Home made Nitric

[depperl001]

Hi,
I am having some trouble with Nitric acid made to Lazersteve's recipe.
I used Potassium nitrate as nitrate which I bought on e-bay. I made 5 times the specified quantity. The colour of the mixture reminds one of iron yellow, after freezing for 30 min. crystals were found, decanted the top and discharged the crystals. Returned the liquid to the fridge and after a further 30 min. again checked and found more crystals, decanted and again discarded the crystals. By now the liquid was down to 150mL from: 500mL rain water+1kg nitric+ 280mL concentrated sulfuric acid. Heated the remaining liquid to boiling again and added a piece of sterling silver. Left for 2 hrs nothing happened, added a few crystals from the discharge, a faint trace of white went into the clear yellow liquid, left for 5 hrs and liquid turned a coppery green. Which indicated that there was some silver in the mixture, added a piece of copper pipe, again nothing happened except that the copper pipe tarted to dissolve. Am now at a dead end, if anybody can help it would be greatly appreciated.
Regards,
Josef Vavryn

 

[goldenchild]

Because of your repetition of the freezing and decanting I'm assuming that you read the post I have somewhere about doing this. If so you should also take note that I mentioned vaccum filtering the crystals after decanting. There are probably hundreds of milliliters caught up on the crystals. Thats where your difference probably is. Also 30 minutes per freeze is not enough. You probably want to do your first freeze over night. You gotta be patient.

Rain water? You should be using distilled water.

There should be no boiling of the final yeild and you put 1 gram of silver nitrate/dust per liter into the finished product. 150ml is way too small of a quantity to add silver. Thats probably why your end product was green.

What crystals are you speaking of from the discharge? If its from the condensation(freezing) of the nitric you should never be putting them back into the solution.

Lastly what were you trying to accomplish by putting the copper pipe in the acid? That will only dissolve the copper. If you were trying to cement the silver out it will now be replaced by copper and your nitric will be spent. I think you should really do a little more reading on the forum to understand what these acids do and what they are used for. I know this is a shameless plug buy you may also want to look at this http://www.youtube.com/watch?v=T-UkqAs2MWE

Good luck

 

[philddreamer]

The post is "Nitric Acid", under "CHEMICALS" @ Board index.
Goldenchild, you help me out understanding the making of nitric @ home & most importantly, that this nitric doesn't work good digesting silver. So, I'm going to try cu next time I inquart, that way I can use home made nitric.

(I picked up a case of 70% nitric yesterday for my more serious refining. I sold my first oz of Au & bought chemicals, some lab glass. & last, but not the least, 300gm of GF that had 88gm of 14k! And this for only 250.00!
That's why I was able to afford the 70% nitric!)

I have a question, because of using the home made nitric to digest my silver, now there's a coat on the flakes & the acid dissolves very little of the metals. I've read how to solve this problem, but I can't find the post. I believe is using 10% sulphuric... or?

Thank you!

Phil

 

[goldenchild]

No problem Phil

So, I'm going to try cu next time I inquart, that way I can use home made nitric.

This is fine but there are some downfalls to inquarting with copper. I think this was in a post somewhere but I think the main thing was rinsing the copper nitrate completely was a bit more difficult. It will also take more nitric to digest. But it can be done. Test a small lot first. Test test test.

& last, but not the least, 300gm of GF that had 88gm of 14k! And this for only 250.00!
That's why I was able to afford the 70% nitric!

Are you saying that you had 88 grams on solid 14k? If so thats awsome! Be prepared for another 50 grams of the good stuff. This is how it starts. You refine your first few lots and learn the process. Then when you sell the gold you get money to buy more scrap and better equipment. Before you know it the money will be coming in steadily. My first button was 3.1 grams. Now I'm processing ounces of gold every month.

I have a question, because of using the home made nitric to digest my silver, now there's a coat on the flakes & the acid dissolves very little of the metals. I've read how to solve this problem, but I can't find the post. I believe is using 10% sulphuric... or?

You can reduce it with caustic soda and sugar but what I would do is just reshot what you have and digest again with the 70%. I assume you had it all weighed out and know what % of silver you used. So before you remelt, weigh out the silver encrusted cornflake and compare it to your original weight. Add silver to make up for the difference. This will account for the silver that was lost as chloride. It may not be much but it also doesnt hurt to have extra silver in inquartations.

 

[Barren Realms 007]

No problem Phil

So, I'm going to try cu next time I inquart, that way I can use home made nitric.

This is fine but there are some downfalls to inquarting with copper. I think this was in a post somewhere but I think the main thing was rinsing the copper nitrate completely was a bit more difficult. It will also take more nitric to digest. But it can be done. Test a small lot first. Test test test.

& last, but not the least, 300gm of GF that had 88gm of 14k! And this for only 250.00!
That's why I was able to afford the 70% nitric!

Are you saying that you had 88 grams on solid 14k? If so thats awsome! Be prepared for another 50 grams of the good stuff. This is how it starts. You refine your first few lots and learn the process. Then when you sell the gold you get money to buy more scrap and better equipment. Before you know it the money will be coming in steadily. My first button was 3.1 grams. Now I'm processing ounces of gold every month.

I have a question, because of using the home made nitric to digest my silver, now there's a coat on the flakes & the acid dissolves very little of the metals. I've read how to solve this problem, but I can't find the post. I believe is using 10% sulphuric... or?

You can reduce it with caustic soda and sugar but what I would do is just reshot what you have and digest again with the 70%. I assume you had it all weighed out and know what % of silver you used. So before you remelt, weigh out the silver encrusted cornflake and compare it to your original weight. Add silver to make up for the difference. This will account for the silver that was lost as chloride. It may not be much but it also doesnt hurt to have extra silver.

He should dilute the 70% in half with water to get a better reaction.

 

[goldenchild]

He should dilute the 70% in half with water to get a better reaction.

Oh yeah that too. 1:1 ratio of 70% nitric and DISTILLED water. Very important that its distilled.

 

[philddreamer]

Thank you guys!
The use of cu for inquating is so to use the sodioum nitrate. I won't use my 70% that way; I'll use it to refine ag scrap that I would buy & when inquart w/ag.

Yes, 88gm of solid 14k, . I, like you, want to get to that point of processing ounces per month.

I always dilute my nitric 50/50. The problem is not with ag refining, its with the ag inquarted gold. There's a coat that will not allow the gold to dissolve.
I tried incenarating, but I get a dark/reddish slag & when I get it to smoke,
a golden hue appears on the iron plate. I tried melting a piece, but a blood red slag is what a get first. After more heat'n & smoke, the golden button appears.
How can I wash that coat off?

Phil

 

[Barren Realms 007]

Boil the button in sulfuric.

 

[goldenchild]

I tried incenarating, but I get a dark/reddish slag & when I get it to smoke,
a golden hue appears on the iron plate. I tried melting a piece, but a blood red slag is what a get first. After more heat'n & smoke, the golden button appears.
How can I wash that coat off?
Phil

I forgot to mention this and really should have. That smoke that is forming is most likely silver chloride burning and is very dangerous and toxic. Whatever you do dont breathe it in!

As Barren Realms suggests you can boil the button in dilute sulfuric acid to get the slag off. To get a majority off the button before removing it from the crucible you should add a pinch or two of boric acid to the button when its molten. This will push the slag off to the side.

Im sure by now you have a crucilbe with a bunch of the reddish slag in the shape of a circle on the bottom. You will most likely have to get this out by using sodium carbonate aka soda ash. You can get this at walmart at a purity of 98% quite inexspensively. Its called PHup or hth ph plus and is found in the pool section.

You melt the soda ash in the crucible and get the liquid that is formed to touch all the slag. This reduces the slag. Any metals that you thought werent there will come together. You then do as you would with inquarting and "shot" it out of the crucible(you dont keep whats left over except for any metals). Needless to say this crucilbe is now best reserved for inquarting/incinerating.

 

[philddreamer]

I suspected that! :shock: So ag/Cl is the culprit of the red slag... :evil:
OHHHHH, I know where it came from! I inquarted the gold with ag from an ag cell. I saw thew ag/cl, but it was days later I used it, & by then I had forgotten, DUHHH! Oh well, we live & learn!

Boiling in sulphuric also confimers what I read in a post, somewhere. I used ammonia, but I guess is not as strong as sulphuric.

I'll kep in mind the boric acid. I'll clean the crucibles with soda ash. I keep them separated.

Thank you guys!

 

[Oz]

I know where it came from! I inquarted the gold with ag from an ag cell

A silver cell with chlorides?

 

[dtectr]

I suspected that! :shock: So ag/Cl is the culprit of the red slag... :evil:
OHHHHH, I know where it came from! I inquarted the gold with ag from an ag cell. I saw thew ag/cl, but it was days later I used it, & by then I had forgotten, DUHHH! Oh well, we live & learn!

Boiling in sulphuric also confimers what I read in a post, somewhere. I used ammonia, but I guess is not as strong as sulphuric.

I'll kep in mind the boric acid. I'll clean the crucibles with soda ash. I keep them separated.

Thank you guys!

Ammonia is a base and sulfuric is ... well, an acid. I wouldn't expect that they could be used interchangeably, or am I wrong? I haven't finished Hoke, yet.

 

[philddreamer]

The chloride came when I tried to get rid of any cu present when I got done with the ag cell. I started with cu nitrate, got most of the cu out, but knew some would be left. I went to do other things, & a few days later I tried to continue the refining of some karat gold, needed to inquart & did a quick rinse of the ag & that's when my troubles began. It's under control now.

I used the ammonia as part of the rinsing steps, but it wasn't enough to get rid of the ag cl; 1hr into the 50/50 nitric, the white coat came back, (like the cat) :roll: But we live & learn! :lol:

Phil

 

[depperl001]

Because of your repetition of the freezing and decanting I'm assuming that you read the post I have somewhere about doing this. If so you should also take note that I mentioned vaccum filtering the crystals after decanting. There are probably hundreds of milliliters caught up on the crystals. Thats where your difference probably is. Also 30 minutes per freeze is not enough. You probably want to do your first freeze over night. You gotta be patient.

Rain water? You should be using distilled water.

There should be no boiling of the final yeild and you put 1 gram of silver nitrate/dust per liter into the finished product. 150ml is way too small of a quantity to add silver. Thats probably why your end product was green.


What crystals are you speaking of from the discharge? If its from the condensation(freezing) of the nitric you should never be putting them back into the solution.

Lastly what were you trying to accomplish by putting the copper pipe in the acid? That will only dissolve the copper. If you were trying to cement the silver out it will now be replaced by copper and your nitric will be spent. I think you should really do a little more reading on the forum to understand what these acids do and what they are used for. I know this is a shameless plug buy you may also want to look at this http://www.youtube.com/watch?v=T-UkqAs2MWE

Good luck

Hi goldenchild,

Point 1/ I was using lazersteve's Formular for KNO3, multiplied 5 times
Point 2/ If I had left it in the freezer over night my wife would have had kittens or
used a shotgun on me. And also I would have no liquid left, as the second
freezing took every thing bar 150mL and the balance was in salt crystals.
Point 3/ The 150mL did not start reacting until I returned 2 or 3 crystals, from the second
freeze, into the liquid. Then there was a slight fizzing, by that I mean a slight
trace of a white plume. Left it do what it wanted for 4 hrs., returned to it and
found that the silver button had dissolved a slight amount. Now the color of the
liquid was a greenish blue, which according to lazersteve's video indicated that
there was metal, apart from copper in the liquid.
Point 4/ Used a copper pipe to drop the cement of silver out of the liquid.
Point 5/ As there in no distilled water available in R'ton, where I live, the next best thing
is demineralised water, which should be the same as rain water.
Point 6/ There is no mention of vacuuming the end product on lazersteve's video.

To continue, after leaving the copper pipe in the liquid over night there was a light grey to
brown cheesy deposit on the copper pipe, which I presume to be silver and ??????????
metal. When I decanted the liquid from the top and filtered the brownish grey cheese there are some yellow crystals in the bottom of the flask. Perhaps you can tell me what those are.

Until I am set up to vacuum filter and make my own distilled water, demineralised water will have to do.

Regards,
Josef Vavryn

 

[goldenchild]

Hi goldenchild,

Point 1/ I was using lazersteve's Formular for KNO3, multiplied 5 times
Point 2/ If I had left it in the freezer over night my wife would have had kittens or used a shotgun on me.
Point 3/ The 150mL did not start reacting until I returned 2 or 3 crystals, from the second freeze, into the liquid. Then there was a slight fizzing, by that I mean a slight trace of a white plume. Left it do what it wanted for 4 hrs., returned to it and found that the silver button had dissolved a slight amount. Now the color of the liquid was a greenish blue, which according to lazersteve's video indicated that there was metal, apart from copper in the liquid.
Point 4/ Used a copper pipe to drop the cement of silver out of the liquid.
Point 5/ As there in no distilled water available in R'ton, where I live, the next best thing is demineralised water, which should be the same as rain water.
Point 6/ There is no mention of vacuuming the end product on lazersteve's video.

To continue, after leaving the copper pipe in the liquid over night there was a light grey to brown cheesy deposit on the copper pipe, which I presume to be silver and ??????????
metal. When I decanted the liquid from the top and filtered the brownish grey cheese there are some yellow crystals in the bottom of the flask. Perhaps you can tell me what those are.

Until I am set up to vacuum filter and make my own distilled water, demineralised water will have to do.

Regards,
Josef Vavryn

Based on the facts stated here I dont know if you will be able to make quality nitric acid. In the video that you keep referring to as lazersteve's and in fact is mine, I am using sodium nitrate and not potassium nitrate. Are you using the video's requirements or lazersteve's written instructions? If you are following my video using potassium nitrate it will not work(not well at least).

If you arent able to condense the liquid using a freezer or other type of cold storage I believe the only other option you have is a salt water ice bath which wont work as well. You will have to do a few of these to simulate the overnight refrigerated freezings. Distillation is reserved for the final product after all the condensation has taken place. This is to remove TRACE amounts of chlorides so this isnt an option either.

Again crystals should never be reintroduced into the mix. The whole point of the condensation is to remove the crystals. The non reaction of the silver you describe is probably just due to the nitric acid not being properly produced.

Dont use the copper pipe. All this will do is exhaust your nitric acid.

Where is R'ton? Not familiar with this abbreviation. It is very important that you used distilled water. If it isnt available in your area you may have a problem. I would tell you to go on ebay for some distilled water but it is ridiculously expensive on there. If there isnt distilled water I'm guessing there also isnt spring water as a possible alternative?

The vacuum filtration is something I discovered after the videos production. Just keep in mind that each vacuum filtration should be parallel with each condensation. So you vacuum filter the crystals that are produced after first making the acid and add the filtered acid to the bulk. Then the second accumulation of crystals from condensing is vacuum filtered and added to the bulk and so on. The point I'm trying to make is not to hoard all the crystals from each condensation, filter, and then add to the final product.

I think I addressed all the points here. If you still cant get it after this I'm wondering if buying the nitric is an option?

 

[lazersteve]

Distilled water is simply water that is evaporated and condensed in a separate container.

Place the source water in the boiling flask and affix a poly hose to the boiling flask.
Gently boil the water in the flask and collect the water from the hose in a cold receiving flask.

Steve

 

[depperl001]

Distilled water is simply water that is evaporated and condensed in a separate container.

Place the source water in the boiling flask and affix a poly hose to the boiling flask.
Gently boil the water in the flask and collect the water from the hose in a cold receiving flask.

Steve

Hi Steve,

That is what I am doing now. This does not explain the yellow crystal that I finished off with, they are reminiscent of Sulphur crystals. Also when I filtered the silver "cheese ' there are a few dark green crystals mixed in with the silver. I realise that all this is contamination in either the water, which I would find rather hard to believe, or in the sulphuric acid. I know that I have iron in my Hydrochloric acid as the the stannous chloride turned a light purple when I placed a bit of tin in it. Those green crystals remind me of iron sulfite, don't know where that came from.
Oh, the CD arrived to day, I am looking forward to the next order.

Regards,

Josef Vavryn

 

[depperl001]

Hi goldenchild,

Point 1/ I was using lazersteve's Formular for KNO3, multiplied 5 times
Point 2/ If I had left it in the freezer over night my wife would have had kittens or used a shotgun on me.
Point 3/ The 150mL did not start reacting until I returned 2 or 3 crystals, from the second freeze, into the liquid. Then there was a slight fizzing, by that I mean a slight trace of a white plume. Left it do what it wanted for 4 hrs., returned to it and found that the silver button had dissolved a slight amount. Now the color of the liquid was a greenish blue, which according to lazersteve's video indicated that there was metal, apart from copper in the liquid.
Point 4/ Used a copper pipe to drop the cement of silver out of the liquid.
Point 5/ As there in no distilled water available in R'ton, where I live, the next best thing is demineralised water, which should be the same as rain water.
Point 6/ There is no mention of vacuuming the end product on lazersteve's video.

To continue, after leaving the copper pipe in the liquid over night there was a light grey to brown cheesy deposit on the copper pipe, which I presume to be silver and ??????????
metal. When I decanted the liquid from the top and filtered the brownish grey cheese there are some yellow crystals in the bottom of the flask. Perhaps you can tell me what those are.

Until I am set up to vacuum filter and make my own distilled water, demineralised water will have to do.

Regards,
Josef Vavryn

Based on the facts stated here I dont know if you will be able to make quality nitric acid. In the video that you keep referring to as lazersteve's and in fact is mine, I am using sodium nitrate and not potassium nitrate. Are you using the video's requirements or lazersteve's written instructions? If you are following my video using potassium nitrate it will not work(not well at least).

If you arent able to condense the liquid using a freezer or other type of cold storage I believe the only other option you have is a salt water ice bath which wont work as well. You will have to do a few of these to simulate the overnight refrigerated freezings. Distillation is reserved for the final product after all the condensation has taken place. This is to remove TRACE amounts of chlorides so this isnt an option either.

Again crystals should never be reintroduced into the mix. The whole point of the condensation is to remove the crystals. The non reaction of the silver you describe is probably just due to the nitric acid not being properly produced.

Dont use the copper pipe. All this will do is exhaust your nitric acid.

Where is R'ton? Not familiar with this abbreviation. It is very important that you used distilled water. If it isnt available in your area you may have a problem. I would tell you to go on ebay for some distilled water but it is ridiculously expensive on there. If there isnt distilled water I'm guessing there also isnt spring water as a possible alternative?

The vacuum filtration is something I discovered after the videos production. Just keep in mind that each vacuum filtration should be parallel with each condensation. So you vacuum filter the crystals that are produced after first making the acid and add the filtered acid to the bulk. Then the second accumulation of crystals from condensing is vacuum filtered and added to the bulk and so on. The point I'm trying to make is not to hoard all the crystals from each condensation, filter, and then add to the final product.

I think I addressed all the points here. If you still cant get it after this I'm wondering if buying the nitric is an option?

Hi Goldenchild,
It is Lazersteve who produced the video I am referring to. It is on his website. Spring water has more garbage in it than rainwater. To name a few possibles: Sulphur, fe3, NaCL, Calcium bicarbonate, and any other mineral that is in the area. Oh sure buying the Nitric is an option, locally I can buy it for $135/20L. A bit steep, don't you think? Copper pipe is used by me to cement out the silver. I suppose I could go and buy copper sheeting, again at considerable cost. At this rate I might as well throw the Sterling Silver away and buy more 92.5% silver. Now I know that you think I am a complete newchum to all this, but I have been making SS jewelery for 20 years. Oh, you don't recognise R'ton as an abreviation. Correctly spelled it is Rockhampton, Queensland, Australia. So please give me a break with your advice and spare me your opinion.

I will endeavour to post a couple of pics re. the crystals I don't know.
Regards,


Josef Vavryn

 

[lazersteve]

If you can get 70% nitric for $6.75 per Liter, I would go that route.

I would love to be able to get my nitric that cheap.

Steve

 

[goldenchild]

Hi Goldenchild,
It is Lazersteve who produced the video I am referring to. It is on his website. Spring water has more garbage in it than rainwater. To name a few possibles: Sulphur, fe3, NaCL, Calcium bicarbonate, and any other mineral that is in the area. Oh sure buying the Nitric is an option, locally I can buy it for $135/20L. A bit steep, don't you think? Copper pipe is used by me to cement out the silver. I suppose I could go and buy copper sheeting, again at considerable cost. At this rate I might as well throw the Sterling Silver away and buy more 92.5% silver. Now I know that you think I am a complete newchum to all this, but I have been making SS jewelery for 20 years. Oh, you don't recognise R'ton as an abreviation. Correctly spelled it is Rockhampton, Queensland, Australia. So please give me a break with your advice and spare me your opinion.

I will endeavour to post a couple of pics re. the crystals I don't know.
Regards,


Josef Vavryn

Sorry for my ignorance on R'ton. Did anyone else know that one? I was trying to help you but will keep my opinions and advice to myself from now on.

Good luck