation, to keep these salts in solution:
Nitric acid not condensing.

What's your general plan for handling waste?
 
When I make nitric by distillation, I normally get some sodium hydrogen sulfate salt precipitate in the boiling flask, since both the water and nitrate have been distilled off.

My standard operating procedure for making nitric calls for adding about 10 mL of water to the boiling flask after doing the distillation, to keep these salts in solution:
Nitric acid not condensing.

What's your general plan for handling waste?
I have stock pots (buckets set up that collect waste. First bucket has copper in it to cement out precious metals. Then it gets moved to bucket with cast iron to remove copper. Then my plan is to use baking soda to bring the ph to seven. Is this wrong?
 
I have stock pots (buckets set up that collect waste. First bucket has copper in it to cement out precious metals. Then it gets moved to bucket with cast iron to remove copper. Then my plan is to use baking soda to bring the ph to seven. Is this wrong?
Do you even check where you post?
This has to do with waste treatment not making Nitric?
 
What is the source you are using for your potassium nitrate ?

Product type (like 15-0-0 fertilizer - stump remover - other) &/or product name (Hi-Yield - Spectracide - etc.)

Kurt
First source was stump remover but latest source was a 10# bag of pellets, I assume fertilizer, that is supposed to be 99.8% pure. Which I ordered online through Walmart.
 
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