evape of excess HN03 add hcl.. no color change

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Actually gold chloride is a salt of gold, the gold we see dissolved in that yellow solution could be evaporated to crystals of gold salts.

Metal + Acid = salt of that metal.
Example:
Copper + HNO3 --> copper nitrate salt {dissolved in a solution, the cation copper ions, the anion nitrate ions}

The solution or salt could be high in NaCl depending on the process, and taste like table salt, but you could have other base metal chlorides involved depending on the source, many of which can be poisonous, and may not taste much different from the salt, not a good idea to be tasting.
An old method of testing an unknown was touching a dab to the tongue, acid would bite the tongue, but nowadays we have much better testing methods, and more common sense than to be tasting our solutions.
 
I was using evaporation as a denox process until when I read somewhere hear with controlled nitrate additions during gold dissolution, then at the end add urea until no fissing. It works very fine and I was served from that tedious evaporating process.I use that everytime and get instant drop with Smb. So fot your case if you have urea at hand which is normal fertilizer toss 5 to 6 pellets into your solution and watch if no fissing then be sure no free nitrates from which you can proceed to dropping. I can't explain in detail the chemistry behind but after I read from here tested and it works, serves labour and time.
Regards,
Esau
 
even though the use of urea is commonly accepted and widely used, its normally not recommended because it just adds another chemical to the mix. if you follow good work habits when putting metals into solution, you shouldnt have to remove free nitric in the first place.
 
Esau Nisalile,
Urea is not a good idea, in my opinion, actually a very bad idea, as far as I am concerned, it can add contaminates, it can form ammonium nitrate (an explosive mix) which under some conditions could be very dangerous (especially with heated glassware being so close to our face, the urea can also form ammine in solutions the ammine compounds can complicate platinum group recovery (if involved).

Sulfamic acid will work better if needed, as its byproduct is sulfuric acid which has the benefit in solution (can help when evaporating to keep from forming salts if the process carried too far), (and will precipitate lead from solution as an insoluble lead sulfate), sulfamic acid can be found as a grout cleaner for tile grout (found in the flooring section of the hardware store near where I live).

Harold's trick of adding a button of gold to use up excess nitric acid, with heating, is a great way to remove excess HNO3 from solution.

Knowing How much acids to use for each gram or ounce of gold, and adding the nitric measured in small increments, using heat to drive the reaction and dissolve the gold, using up the added HNO3 before adding a bit more to insure excess nitric is consumed in the reaction, is the first step to not using too much nitric or having to eliminate it later in the process.

Leaving a little bit of undissolved gold behind in the reaction (works similar to Harold's method above), this little bit of gold can be added to the next refining process.

4 fl. Oz. of 32% HCl and 1 fl. Oz of 70% HNO3 will dissolve a troy ounce of gold (31.103 g Au).
Using the formula above from Hoke's book we can figure from this:
118.29 ml HCl + 29.57 ml HNO3 per Troy Oz of gold.
3.8 ml of HCl and 0.95 ml HNO3 per gram of gold

With this, lets say I have 10 grams of gold powders recovered and I wish to refine them, I can cover them with 38 ml of HCl (I may add just a bit more no harm), set this on a mild heat, then measure out 9.5 ml HNO3 in a clean vessel, using a pipette I can add only a few milliliters of HNO3 at a time, waiting for the reaction to complete before adding more, heating the solution also speeds the reaction, but also concentrates the acid, as it evaporates the water added (involved in acids and the water produced from the reaction), this is actually concentrating and evaporating my solution as I work, we just do not want to heat too hard, or we could vapor off the needed HCl in solution. We may not need all of the measured nitric to dissolve our gold.

At this point after the gold has reacted, we can leave a bit of the gold undissolved for the next batch, or add a gold button to consume any free HNO3 (if we used more than needed), we can continue to concentrate the solution through evaporation, getting the solution concentrated, (here we normally add a few drops of H2SO4) but we can add a little sulfamic acid for the same purpose, which will also work to eliminate free HNO3, after concentrating we can cool the solution down with three to four volumes of water, let it sit overnight to precipitate silver chloride and lead sulfate..., and filter the clear bright yellow decanted solution before precipitating the gold with our choice of chemical precipitant.

Although not all of these methods are needed to eliminate free HNO3, using a combination of them for me insures I do not have problems with precipitating the gold, because of excess nitric in solution.

A trick I use is the stannous chloride test of the gold solution before precipitating gold, getting a positive purple of Cassius reaction, lets me know the stannous chloride can reduce the gold to metal colloids, this is a good indicator free nitric acid has been eliminated from the gold chloride solution, and thus my chemical precipitant (such as sodium metabisulfite) should not have problems reducing the gold ionic salts back to elemental metal gold powders and precipitate my gold.
 
butcher said:
A trick I use is the stannous chloride test of the gold solution before precipitating gold, getting a positive purple of Cassius reaction, lets me know the stannous chloride can reduce the gold to metal colloids, this is a good indicator free nitric acid has been eliminated from the gold chloride solution, and thus my chemical precipitant (such as sodium metabisulfite) should not have problems reducing the gold ionic salts back to elemental metal gold powders and precipitate my gold.

Sorry Richard, but I just can't agree with that. Recently, I mentioned that one of my gold dissolving processes used a solution of 50% (v/v) nitric plus water and a little HCl. After precipitating the gold, I tested for gold in a spot plate with stannous chloride. I used 1 drop of sample and 1 drop of SnCl2. The purple/black appeared immediately but then quickly disappeared. To a clean cavity on the spot plate, I then added a drop of sample, 4 or 5 drops of water, and a drop of SnCl2. This time, the color formed and lasted for a very long time - hours, maybe. The free nitric was still there but it was diluted to about 5 - 10%. In the dissolving of the gold in this case, very little nitric was consumed, 2 or 3%, maybe. I did this test on that material 100s of times. Try it.
 
I have run maybe only 6lbs of ceramic cpus using poor man's AR and I have never had to add urea, I don't even have any on property. Jeff has given me the best advise when I started and that was to just add small additions of the nitrate and wait till exhausted. By doing the process this way I have never had to use urea and don't think I ever want to. Thanks again to all the members here you have made my short time of refining great and now will be a hobby of mine forever. I have gold fever!!


Thanks
Tyler
 
moose7802 said:
I have run maybe only 6lbs of ceramic cpus using poor man's AR and I have never had to add urea, I don't even have any on property. Jeff has given me the best advise when I started and that was to just add small additions of the nitrate and wait till exhausted. By doing the process this way I have never had to use urea and don't think I ever want to.
For the record, the concept of adding nitric in small quantities has been promoted from the outset by GSP. It's a wise method of limiting free nitric, but isn't always the best solution to the problem, depending on the nature of the material being processed. I offer you, as an example, filings from the jeweler's bench. They typically contain substances that do not dissolve (often abrasive bits), and are not easily discerned from filings, so to guarantee that all of the gold is recovered from such material, a slight excess of nitric is desirable, as it ensures that you leave nothing of value behind.

In instances such as this, evaporating to eliminate the free nitric isn't necessary, assuming you're willing to add a button of gold to consume the unused nitric. It's the best of all worlds.

In all of my refining career, which lasted more than 20 years, urea was NEVER used.

Harold
 
Thank you GSP, I will do some more getting acquainted experiments with various additions of HNO3 to a gold chloride solution and testing with Stannous chloride, to get more familiar with that reaction, and how of various amounts of nitric or or dilution effects this test.

I have noticed before with small amounts of free nitric in solution the immediate violet reaction disappear as the gold was re-oxidized back into solution, and I have also noticed with more nitric in solution the stannous chloride would not show a reaction even with gold in solution.
 
Harold I keep a few grams of dried gold flakes from some fingers and I always drop 1or 2 in to see if they dissolve. Now I know there are BMs in these flakes but the small amount I add will be nothing that isn't washed out at the end. Like I said maybe 1 or 2 flakes from some fingers just to see if there is free nitric. So I guess you could say I kind of do what what has been mentioned here. Now that I have melted my second button though, I am going to use that from now on to use up any free nitric.

Tyler
 
I have used the incremental additions of nitric method for more than 30 years and I introduced it to the forum in the early days, as Harold said. I kept pushing it and it took about a year before it finally caught on. I think Lazersteve was the first to adopt it. Now, most people on the forum use it.

When using this method, although I am careful, I probably always end up using a little extra nitric and I believe that anyone using the method will also end up with a little free nitric in the solution. I don't worry about this because I know that it will be eliminated by the sodium sulfite or SMB (I prefer the sodium sulfite, but the SMB is slightly stronger). To eliminate 1 ml of 70% nitric, it takes about 1.5g of SMB, or a little less, if I remember right (that's 3.3 pounds of SMB per liter of nitric). However, if you try to neutralize too much nitric with the SMB or sodium sulfite, there will likely be reaction-products and solubility problems and undesirable crystals can form. Please note that it doesn't take very much to be "too much." The use of SO2 gas will reduce these problems somewhat and allow a greater amount of free nitric to be present.
 
Thank you GSP for all your contributions! I have also always felt that way that there has got to be a little free nitric just simply because what are the chances it is totally used up and all metals are in solution. Seems to me that you would have to have a little extra or not enough and we all know not enough is no good. I always add a little extra SMB to make sure that the free nitric would be used up as the gold would drop then go back into solution and drop again until it's used up. But as stated earlier by following your method there is very little free nitric so one addition of SMB is all I have ever had to do.


Thanks
Tyler
 
Since the reaction of nitric acid produces NOx that can be oxidized and reabsorbed in the solution it is really hard to give an exact amount of nitric to use. I dissolved 50+ grams of gold a couple of months ago, I started with all the 150 ml HCl needed but only half of the nitric needed (25 ml). The temp was a bit low around 10C, doing it outside, but without any reflux... almost all gold dissolved. In the end I heated the solution below boiling until I could see no additional reaction. I poured off the gold chloride and added new fresh HCl and a little bit of HNO3 t dissolve the last part.
In the end I had dissolved 50-53 g of gold in 28 ml HNO3 and 170 ml HCl. I now have 200 ml beautiful orange solution (water added during filtration).
I will add some water to precipitate silver chloride and then filtering it again before final drop.

I was very surprised of how little nitric acid I needed, the slow process and cold weather must have reabsorbed the nitric oxides.

When coming to the end of dissolving some gold, the acids are very weak, diluted in a lot of liquid and the surface area of the gold left is a lot smaller. Then it can be faster to pour off what you have and just add small amounts of fresh acids. The strength goes up and there is less of a risk of adding too much acid.

Göran
 
Hello
thanks gsp,harold,butcher

I have also never used urea
With poor mans A/R it is a little more difficilt
I use potassium nitrate as my nitre

This all came from a few months ago
I do not add to much nitre now

For the record I have dropped gold when stanmous
showed no color at all
And I have still a solution of beautifull golden yellow
That turns purple instantly but has no gold( I just can't
Seem to get rid of it) :lol:

Goran that's the same method I have been using
Thanks steyr223 rob
 

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