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Oneal,
Below is one I posted, I really like it, one of my favorite’s actually I tried to explain this process I came up with, one on one of the first posts I made coming to the forum, I could not type then and was not very good at computers or the English and grammar, running all the sentences together (I may have gotten a little better now but sure you guys still have a hard time with my skills in this matter), I was a newbie, and had been lurking for a while before deciding to post, so I had an admiration of Harold, GSP, (Chris), Irons, Lou, and others, well I made my this first post trying to share my process, Harold chimed in saying he could not read a word I said, (man that hurt, I almost said to heck with this forum and quit then, but Ragbone chimed in, and calmed down my hurt pride, and I stuck with the forum trying to make my posts where Harold could read them), (Harold has taught me much not only in gold refining but in other walks of life, funny how a man who you have never seen, but you look up to can make such a difference in your life, never met Him but will always consider Him a friend and mentor
I also make nitric the cold method Laser Steve’s recipe, it is the best I have found (I have studied nitric intensely), this solution, works well for everything but silver (but you can distill it and then it is good for silver. So this is the method I suggest you begin with, there is also much information of this process here on the forum.

I have also made fuming nitric, but there is no need to make that or use that.
So 68% is the strongest you need (used in aqua regia), and more dilute to remove base metals and silver.
Always distill homemade nitric for silver.
I have made many posts on the properties of nitric acid, how to concentrate it, and its azeotropic nature, I will not go into that again now,
There are other processes to make nitric, I will not mention now, as it would just clutter this page.

I can process gold plated pins and make nitric acid at the same time here is my favorite process “Kill two birds one rock”, the principles here have many uses not only with the process stated here, and can be adapted to other processes.

You can use lab glass, distilling rig, but I still use my old pickle jar.

Process for pins, nitric acid and copper sulfate
Kill two birds one stone

A few principles:
You need sulfuric acid with nitrate (salts) to create nitric acid,
Gold will not dissolve in nitric acid alone,
Copper will dissolve in nitric acid evolving NO2 gas.
NO2 gas bubbled into water can form nitric acid.
NO2 + H2O --> HNO3
NO gas also evolves; oxygen will convert this to NO2,
NO + O2 --> NO2
So: if we add a little H2O2 to this we have oxygen and water, we can convert NO gas to HNO3,
NO + H2O2 --> HNO3

Gold will not dissolve in copper nitrate or copper sulfate.
Nitric acid will evaporate from a solution at a much lower temperature than a sulfate will.
2 NaNO3 + H2SO4 --> Na2SO4 + 2HNO3
Nitrate fertilizer + sulfuric acid àsodium sulfate + nitric acid.
In our case we are using copper to help.
Copper dissolving in nitric acid evolves NO2 and NO fumes.
Cu + 2 HNO3 --> CuNO3 + 2NO2(g) + 2 H2O
When we distill this copper nitrate we remove the Nitrate and leave the copper sulfate behind, diluting this to retrieve our un-dissolved gold.
Cu(NO3)2 + H2SO4 --> CuSO4 + 2HNO3
Copper sulfate is water-soluble.

(Copper sulfate solution we make here is soluble while hot, but will crystallize out as bright blue crystals if allowed to cool, (copper sulfate crystals once formed are harder to dissolve) than if we keep them hot while diluting the solution not allowing them to crystallize).

This is my method for pins (which can be adapted to distill copper nitrate solution to make nitric acid) or adapted for use with other chemicals and processes.

(This process can be adapted to other recovery or refining methods to kill two birds with one stone, like recovering nitric or aqua regia while dissolving karate gold)

A distilling unit rig (I have a nice lab distilling unit), but I like my homemade kit, and use it for this process, my unit has survived many distillations, but as with any distilling glass precautions must be observed,

Some supplies I use:
(My Pickle jar distilling kit)
Large pot with handles
Sand
Canning gallon pickle jar
A lid for gallon jar --made from 1/2" thick Teflon,(or the plastic wood they make decks out of HDPE I think) turned on a lath beveled edge to tightly fit jar, small lip on top edge, a hole in center for tight fit of 1/4" hose.
8' 1/4" Teflon hose
Long neck bottle
(For this bottle either loose fitting Teflon cork with hole or just use tape)
Gallon bucket of ice water
Double burner electric hot plate
(Ground fault protected electrical outlet)
Fiberglass catch tray for burner to sit on to catch any spill
Pyrex coffee pot
Some wire, plumbers Teflon tape, cloth tape, electricians black tape
New battery sulfuric acid 10 cups, (we will boil down to 6 cups)
Cup of sodium or Potassium nitrate fertilizer
One pound of (copper) gold plated pins no solder (cut to expose copper to acid)
(Teflon will withstand temperature and fumes of these acids)
(A nearby box of baking soda and water for safety)

Required:
Understand the dangers of these acids, and precautions to take, understand the danger of the nitrous gases formed, and precautions to take, understand the principles of distilling and precautions needed, understand glass cannot withstand thermal shock (rapid temperature change).

Never cool or lower temperature to boiling reaction vessel without removing line to condenser,(which can cause suck back of cold solution into hot boiling flask breaking it through thermal shock),always remove tube before lowering heat on boiling flask,

Work outdoor using breeze or with fume hood, take safety precautions.

Double hotplate sits on fiberglass catch tray; ground fault electrical source is used outdoors

10 cups of sulfuric battery acid boiled down to 6 cups in the Pyrex coffee pot on one burner boil down to 6 cups and cool. To boil off some water in the acid, it will still contain some water (We will use this cool sulfuric acid later),
(We could also pour concentrated sulfuric acid drain cleaner into water to dilute it).

The large pot, pour a couple of inches of sand in bottom of it spread flat, the gallon canning pickle jar is sits on this sand centered in the large pot and sand poured in between pots metal and outside of pickle jar, to make a boiling reactor with a sand bath. This will help to protect our glass from thermal shock, (sand bath around pickle jar), allowing heat to change slowly, and can act as catch basin if we make a mistake. The 1/4" Teflon hose fits tightly into Teflon lid for our gallon pickle jar boiling reaction vessel, we will be collecting NOx gas from this vessel, so hose just in through the lid just a little ways, to capture gasses formed in reaction vessel.
(Later we will tape on this lid, and tie it down)
(Get tape and wire ready and handy within reach, we will need it as soon as acid is added later)
Get ice water in gallon bucket (plastic ok) this is for cooling our gases and condensing them, our collection bottle will sit in this bucket,
Put small amount of water in the long neck bottle (collection bottle for condensed nitric acid) for NOx gas to bubble through water, (I add a little H2O2 peroxide to help conversion, it is not necessary), put one end of the Teflon 1/4" hose into this collection bottle all the way down into bottom of bottle so gases bubble through water and hydrogen peroxide inside, (through a loose fitting Teflon cork or else just tape hose to top of bottle, air, and some gas will need to escape from this bottle, and we do not want to prevent this with a tight fitting lid), this long neck bottle needs to sit down in iced water of bucket to condense gas to liquid, and we need to hold it down in ice water (it wants to float till it fills), so we tie in down into ice water bucket, this is our condenser receiver for the NOx fume's which will bubble into water in this longneck bottle and convert to nitric acid, a few loops of this hose is under ice water to help condense fumes also.

Set large pot sand bath with our fancy pickle jar boiler reaction vessel on cold electric hotplate, put one pound solder free (copper) gold plated pins, (cut to expose copper to acid I cut mine small for more exposure), in reaction vessel, add one cup of sodium nitrate fertilizer, (with lid and tape handy ready we will need to put on lid to contain brown NOx fumes in next step), pour in cooled 6 cups sulfuric acid on these, quickly put on Teflon fitting on lid and taping on the with Teflon plumbers tape first, then bandage cloth tape, then black electrical tape sealing this lid well, the insulated solid copper tie wire is tied to one handle of the pot over top of lid on jar and tied to other pot handle, this will hold down the lid when pressure builds,
As soon as you pour the sulfuric acid on the nitrate fertilizer and copper, red brown nitrous gas NOx begins to form, so getting lid on quickly and taping to seal is needed, we will need no heat yet, as it creates its own heat from chemical reaction, turning burner on warm will start to heat pot and sand, with time, the heat will saturate sand and starts to warm the jar. When reaction slows (bubbling in receiver slows) and pot is warm raise heat a little, (little bit at a time) giving time for heat to reach and react chemicals as red fume slow, or gas bubble slow in receiver, we want a steady few bubbles, not too fast we only want the gas to go to the condenser and receiver. (There is a point to where nitric will concentrate to azeotrope in the boiling flask and reaction begins to get more vigorous with red fume’s of NOx gas), keeping a steady stream of bubble into our receiver is our goal, not liquid the blue liquids from our boiling flask).

Caution we do not want to change temperature on glass fast, this thermally shocks glass and will crack or break it, always keep this in mind.
Do not lower the temperature of the boiling vessel, with the hose in the condenser receiver, always remove this hose from the receiver first allowing it to suck air, (this higher temperature in the boiling vessel creates a pressure, and if we lower the temperature on this boiling vessel, it will go into a vacuum, this will suck the cooler condensed liquid back into this hot boiling flask, thus causing thermal shock and cracking our jar, by removing this hose first it just suck’s back air, and not liquid, as the pressure lowers in this boiler reaction vessel.

(I preheat a coffee pot of water, just below boil for procedure below, starting the water heating before hand)

We do not want to evaporate this now forming copper sulfate to a dry salt, we just want to drive out the formed nitric acid, so we evaporate to thick syrup, (I have noticed a color change from blue-green to blue-blue as the nitrates are driven out of the copper sulfate),
After we have evaporated down to syrup.

NOTE:
We want to remove hose from the condenser receiver, before lowering temperature.
(See caution on suck-back of these cooler liquids when lowering temperature of reaction vessel, thermal shock),
We can let cool before diluting this copper sulfate syrup, but this will form salts and it takes more water to dilute, (that may be best for you as this step if not done properly can thermally shock your boiling vessel), I use the water we heated above (on second burner in coffee pot, getting this water to about the same temperature of this syrup, and very slowly adding this boiling hot water to the syrup to dilute it, starting with just drops at a time, not pouring in all at once, this dissolves the blue copper sulfate syrup and leaves gold shells and powder from pins.
Allow this dilute copper sulfate liquid to settle the gold, and then decant liquid from gold and filter solution.

These gold foils will need further treatment to refine to pure gold.

This copper sulfate can be evaporated to nice blue crystals of copper sulfate for other chemical reactions, or for an electrolytic cell or other uses, wall mart sells them at a high price to keep roots from growing in sewer lines.

This nitric acid tested for strength, and evaporated to 68% concentration azeotrope if necessary, cool, stored in amber nitric bottle with proper lid put out of light (light breaks down nitric). Store in safe place for later use in recovery or refining

Distilling copper nitrate, (adding copper or gold plated copper can assist creating NOx fumes in boil, which also is a way I get gold plating from Pins. killing two birds one stone) would get nitric back from this copper chloride solution, bubble NOx gas into water, for dilute nitric, which can then evaporate water from dilute nitric until 68%HNO3 azeotrope, (many acids form azeotropes), so if just evaporating a dilute nitric solution, below the boiling point of the acid (for the concentration that the acid is at the time in solution), would boil off water (or other volatile components if in solution), making the acid more concentrated in solution, up to the azeotrope of the acid, which for nitric is about 68%, further boiling would only boil off the 68% solution till dry, meaning it cannot be further concentrated by this method, by using the boiling point information a person can have a good idea if they are boiling off acid or just water, the concentration can be tested with specific gravity, or judged by how it attacks metals.

(100% H2O) boils @100 degC density 1.00.
20% HNO3 density 1.115- boiling point 103 degC.
30% HNO3 density1.180 boiling point 107 degC.
50% HNO3 density 1.310 boiling point 116 degC.
70% HNO3 density 1.413 boiling point 121.5 degC.

(Pure HNO3 boiling point is about 83 degC, so you can see the boiling point goes up as the nitric is less concentrated, till about 68% azeptrope (nitric acid’s highest boiling point about 120 degC), then as we get more dilute towards just water the boiling point falls toward the boiling point of water 100 degC).

As you can see the boiling points change with how concentrated the acid is. Keeping below the boiling point most all of your acid stays in solution, and mostly water vapors off, above the boiling point acid leaves solution in vapors with the water.
Other acids and have reaction similar to this. For more information you can study the azeotrope of acid, boiling points, acid concentrating, I have also posted this information on forum in other posts.

{Basically we made nitric acid with nitrate fertilizer and sulfuric acid, nitric acid distilled off in condenser bottle, the copper helping to drive the reaction, dissolved copper from the gold making copper nitrate in solution in boiling vessel, and since we had a slight excess of sulfuric when we distilled out the nitric fumes (making nitric acid ) we left sulfuric acid in boiling flask which forms copper sulfate solution, and gold foils, which we will dilute the copper sulfate with boiling hot water before allowing to cool so we can seperate gold foils from copper sulfate solution}.


I have added some points to this post today; here was the one posted and some questions answered about it,

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=38&t=6199&hilit=kill+two+birds+one+rock

Read and understand dangers involved before attempting, this method it is safe I have done it many times, but precautions must be taken, and dangers must be taken into account.

My hope is this is readable and understandable, and someone will gain information or it will spark ideas in others.

Butcher
 
Hi Butcher, I appreciate it buddy, I knew you could be counted on! You truely are a wonderful person and I appreciate you!
Butcher, I follow 95% of the process but have a few questions here and there. Mainly just on quantities/expected returns/ weights of gold pins/plus copper, Etc;. such things as that. Maybe the size of the long neck bottle (wine?) and how much water to put into it, such things as that. Just the odds and ends of the process. But let me gather up everything I need and put it together and I will make sure and clear up that other 5% before I even think about starting up, I promise.
I got to get me a double burner, been looking for one at the consignment shops (like Kadriver found) that lucky rascle, but haven't found one. I will have to look at it like this, by the time I go by a few gallons of nitric I will have bought a double burner a couple of times over. Butcher the Nitric I have been using is around 68% industrial grade ( I think) so the strength sounds good to me. I don't think I would need anything stronger unless something changes? I got my mind on Platinum already but that's another story. There are several Salvage Yards (hundreds of cars of all kinds) right around me with all the salvage title car/truck rebuilder's in this area. But I haven't even touched on what's involved there yet. Had my hands full with what I have going on now.
Give me a few (or more)days and I will get back with you.
I got to start building my grandaughter a playhouse tomorrow for Christmas. That will take me a week I am sure. Got to keep it hid from her as well, so that's a problem. I guess I will build it behind the old house where she knows not to go near. That might work. Anyway, my daughter keeps changing the plan on me. It started out being about 70 sq. feet and now it's up to 110. I told her is she didn't stop messing with the plans I might as well build her a new house!
But thanks Butcher, I really,really, appreciate you.
I will be back on in a few hopefully, if I can keep my daughter from changing those plans anymore.
Talk at you later Butcher, THANKS!!!
Oneal
 
My hot plates have solid Iron burners with heating coil under iron plate I like these better than the type kadriver uses (coil type burner), I believe the heat is distributed more evenly (less likely for hot spots on cookware, I get mine for just a little over twenty dollars new at BiMart store, I also grab one if I find it in second hand store for a few dollars, you could also use a propane or gas burner with the sand bath.

If using the coil type electric burner or gas type burner I would put a steel plate, or wire screen between burner and cookware to distribute heat evenly.

That is a big playhouse maybe we can see a picture of it with that cutie bug of yours smiling big inside it?
 
Hi Butcher, you got it. I will send you one through a personal email. I am so protective of her I just don't want her picture out there on the web, if you know what I mean? I trust everyone on the site, but now and again you have visitor's come through that you just don't know about. I guess I watch too much news about missing or worse children. I would not allow my daughter to put herself or the kids on facebook or any place else for that matter.
If I could get my hands on that kind of person that would hurt a child, well, that's all I need to say about that! I am sure you can understand why I am like that by her and my grandson. But I promise to send you a picture day of or day after Christmas. I am sure my daughter is going to keep me busy on this thing right on up to Christmas Eve. She is just too much like me I guess.
Every project I start, I say I am going to keep it simple. It always ends up on the upper end of rediculous.
Got to go to work on it now. It's just warmed up enough for me to get outside. Cold snap here, unusual for here this time of year? It's still in the low 40's outside, that's cold for here and for me at my age, with the blood thinners I am on.
Talk at you later.
Oneal
 
Butcher-

I must say that you have made some really great posts regarding nitric acid, manufacturing and recycling/reuse of refining byproducts, and other dynamic methodology. Thanks for the boiling point references.

John
 
John thanks, just trying to share what I learn, this forum and members here have taught me so much, I just want to try and give some tidbits back.

Oneal,
I do understand your not wanting your little angels picture for the world to see, and it is a shame that-that evil does exist, I too would not put a man who would hurt an innocent child behind bars and feed him, even torture or death, may be too kind for that kind of slime of man and the earth.

Only problem being out there building the playhouse is your granddaughter is missing her gramps spending time with her, maybe you can have her help you build some parts of the playhouse, do not tell her what it is she is building, like a wall door or window, these parts you could take around back and install them without here seeing the building going up, and when she finally sees her playhouse and the window she helped her grand pappy build she will like it even more, as she had fun and learned working with you, and also sees her work in her little house, she could also help grandmamma make the curtains for her window, not knowing what she is sewing. Since this forum is about gold I should keep to the subject about gold, I think the smile on her face when she sees her playhouse will be pretty and golden.
 
Hi Butcher,
I hope you and your family (as well as everyone else here on the site) had a wonderful Christmas and I wish you'all a Happy New Year!
I finally got the playhouse for my grandaughter finsihed at 4:00 a.m., Christmas morning. On top of that I have had to work with a case of the flu the last couple of days. I have been in bed ever since. I have just gained enough strength to say hello to everyone and say that I will be back to my aggravating self hopefully in a couple of days asking questions again.
Butcher, I hope to start up on the process of making the nitric acid with your instructions you posted for me. I just want to clarify a couple of things before I get started.
Question 1- I don't have any gold plated pins, but have plenty of copper tubing. I have plenty of god filled jewelry but I don't know what the metal content of the jewelry is? If I saw the tubing into 1/4 inch sections will this be OK to use, only?
Question 2-I have a really long neck bottle, one of these that has been heated and stretched, if you have ever seen one? Will this work, probably 18-20 inches tall. Does the distance that the Noxx gases has to bubble through the water/peroxide make a difference. In your opinion how many inches of water/peroxide do I need in the condensor bottle? Percentage of %peroxide to %water? WIll the 3% peroxide from Walmart do the job or do I need to condense the peroxide?
Question 3- In the gallon pickle jar? How high up on the pickle jar reactor do I need to pour the sand up to? And just to veryify, keep 2 inches of sand beneath the jar while heating, is this correct?
Question 4- About how much nitric do I expect to condense from the quantities given in the instructions below. Also have you ever tried making twice the amount at one time?

Question 5 - This question has nothing to do with making nitric, but I am confused about driving off excess nitric in other solutions?
Temperature, when driving off Nitric acid from solution I can tell what temperature the solution is by when the solution boils with nitric in it? If I am trying to drive off nitric by evaporating, I must make the solution boil to drive off the nitric? Gradually lowering the temperature as nitric is being driven off, is this correct?
Question 6-Also, will a floating glass thermometer work here? If not what type thermometer do you use?
Butcher I hope to feel good enough to get started on this tomorrow or maybe the next. I still have a fever and feel weak but can't wait to get back to refining. Thank you for your continued support Butcher. I am going to send you a picture of my little angel's playhouse today if I can get the engery to go take the picture.
Thanks Butcher,
Oneal

Question
butcher said:
Oneal,
Below is one I posted, I really like it, one of my favorite’s actually I tried to explain this process I came up with, one on one of the first posts I made coming to the forum, I could not type then and was not very good at computers or the English and grammar, running all the sentences together (I may have gotten a little better now but sure you guys still have a hard time with my skills in this matter), I was a newbie, and had been lurking for a while before deciding to post, so I had an admiration of Harold, GSP, (Chris), Irons, Lou, and others, well I made my this first post trying to share my process, Harold chimed in saying he could not read a word I said, (man that hurt, I almost said to heck with this forum and quit then, but Ragbone chimed in, and calmed down my hurt pride, and I stuck with the forum trying to make my posts where Harold could read them), (Harold has taught me much not only in gold refining but in other walks of life, funny how a man who you have never seen, but you look up to can make such a difference in your life, never met Him but will always consider Him a friend and mentor
I also make nitric the cold method Laser Steve’s recipe, it is the best I have found (I have studied nitric intensely), this solution, works well for everything but silver (but you can distill it and then it is good for silver. So this is the method I suggest you begin with, there is also much information of this process here on the forum.

I have also made fuming nitric, but there is no need to make that or use that.
So 68% is the strongest you need (used in aqua regia), and more dilute to remove base metals and silver.
Always distill homemade nitric for silver.
I have made many posts on the properties of nitric acid, how to concentrate it, and its azeotropic nature, I will not go into that again now,
There are other processes to make nitric, I will not mention now, as it would just clutter this page.

I can process gold plated pins and make nitric acid at the same time here is my favorite process “Kill two birds one rock”, the principles here have many uses not only with the process stated here, and can be adapted to other processes.

You can use lab glass, distilling rig, but I still use my old pickle jar.

Process for pins, nitric acid and copper sulfate
Kill two birds one stone

A few principles:
You need sulfuric acid with nitrate (salts) to create nitric acid,
Gold will not dissolve in nitric acid alone,
Copper will dissolve in nitric acid evolving NO2 gas.
NO2 gas bubbled into water can form nitric acid.
NO2 + H2O --> HNO3
NO gas also evolves; oxygen will convert this to NO2,
NO + O2 --> NO2
So: if we add a little H2O2 to this we have oxygen and water, we can convert NO gas to HNO3,
NO + H2O2 --> HNO3

Gold will not dissolve in copper nitrate or copper sulfate.
Nitric acid will evaporate from a solution at a much lower temperature than a sulfate will.
2 NaNO3 + H2SO4 --> Na2SO4 + 2HNO3
Nitrate fertilizer + sulfuric acid àsodium sulfate + nitric acid.
In our case we are using copper to help.
Copper dissolving in nitric acid evolves NO2 and NO fumes.
Cu + 2 HNO3 --> CuNO3 + 2NO2(g) + 2 H2O
When we distill this copper nitrate we remove the Nitrate and leave the copper sulfate behind, diluting this to retrieve our un-dissolved gold.
Cu(NO3)2 + H2SO4 --> CuSO4 + 2HNO3
Copper sulfate is water-soluble.

(Copper sulfate solution we make here is soluble while hot, but will crystallize out as bright blue crystals if allowed to cool, (copper sulfate crystals once formed are harder to dissolve) than if we keep them hot while diluting the solution not allowing them to crystallize).

This is my method for pins (which can be adapted to distill copper nitrate solution to make nitric acid) or adapted for use with other chemicals and processes.

(This process can be adapted to other recovery or refining methods to kill two birds with one stone, like recovering nitric or aqua regia while dissolving karate gold)

A distilling unit rig (I have a nice lab distilling unit), but I like my homemade kit, and use it for this process, my unit has survived many distillations, but as with any distilling glass precautions must be observed,

Some supplies I use:
(My Pickle jar distilling kit)
Large pot with handles
Sand
Canning gallon pickle jar
A lid for gallon jar --made from 1/2" thick Teflon,(or the plastic wood they make decks out of HDPE I think) turned on a lath beveled edge to tightly fit jar, small lip on top edge, a hole in center for tight fit of 1/4" hose.
8' 1/4" Teflon hose
Long neck bottle
(For this bottle either loose fitting Teflon cork with hole or just use tape)
Gallon bucket of ice water
Double burner electric hot plate
(Ground fault protected electrical outlet)
Fiberglass catch tray for burner to sit on to catch any spill
Pyrex coffee pot
Some wire, plumbers Teflon tape, cloth tape, electricians black tape
New battery sulfuric acid 10 cups, (we will boil down to 6 cups)
Cup of sodium or Potassium nitrate fertilizer
One pound of (copper) gold plated pins no solder (cut to expose copper to acid)
(Teflon will withstand temperature and fumes of these acids)
(A nearby box of baking soda and water for safety)

Required:
Understand the dangers of these acids, and precautions to take, understand the danger of the nitrous gases formed, and precautions to take, understand the principles of distilling and precautions needed, understand glass cannot withstand thermal shock (rapid temperature change).

Never cool or lower temperature to boiling reaction vessel without removing line to condenser,(which can cause suck back of cold solution into hot boiling flask breaking it through thermal shock),always remove tube before lowering heat on boiling flask,

Work outdoor using breeze or with fume hood, take safety precautions.

Double hotplate sits on fiberglass catch tray; ground fault electrical source is used outdoors

10 cups of sulfuric battery acid boiled down to 6 cups in the Pyrex coffee pot on one burner boil down to 6 cups and cool. To boil off some water in the acid, it will still contain some water (We will use this cool sulfuric acid later),
(We could also pour concentrated sulfuric acid drain cleaner into water to dilute it).

The large pot, pour a couple of inches of sand in bottom of it spread flat, the gallon canning pickle jar is sits on this sand centered in the large pot and sand poured in between pots metal and outside of pickle jar, to make a boiling reactor with a sand bath. This will help to protect our glass from thermal shock, (sand bath around pickle jar), allowing heat to change slowly, and can act as catch basin if we make a mistake. The 1/4" Teflon hose fits tightly into Teflon lid for our gallon pickle jar boiling reaction vessel, we will be collecting NOx gas from this vessel, so hose just in through the lid just a little ways, to capture gasses formed in reaction vessel.
(Later we will tape on this lid, and tie it down)
(Get tape and wire ready and handy within reach, we will need it as soon as acid is added later)
Get ice water in gallon bucket (plastic ok) this is for cooling our gases and condensing them, our collection bottle will sit in this bucket,
Put small amount of water in the long neck bottle (collection bottle for condensed nitric acid) for NOx gas to bubble through water, (I add a little H2O2 peroxide to help conversion, it is not necessary), put one end of the Teflon 1/4" hose into this collection bottle all the way down into bottom of bottle so gases bubble through water and hydrogen peroxide inside, (through a loose fitting Teflon cork or else just tape hose to top of bottle, air, and some gas will need to escape from this bottle, and we do not want to prevent this with a tight fitting lid), this long neck bottle needs to sit down in iced water of bucket to condense gas to liquid, and we need to hold it down in ice water (it wants to float till it fills), so we tie in down into ice water bucket, this is our condenser receiver for the NOx fume's which will bubble into water in this longneck bottle and convert to nitric acid, a few loops of this hose is under ice water to help condense fumes also.

Set large pot sand bath with our fancy pickle jar boiler reaction vessel on cold electric hotplate, put one pound solder free (copper) gold plated pins, (cut to expose copper to acid I cut mine small for more exposure), in reaction vessel, add one cup of sodium nitrate fertilizer, (with lid and tape handy ready we will need to put on lid to contain brown NOx fumes in next step), pour in cooled 6 cups sulfuric acid on these, quickly put on Teflon fitting on lid and taping on the with Teflon plumbers tape first, then bandage cloth tape, then black electrical tape sealing this lid well, the insulated solid copper tie wire is tied to one handle of the pot over top of lid on jar and tied to other pot handle, this will hold down the lid when pressure builds,
As soon as you pour the sulfuric acid on the nitrate fertilizer and copper, red brown nitrous gas NOx begins to form, so getting lid on quickly and taping to seal is needed, we will need no heat yet, as it creates its own heat from chemical reaction, turning burner on warm will start to heat pot and sand, with time, the heat will saturate sand and starts to warm the jar. When reaction slows (bubbling in receiver slows) and pot is warm raise heat a little, (little bit at a time) giving time for heat to reach and react chemicals as red fume slow, or gas bubble slow in receiver, we want a steady few bubbles, not too fast we only want the gas to go to the condenser and receiver. (There is a point to where nitric will concentrate to azeotrope in the boiling flask and reaction begins to get more vigorous with red fume’s of NOx gas), keeping a steady stream of bubble into our receiver is our goal, not liquid the blue liquids from our boiling flask).

Caution we do not want to change temperature on glass fast, this thermally shocks glass and will crack or break it, always keep this in mind.
Do not lower the temperature of the boiling vessel, with the hose in the condenser receiver, always remove this hose from the receiver first allowing it to suck air, (this higher temperature in the boiling vessel creates a pressure, and if we lower the temperature on this boiling vessel, it will go into a vacuum, this will suck the cooler condensed liquid back into this hot boiling flask, thus causing thermal shock and cracking our jar, by removing this hose first it just suck’s back air, and not liquid, as the pressure lowers in this boiler reaction vessel.

(I preheat a coffee pot of water, just below boil for procedure below, starting the water heating before hand)

We do not want to evaporate this now forming copper sulfate to a dry salt, we just want to drive out the formed nitric acid, so we evaporate to thick syrup, (I have noticed a color change from blue-green to blue-blue as the nitrates are driven out of the copper sulfate),
After we have evaporated down to syrup.

NOTE:
We want to remove hose from the condenser receiver, before lowering temperature.
(See caution on suck-back of these cooler liquids when lowering temperature of reaction vessel, thermal shock),
We can let cool before diluting this copper sulfate syrup, but this will form salts and it takes more water to dilute, (that may be best for you as this step if not done properly can thermally shock your boiling vessel), I use the water we heated above (on second burner in coffee pot, getting this water to about the same temperature of this syrup, and very slowly adding this boiling hot water to the syrup to dilute it, starting with just drops at a time, not pouring in all at once, this dissolves the blue copper sulfate syrup and leaves gold shells and powder from pins.
Allow this dilute copper sulfate liquid to settle the gold, and then decant liquid from gold and filter solution.

These gold foils will need further treatment to refine to pure gold.

This copper sulfate can be evaporated to nice blue crystals of copper sulfate for other chemical reactions, or for an electrolytic cell or other uses, wall mart sells them at a high price to keep roots from growing in sewer lines.

This nitric acid tested for strength, and evaporated to 68% concentration azeotrope if necessary, cool, stored in amber nitric bottle with proper lid put out of light (light breaks down nitric). Store in safe place for later use in recovery or refining

Distilling copper nitrate, (adding copper or gold plated copper can assist creating NOx fumes in boil, which also is a way I get gold plating from Pins. killing two birds one stone) would get nitric back from this copper chloride solution, bubble NOx gas into water, for dilute nitric, which can then evaporate water from dilute nitric until 68%HNO3 azeotrope, (many acids form azeotropes), so if just evaporating a dilute nitric solution, below the boiling point of the acid (for the concentration that the acid is at the time in solution), would boil off water (or other volatile components if in solution), making the acid more concentrated in solution, up to the azeotrope of the acid, which for nitric is about 68%, further boiling would only boil off the 68% solution till dry, meaning it cannot be further concentrated by this method, by using the boiling point information a person can have a good idea if they are boiling off acid or just water, the concentration can be tested with specific gravity, or judged by how it attacks metals.

(100% H2O) boils @100 degC density 1.00.
20% HNO3 density 1.115- boiling point 103 degC.
30% HNO3 density1.180 boiling point 107 degC.
50% HNO3 density 1.310 boiling point 116 degC.
70% HNO3 density 1.413 boiling point 121.5 degC.

(Pure HNO3 boiling point is about 83 degC, so you can see the boiling point goes up as the nitric is less concentrated, till about 68% azeptrope (nitric acid’s highest boiling point about 120 degC), then as we get more dilute towards just water the boiling point falls toward the boiling point of water 100 degC).

As you can see the boiling points change with how concentrated the acid is. Keeping below the boiling point most all of your acid stays in solution, and mostly water vapors off, above the boiling point acid leaves solution in vapors with the water.
Other acids and have reaction similar to this. For more information you can study the azeotrope of acid, boiling points, acid concentrating, I have also posted this information on forum in other posts.

{Basically we made nitric acid with nitrate fertilizer and sulfuric acid, nitric acid distilled off in condenser bottle, the copper helping to drive the reaction, dissolved copper from the gold making copper nitrate in solution in boiling vessel, and since we had a slight excess of sulfuric when we distilled out the nitric fumes (making nitric acid ) we left sulfuric acid in boiling flask which forms copper sulfate solution, and gold foils, which we will dilute the copper sulfate with boiling hot water before allowing to cool so we can seperate gold foils from copper sulfate solution}.


I have added some points to this post today; here was the one posted and some questions answered about it,

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=38&t=6199&hilit=kill+two+birds+one+rock

Read and understand dangers involved before attempting, this method it is safe I have done it many times, but precautions must be taken, and dangers must be taken into account.

My hope is this is readable and understandable, and someone will gain information or it will spark ideas in others.

Butcher
 
Oneal-

I will let Butcher answer the bulk of your questions, but from everything I know you should not boil a solution to effect evaporation. Boiling may cause you to lose values, keep in mind that with any pregnant solution if small particles or mist manage to escape the container, any dissolved metals shall be included, and with a highly concentrated solution the losses can be substantial. For depleting nitric, I believe the very best method is what Harold advises, specifically to place a 24K gold button in the solution AFTER filtering during the final stage of AR to consume the excess nitirc. I myself have adapted this strategy when I am in a hurry, by using gold powder from a previous precipitation, and whatever does not dissolve simply contributes to the weight of the new batch. Either way you can weigh whatever gold is used to keep your yield calculations accurate.

In regards to a way of measuring temperature, I personally like a "point and shoot" infrared thermometer, and Harbor Freight Tools has one that is fairly inexpensive at $30 TO $40. Of course this reads surface temp and not the actual liquid, but still a great way to keep tooling out of the acids and very fast/easy to use.

Hope you feel better soon.
 
Question 1- I don't have any gold plated pins, but have plenty of copper tubing. I have plenty of gold-filled jewelry but I don't know what the metal content of the jewelry is? If I saw the tubing into 1/4-inch sections will this be OK to use, only?

ANS.
The process killing two birds with one stone, making nitric acid and removing gold from pins is best used when you have gold pins to process, it would work using copper but in my opinion unless you needed copper sulfate, it would be a waste of material, time and trouble, to just use this method to make nitric unless your de-plating gold from copper,

In this case I would use Laser Steve’s poor mans cold nitric recipe, following all of its instructions and then distill the nitric acid if usinit for silver.

Dilute nitric acid can be concentrated to 68% by evaporation, but for most processes we dilute nitric any way.
Question 2-I have a really long neck bottle, one of these that has been heated and stretched, if you have ever seen one? Will this work, probably 18-20 inches tall. Does the distance that the Nox gases have to bubble through the water/peroxide make a difference. In your opinion how many inches of water/peroxide do I need in the condenser bottle? Percentage of %peroxide to %water? Will the 3% peroxide from Wal-Mart do the job or do I need to condense the peroxide?

ANS
You only want as little water and peroxide as possible, if your using 35 peroxide I would only use that without water as it already mostly water, the longer the bubbles stay in solution the better the gas and water convert to nitric acid, but then the more water you add the more you dilute the nitric acid, starting with as little water as possible in receiver, that the gas has to bubble into in my opinion is best, as the very first portion to distill over will add water to your receiver as time goes on the bottle fills there is more solution for the gasses to bubble into, when making several batches I will use previous batch of nitric which gives me more volume of liquid for bubbles to flow through, also a dilute solution of nitric can also be used to bubble the NOx gases into to some what concentrate the dilute solution and convert NOx gases into more nitric acid.


Question 3- in the gallon pickle jar? How high up on the pickle jar reactor do I need to pour the sand up to? And just to verify, keep 2 inches of sand beneath the jar while heating, is this correct?


ANS
A couple of inches of sand for jar to sit on and I would put sand almost up to level of the solution in jar, the height here is not that critical, you just do not want jar to touch sides of pot and create hot spots, also being able to see the reaction in jar is nice feature.
Question 4- about how much nitric do I expect to condense from the quantities given in the instructions below. Also have you ever tried making twice the amount at one time?

The distilling (boiling reactor need room for expansion of liquids, foaming and so on you do not want to fill the vessel very full, and have solutions boil over into your condenser, the ratio’s I gave for the pickle jar worked well for me, after many experiments these seemed to be best proportions for this.
If your distilling just nitric acid I would say keep the solution less than one third volume, the more room in vessel for expansion and foaming the better.

Question 5 - This question has nothing to do with making nitric, but I am confused about driving off excess nitric in other solutions?
Temperature, when driving off Nitric acid from solution I can tell what temperature the solution is by when the solution boils with nitric in it? If I am trying to drive off nitric by evaporating, I must make the solution boil to drive off the nitric? Gradually lowering the temperature as nitric is being driven off, is this correct?

ANS
No need to boil, if you see some fumes coming off solution when heating these fumes are forming gases from liquids in solution, vapors of liquids will vapor off way below a solutions boiling point, as the solution concentrates the boiling point of solutions also change (as will the point of evaporation),

Nitric acid in solution once the solution concentrates in the evaporation dish will get to a point where the nitric wants to boil over all of a sudden (when getting concentrated I pay very close attention watching for the very small bubble that form on outer edge of solution these small bubble give me the clue I am at this point of boil over, lowering heat at this point and having my mist water bottle handy to mist with water saves me from boil over at this point (after this reaction completes I can usually raise heat back to where I get good evaporation of gas fumes and do not have to worry about boil over again.

Question 6-Also, will a floating glass thermometer work here? If not what type thermometer does you use?


ANS
I normally do not use a thermometer, but when I do just to see what is going on I use an infrared thermometer, it allows me to just point at several places and see what temperatures they are (thermometer in not necessary but can be nice feature).

Butcher I hope to feel good enough to get started on this tomorrow or maybe the next. I still have a fever and feel weak but can't wait to get back to refining. Thank you for your continued support Butcher. I am going to send you a picture of my little angel's playhouse today if I can get the energy to go take the picture.


We hope you get to feel much better soon.


Edit to help clarify a point:
When distilling we do boil a solution to form gases capturing the gases, but we do not want to boil to the point we get carry over of the solution that will contaminate or receiver vessel with substances we are trying to leave behind in the boiling reaction vessel.

When evaporating a solution to concentrate or to remove one component as a gas, we do not want to boil only evaporate the solutions, heating to the point of gases rising (fumes) from solution, very small reaction bubbles are ok, but these are different from large popping bubble’s of a boiling solution.
 
Hi Everyone, thanks for the clarifications on the nitric production.
I have another problem now. I felt good enough to go over to the old house last night. I had a batch of AR ready to evaporate and finish up. I evaporated down to syrup, added Hydrochloride a couple of times, evaporated off then added a few drops of sulphuric for the last evaporation. Added 4 times the amount in distilled water and left to sit overnight. It got down to 31degrees F. last night, very cold for here. Anyway, I went over just a while ago and added the Sodium Metabisulfate (Stump Out). I used warm distilled water to dissolve the Sodium Metabisulfate. I added 4 teaspoons not wanting to come up short because this was my largest refine yet. I added maybe 1/4 of the Sodium Metabisulfate while stirring vigorously and nothing happened, I added more and the AR turned dark brown. Just like it did with my first refine. I thought I would see the gold droping out of solution. The gold drop never happened? I added the remaining Sodium Metabisulfate and still no drop. Thinking that my AR may be heavy laden with gold causing this, I mixed up another batch of Sodium Metabisulfate and poured in about 1/4 of it still stirring vigorously. Nothing happened, I poured in another 1/4 and still no drop. I have gold floating on top of solution and in solution but not dropping. The floating gold powders flock together for some reason? My solution was very cold, probably near freezing 34 Degree F. I was adding warm/hot Sodium Metabisulfate to the near freezing gold bearing solution. Thinking that I had put more than enough of Sodium Metabisulfate in to do the job I stopped and came in. So this is where I am at, a beaker full of Sodum Metabisulfate, Approximately 6 teaspoons in 800ml of fluid. Brown colored liquid that will not settle out.
Question 1- Where did I go wrong and how do I correct it? Did I not get all the nitric out of the AR solution last night or did I have left over Hydrochloric and or Sulphuric that caused this?
Question 2-Should I have warmed the AR before I tried to drop the gold?
Question 3- I expect I have near 1/2 ounce of gold in this batch so I sure do not want to lose it. To correct this do I evaporate off all the Sodium Metabisulfate, down to powder and start over again? I can't figure out why the gold will not drop out of solution with more than enough Sodium Metabisulfate to do the job.
Question 4- If I evaporate off all the liquid, I still have the Sodium Metabisulfate in with the gold now, right?
Thank Everyone for your help, it really is appreciated.

NOTE! UPDATE, I went back over to the building. It had been about 2 hours or so. The Gold powders are starting to drop, the solution isn't clear but I can tell that the gold is droping out of solution. The scent of Sodium Metabisulfate is very strong in solution. I really don't think that I didn't put enough to do the job? By morning I suspect that all the gold should be droped but I still have the floaters. I stirring the top part of solution to try and get some of the floating gold to drop. I had some success with this but some refuses to drop from top of solution.
I thought I would wait untill morning to test solution with stannous chloride. The solution looks funny, not like the first gold drop I did. I have brown powders sticking to the sides of the vessel, especially at the level the solution is at (top). I washed and cleaned the vessel very good with Dawn detergent before I decanted the solution so I had a clean vessel. Still don't know what happened?
Thank you so much for your help.
Oneal
 
Oneal,
You may go out later and find the brown powders settled (maybe with excess SMB), if not I would try adding just a little HCl and a good boil then let it cool and sit overnight see if that works to precipitate the gold, if nothing else you can use cementing on copper to recover the gold.

Did you filter before precipitation?
If it filtered easily tin is not your trouble.

Was solution a nice yellow, or at least yellow with just a hint of green, if so base metals are probably not your trouble?

You may have had low acid content in the gold salts?
Or may just have not given enough time for the reaction to complete under the conditions?
 
Hi Butcher,
This was the second run on the AR. What I mean is that I had already added Hydrochloride and a few drops of sulphuric to the AR. Then distilled water and let sit overnight. The next morning I had a good bit of either tin/silver or lead in the bottom of the vessel after the first evaporation. So,this concerned me, I then decided to go back through the process again because of the amount of tin/lead I had from the first run. I was afraid I had tin/lead that carried over. So, I went back to the batch to make a second run/evaporation which was last night. This morning I only had just a little dusting of tin/lead in the bottom of the vessel. I had a nice clear yellow solution, much better than the first evaporation. The solution filtered about as fast as I wanted to pour it. I couldn't see any particulate in the second solution and was pleased with the result. I was expecting good results because of all the steps I had been through with this batch.
Question 1- Can you overwork a batch of AR? I mean doing what I did instead of going ahead and dropping the gold the first time and then refine again. Which should I have done, just go ahead and drop after the first evaporation and do another refine or do what I did. What concerned me was seeing all the tin/lead or silver that had dropped out of the first AR. Did I overwork the solution taking the gold salts out of solution?
Question 2- I have went back out and taken another look at the solution. The solution is nearly clear now. Will it hurt to leave the Sodium MetaBisulfate in the vessel overnight. Will any of the Sodium MetaBisulfate crystalize out in the cold tonight or will it stay in solution?
But I did add Hydrochloride many times, not just 2 times. Probably 4 times, I wanted to make sure I got all the unwanted metals out. I added sulphuric a couple of times also.
So, I guess the big question is, did I cause this due to going through too many steps to clean the solution? Should I have just went ahead and dropped the gold on the first evaporation and then just do another refine on the gold button instead of doing what I did?
Which would have been the quickest and easiest to do?
Question 3- Is there a sure fire way to tell when you have depleted all the nitric out of a solution short of dropping a pure gold button into the solution? If not, when you drop a pure gold button into a solution will you be able to tell if the nitric is spent because of no reaction at the button? Or do you just leave the button in overnight to be sure all the nitric has been depleted.
Question 4- Puzzled, if nitric will not dissolve high karated gold unless inquarted to around 75% silver, why would you put 24K gold into it (nitric) and expect a reaction? I have not refined any karated gold yet but am puzzled by this?

Thanks Butcher for your time and help.
Oneal
 
Oneal.
I am unsure what you mean can you overwork a gold solution.

Lets say we had a jar of water and we added salt, until we could no longer make salt dissolve, now we evaporated one of the volatile components in this solution (water), until we made a syrup of salt water,(note the salt like gold in our solution does not leave on evaporation),now we can add back water and redo this as many times as we want (unless we boiled too strongly and splashed some salt out we would still have as much salt as we started with.

Now our solution of gold similar to this salt water above except we have three components (besides mixes of these forming gases), water, nitric, and HCl, and in this order are they volatile in solution (not that they will evaporate as pure substances but the fumes of evaporation will mainly be composed of on of these in this order).

The way whisky is distilled the first distillation is more "rich" in the volatile gas,(higher proof) and if we condensed this gas(alcohol) (and did not drink it), and then redistilled it we could get higher proof the second or third time of condensing and redistilling, this same alcohol, (each cycle) a higher alcohol in condensate and less water is in fumes each cycle, and each cycle leaving a richer solution of water behind in the boiling vessel.
Also on the first run distillation the alcohol content is higher the first portion of gas in the beginning of the distillation, as the alcohol is distilled from the boiling pot the boiling point of solution also changes, and more water also vapors over with the later portions being distilled.

So when we evaporate out aqua regia the first fumes are higher in water content, as we proceed the fumes become higher in nitric, and upon concentration the fumes become high in HCl, but as we said these gases do not come out as pure substance and we may still have some nitric in our gold chloride syrup (some of this may have made nitrate salts I'm not sure), adding HCl we replace some of the HCl we may have boiled out from concentrating the solution (remember we are making a gold salt chloride that needs the Cl- from our acid with the Au+), (also the acid may help to change any nitrate salts forming back into HNO3 in solution) (which may be why we may see NOx brown fumes on addition of acid to the concentrated solution of gold salts, I am just guessing here), this also helps to keep solution acidic, and gold in solution as salts, also the HCl is 20%acid and 80%water so here we also diluted our gold salts (and also diluted any remaining nitric in solution).
So you can see we do not need to add high volumes of HCl after we do the first evaporation, adding excess HCl just means we need to evaporate off more water before the remaining nitric comes over again. Now with some more evaporation of this thick syrup wetted with some HCl evaporates off water mostly at first the after most of water is evaporated the fumes become more rich in remaining nitric then HCl. after this we add HCL to wet and repeat.

Evaporation would not be needed three times if we did not use too much nitric when we first dissolved the gold, we may get by with one evaporation, or using a little excess precipitant to overcome the small amount of excess nitric acid in solution,

If only we just listened to the great advice of GSP, His advice of only using the amount of nitric needed to dissolve gold in the beginning.

Harold's trick of using the gold to remove excess nitric in aqua regia evaporation, here the nitric does not dissolve the gold, but if we have free HCL and free nitric in solution it will gobble up our gold button, if we did not have free HCl the nitric in solution would not touch the gold button much, or if we did not have any free HNO3 but had plenty of free HCL in the gold salts on evaporation you would not attack the gold button, mainly remember one of these acids alone do not dissolve gold but the combination of both of them will, also remember that excess HCl in the gold chloride salt does no harm, and can actually be a benifit (like when in the precipitation stage).

It is my opinion that other metal salts in solution can give troubles when precipitating gold, tin being one of the worst (forming gold colloids that stay in solution and will not come out.) even copper in higher quantity will lock up gold in the solution with copper, and the copper not releasing the gold from its bond, the purer the solution of gold chloride (without free nitric acid to redissolve the gold), the better and easier will be the precipitation and purer the gold powders.

get rid of trash early in the game, (trash in is trash out), or troubles getting back your gold.

Not sure if this helps or confuses you more?

I know your using your stannous test to tell if you have all of gold out of solution.

If you end up with SMB (from excessive use) you should be able to rinse these out of powders later, may just take you more rinses.

From your statement it is looking clear (assuming your talking of color, and not turbidity) then sounds like gold is precipitating, did you have to boil?
Or was just waiting letting it sit to precipitate that brown powders?

color of the powders after washes, are also an indicator if they will need refined again for high purity.

Glad to see you feeling good enough to brave the cold weather, I guess this hobby is motivating you to get out of that sick bed.
 
Hi Butcher, I just got back in from running the making gold pure process that Harold advises to do. I ran another HCL boil, dilute/decant, rinse/ repeat. I then added the ammonia hydroxide boil/dilute, rinse, reapeat and a final HCL boil, dilute, rinse/repeat. Checking decants with stannous. I dried gold powder that turned out to be granular in structure. I dried the gold, and came out with a very good looking button. I didn't drop this one and ended up with a nice looking clean button. One more run of this size will give me a troy ounce which I have already found a market for.
I am at the beginning stages of understanding what you are saying about the chemicals and the parts each play in this process of refining. Trouble is, the more I understand the more I realize how little I know about them. I followed each and every thing you explained in your previous post. I see now instead of concentrating so hard on turning out good quality refined gold I need to make myself knowledgable about the chemicals I will be using as well. At first I didn't see why I needed to know about the chemicals, not in depth anyway. My thought pattern was on turning out the gold, my thinking was to just give me the amount to use and directions to put it to work and don't worry about what's happening during the process. But I am beginning to understand now that I truely need to study the characteristics of these chemicals to fully understand what is happening when I do the refine. Any quality refiner needs to know this part of the process, that I hope that I will be one day.
Butcher, thank you so much for your mentoring me. I just don't know where I would be if you hadn't found me. Proably still struggling on the first refine. Thank you so much for your patience and ability to teach common folk that aspire to do greater more technical things. It really is appreciated, You are appreciated, I just can't say this enough.
Good night Butcher, it's bedtime here in on the East Coast. I am running on empty now. Talk to you tomorrow Butcher, hope you have a restful night.
Oneal
 
Oneal.
I am just a parrot, spitting out words I heard from others on this forum the thanks really goes to them.
I know your well on your way to becoming a good refiner.
good night.
 
Hi Butcher,
Should I evaporate my sulphuric acid down to make my (poor mans nitric)? I have read on some of the post that if you evaporate off about 60% of the sulphuric (drain opener)to fumming sulphuric you will get stronger nitric when making nitric. Is this correct? I didn't want to do this until I checked with you.
Also, I have used copper busbars I have accumulated through the years. Heavy gauge busbars for 3/0 and 4/0 wire. Will these do for the copper? Does the amount of surface area of the copper exposed to the Potassium Nitrate make a big difference? When copper hit near $3 a pound a while back I sold a good many of what I had but still have some left.
I have .925 sterling silver I want to refine, so I will need to condense some of the nitric I make. Would like to make it as strong as I could to start. I know that you have said the best I can do is about 68% without using a condensing unit. But I do have the set up to do this with, just that I am not ready to start on the sterling silver right now. Plus the 68% nitric will do just fine right now until I get through all the gold filled I have. I am going to triple the amount of the refine this time. I need to start processing larger lots so I need to get the nitric made.
Thanks Butcher for your continued support.
Oneal
 
Rooto stump remover is about 98% sulfuric from what I’ve been able to ascertain. I’ve never refined any silver, so I really don’t know what it would take to do that job. Most lawn and garden shops will have this product. Seems a waste to have to evaporate battery acid down to accommodate your needs.
 
The Rooto you can get at the store is 93.2% pure to be exact https://www2.itap.purdue.edu/msds/docs/12070.pdf. At 98% it would be the dark brown to black stuff. Even more dangerous than the lower percentile stuff.

You will be hard pressed to make poor mans nitric that can dissolve silver. Usually too many nitrates are left in solution to effectively digest the silver. You would have to distill your nitric to get a better quality acid capable of digesting silver. Distillation comes with a whole other set of safety issues and concerns though.
 
Thanks fellows for the information on the sulphuric. I will go take a look at the Hardware Stores tomorrow, (rooto).
I watched a video on how to purify potassium nitrate fertilizer, it envolved dissolving the potassium nitrate fertilizer in hot water and then letting it settle out the impurites that sunk to the bottom of the container? Then decant only the clear liquid off the top. The video didn't get into how to get the liquid back into a solid. I guess that would be just to put it outside and let the water evaporate off, leaving the solids behind. Or putting it in the freezer and letting it freeze, pour off the liquid and collect the crystals. I have seen 1 method that did this.
Also I couldn't find Potassium Nitrate or Sodium Nitrate fertilizer when I first started with this endevor 2 months ago. The ammonia nitrate fertilizer I have until I know for sure how to handle it safely. Is there a method to take the ammonia out of ammonia nitrate fertilizer. Leaving only the nitrate salts behind? I have some ammonia nitrate fertilizer that I would like to make use of but am somewhat afraid to mess with it having the knowledge or lack of it right now?
Thanks in advance.
Oneal
 
Poor man cold nitric acid, the very famous post by Laser Steve see below.

There are many way's to make nitric acid but this is the best method in my opinion for making nitric acid.

Steve done an excellent job figuring the proportions and solubility,
I tried to make it 68% before, using a little less water than his recipe, but found it was harder to get rid of salts, (the 50% nitric from this recipe works great as is, or can be concentrated up to 68% if wanted through evaporation (not boiling, just heating till fumes vapor off), and (can be distilled and purified for use on silver easily).(the sulfate salts do not react with gold so with gold distilling is not needed).
Many things we need about 35 to 40 % nitric acid like silver, or to remove base metals, and 68% or less for aqua regia.
(I do not want to confuse anybody, but if you note in the recipe Steve gives in link below he adds water and concentrate sulfuric acid (you can use a less concentrated sulfuric acid in the recipe, just figure in the water contents involved).

(http://goldrefiningforum.com/phpBB3/viewtopic.php?f=49&t=315&hilit=concentrate+nitric+acid&start=20#p2572

If you are using nitric acid for silver it will need to be distilled, (boiling of gas fumes and condensing them), this will leave the sulfate salts formed (sodium or potassium sulfate salts), behind in the boiling vessel and will give you a purer nitric acid product (as long as you did not produce carry over too hard of boiling or bumping, of solution in your distilling rig.

The problem with using home made nitric without distilling on silver, is that silver will form sulfates easily, silver sulfate is only very slightly soluble, something like 55g in 100ml H20, so you would loose much silver to become silver sulfate powders, these are also more trouble to convert back into elemental silver before melting, so basically if working with silver and home made nitric distill your nitric first.


Distilling is really not hard at all, all you are doing is boiling a solution, capturing the gases and condensing them back into a more pure liquid, leaving the impurity in the boiling flask. As you can see in the post above I made a distilling rig out of common household things, you can get a lab-glass distilling rig for about 60 dollars on up, as hard and expensive as nitric is and if you do much with nitric it will pay for itself.

You can make concentrated fuming nitric, but it is dangerous and not needed for what we do. And I will not say how to make it here because it can have illicit uses.

nitric acid has an azeotrope of about 68%, this is the strongest you can make it using the cold nitric method, or if is made much weaker, this is the strongest you can get it by evaporating off water, but this is the strength you normally buy it at, and it is the strongest we would need to recover and refine with.

Acids strength can be tested by seeing how it reacts on metals or by measuring specific gravity of the acid.

you can make nitric acid out of ammonium nitrate fertilizer, but if not done right in can be very dangerous, so I normally will tell people on the forum do not do it is too dangerous, as I would feel terrible if I told somebody how, and a distilling rig blew up in their face.

Sodium nitrate works great and can be found easily as a fertilizer, you can even order sacks of this from garden suppliers on the intranet, potassium nitrate found as sump remover is easy for me to find (Lots of stumps around here), and it works great also.

Save the sulfate salts byproducts from making nitric acid, I use them to make several other chemicals, (or for fusion) in my refining lab.
 

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