precipitating gold

Gold Refining Forum

Help Support Gold Refining Forum:

This site may earn a commission from merchant affiliate links, including eBay, Amazon, and others.
i may be wrong about this, but you may have to precipitate all values and start over.not sure how much you have invested in this batch but i do understand that silver in AR is not a good thing.sounds like you may have a do over.copper should cement all values out,filter, then follow with a HCI bath to remove excess copper and tin.boil your sludge thats left in water and rinse then repeat the boiling water rinse about five more times then wash with dilute nitric to remove silver and palladium.you should have a workable material to use your AR on and may have a more favorable outcome.
 
(If tin is your trouble), Inceneration to oxidize tin and HCl works wonders for tin, without it your asking for trouble with metastannic acid.

edit: some thoughts on adding sulfuric to help eliminate nitric, the only way I see this is benificial is that the sulfuric will act as a dehydrator, keeping water (behind in the pot)the water that would normally need to be evaporated before the nitric would come over, this is one of the tricks when distilling nitric acid, I do not use this method for eliminating nitric from aqua regia, so I cannot comment on how effective it would work, although a few dropps of sulfuric work very well to precipitate the lead as chloride.
 
butcher said:
I see this is benificial is that the sulfuric will act as a dehydrator, keeping water (behind in the pot)the water that would normally need to be evaporated before the nitric would come over, this is one of the tricks when distilling nitric acid...

What do you mean by a trick? I'm curious because I distill some of my own nitric. I'm always looking for pointers in all of our processes.
 
goldenchild said:
butcher said:
I see this is benificial is that the sulfuric will act as a dehydrator, keeping water (behind in the pot)the water that would normally need to be evaporated before the nitric would come over, this is one of the tricks when distilling nitric acid...

What do you mean by a trick? I'm curious because I distill some of my own nitric. I'm always looking for pointers in all of our processes.
when making nitric acid by condensing,especially if your using muriatic acid,water will boil off first.i always test with a piece of copper as it drips to assure its acid and not water dripping out of my apparatus.
 
I don't use water when distilling nitric. Only sodium nitrate and H2SO4. This will produce red fuming. If you want to cut your nitric to 70% during distillation, the calculated amount of water is added to the receiving vessel. I would not recommend that because if your drip rates gets too fast the receiving vessel will get very hot. Bad things can happen when glass vessels get too hot too fast. How do you use HCL to produce nitric? That will produce AR.
 
goldenchild said:
I don't use water when distilling nitric. Only sodium nitrate and H2SO4. This will produce red fuming. If you want to cut your nitric to 70% during distillation, the calculated amount of water is added to the receiving vessel. I would not recommend that because if your drip rates gets too fast the receiving vessel will get very hot. Bad things can happen when glass vessels get too hot too fast. How do you use HCL to produce nitric? That will produce AR.
i was referring to the method of dissolving copper using sodium nitrate and HCL to create nitrogen dioxide gas.its not a very good method but it will make a workable nitric acid.
 
Ahh ok. I saw something like that on youtube. IMHO, no matter how you do it, I feel you will always get AR if HCL is in any part of the equation. Think about when you dissolve base metals in AR. There are always the red fumes and the effervescence from the HCL (lots of effervescence if the reaction is vigorous).
 
Thanks for clearing up the Sulphuric acid question,

As for the Stannous, from what I have read, this test will indicate you if there is gold, not the concentration of gold, is my undertanding of this correct? (since from what I read, the Acid concentration in your solution affects the color of the test strip) ?

2- Can anyone tell me where would be the best place in Canada to find Copperas ? ? and powder Tin?

Thanks

Nighthawk
 
You are correct stannous chloride will detect very minute amounts of gold in solution, and telling you how much gold is not possible, although there may be slight shade differences for differing concentrations, and color may shift if other contaminates are in your solution of gold.

The test strips I am not sure what you’re talking about, PH percent hydrogen test strips? Chlorine test strips?

PH can be measured with a color change of an reagent (one can be made from red cabbage) the reagent can be very PH specific or can have a wide range (usually several different reagent in one solution).

Lead free solder from hard ware store is a good source of tin metal; look for 95% tin on label.
Read this http://en.wikipedia.org/wiki/Pewter

copperas make yer own, look for how to make it on forum, maybe search for (dilute sulfuric acid and transformer laminates, using butcher as author), see lasersteve’s web site, he has a better search engine for the forum and read all you can on his web site, Heck you may see some supplies you can use from there he also has video's of many of the processes we discuss here.
 
Thanks butcher,

I will look that up, I'm always looking to get the product and forget to look at ways to make it from people's experience :(

Sorry about the confusion, I did not want to say TEST STRIP, but should have said TEST RESULT..

Nighthawk
 
Another question for the experts.... in Hokes book, she seems to only refear to Copperas , and was wondering if Sodium bisulfite is a acceptable way to precipitate, I realize that the book is quite old and might not have been a option then, I seen reference to this in older post, but did not find anyone realy admitting that it is just as good as green Copperas, (assuming I did not miss any post that is) ... I ask because it does not seem to be something easy to find (well eccept in a 50 lbs bag anyways) and Sodium bisulfite can be easely found at any local wine making shop. I realize I can make it, but finding the supplies for that is also a little treck, and wanted your opinion. Alos, if this is a acceptable product, do I need to mix it with water as axplained with Copperas, and if so, what would be the ratio?

thanks

Nighthawk
 
Sodium bisulfite will work fine as a precipitant - It produces sulfur dioxide when it comes into contact with acidic solutions. That is what precipitates the gold from solution. Be very careful, do not breathe the fumes, they are quite dangerous.

I have been using Poor Man's AR lately, as Potassium nitrate is easier for me to obtain than nitric acid. If you add the potassium nitrate in increments, even though it does produce nitric acid, it only does so a little at a time. Therefore, I have had no problem with the formation of metastannic acid from the tin present, as is often the result of using nitric acid on materials made from bronze or those that contain tin, such as solder.

Search for Poor Man's AR with lazersteve as the author, using butcher's advice above.

Good luck, my friend.
dtectr
 
Thanks dtectr..

I will definatly look into making poor man's ar once my container of nitric is done, as it was as you said very hard to obtain, although I now have a source for it, it was VERY expensive...

Will I get sulfur dioxide fumes even if i use urea to nutralize the nitric? or because there is still hcl in the solution the fumes will still be present?

do I need to mix the bisulfite with water as I would do with copperas?

As you might have read from my previous post, I had missed a few steps in my process, and incorporated bisulfite before I had removed the nitric, it will be interesting to see what hapens when I incorporate urea at this point...will the bisulfite still be active and precipitate, or will I need to add more bisulfite?? it should be a good learning experience ..


thanks

nighthawk
 
Nighthawk said:
Thanks dtectr..

I will definatly look into making poor man's ar once my container of nitric is done, as it was as you said very hard to obtain, although I now have a source for it, it was VERY expensive...

Will I get sulfur dioxide fumes even if i use urea to nutralize the nitric? or because there is still hcl in the solution the fumes will still be present?

do I need to mix the bisulfite with water as I would do with copperas?

As you might have read from my previous post, I had missed a few steps in my process, and incorporated bisulfite before I had removed the nitric, it will be interesting to see what hapens when I incorporate urea at this point...will the bisulfite still be active and precipitate, or will I need to add more bisulfite?? it should be a good learning experience ..

thanks

nighthawk
My friend
When I was training for wilderness survival, I received one of the wisest bits of advice that applies, in principal, to so very many areas of life. "The best way to survive a critical situation in the wild is to not get into one in the first place."

That REALLY applies to the use of nitric in AR. If you don't put in too much to begin with, you don't have to worry about getting it back again. That is easier said than done, though. Even Hoke acknowledges that we, as beginners, tend to overdo it when it comes to the addition of nitric.

Most here would recommend NOT using urea, as it adds one more chemical variable to address. This is really only true, though, if you are going after the Platinum Group Metals (PGM), according to Gold SilverPro. If not (I don't, for now), add the urea a a prill at a time, and watch for the characteristic red fumes, accompanied by a visible reaction. Continue until the reactions/fumes cease.

Urea doesn't really neutralize the nitric acid - it converts it to Nitrous Oxide, as well as other gases. The expressions "expel the nitric" or "convert the nitric", would be more accurate, I believe. I use sulfamic acid for now, to accomplish the same thing, simply because I have some. Your solution will, therefore, still be highly acidic, which you want.

If you still have some solid metals present, you can start with adding a few ccs of HCl, watching for a reaction. If it reacts, then you likely have some free nitric. Remember, for AR to work, you need your HCl:nitric ratio to be either 4:1 or 3:1, depending on who you ask. If the formula gets out of balance either way, the reaction stalls, which doesn't necessarily mean that you have used up all your acid.

With Poor Man's AR, since you add the nitrates incrementally, about 5 cc. at a time, only a small amount of nitric is formed & is quickly consumed by the metals present. The above procedure, balancing the HCl:Nitric ratio, also applies here.

Using nitric, its important to know first how much copper or silver, weight in grams, you will be digesting. Using the formulas posted on the forum (someone made a nitric/silver spreadsheet the other day & posted it somewhere) measure out your Nitric & add a little at a time, as you do nitrates above. Some (mic, for one) have had good success in using just under the recommended amount, achieved good digestion, & didn't have free nitric to worry about in the end.

Re: the sodium bisulfite, I would check to make sure how pure it is & if there are any other agents added, insolubles. You may try dissolving a tablet in warm water, then check to see if there is any insoluble matter left in the bottom. If so, i would dissolve & filter, making as concentrated a solution as possible.

The sulfur dioxide (SO2) is formed as a reaction with the acidic solution, it is actually what causes the gold to precipitate.

Hope this helps. While i believe that what I posted here is accurate, still, I may have misstated some of the above - if so, I invite anyone to correct my errors.

Good luck & keep us posted.
dtectr
 
dtectr

that is a world of help, thanks so much for your post, I am not at this time looking to process platinum group metal at this time, I'm only working with gold, and possibly silver if I find that I have sufficient amount of silver chloride from my gold recovery process to continue further with it.

I tried to use as little Nitric as I could, I messured to cover my material being processed and no more, but since I am prosessing electronic material, it can get bulky, so in total I probably used 400 ml of nitric to make 3 small batches. I forgot about the Nitrous oxide gas, there is sooo much information in Hokes book It gets overwelming, After reading the book, I decided to keep to concentrate on the chapters relating to gold and silver for now, the other precious metals will have to wait for now :) baby steps ...

thanks again

Nighthawk
 
Another piece to the puzzle. When making poor mans AR....

If you distill your own nitric it takes 255 grams of high purity (98-99%) sodium nitrate to produce approximately 125ml of red fuming nitric. Distillation should in theory produce 100% pure nitric acid. In reality the home refiner will only be able to produce 92-96% pure nitric. Let's use 90% to be safe.

If you take your 125ml of 90% nitric and cut it with 36ml of distilled water you will now have 161ml of 70% nitric.

((90/70) * 125) - 125

Thanks to GSP for helping me figure that one out.

Using these numbers you can now more accurately guess how much nitric acid you are putting into the HCL to prevent excess nitric additions.
 
goldenchild said:
Another piece to the puzzle. When making poor mans AR....

If you distill your own nitric it takes 255 grams of high purity (98-99%) sodium nitrate to produce approximately 125ml of red fuming nitric. Distillation should in theory produce 100% pure nitric acid. In reality the home refiner will only be able to produce 92-96% pure nitric. Let's use 90% to be safe.

If you take your 125ml of 90% nitric and cut it with 36ml of distilled water you will now have 161ml of 70% nitric.

((90/70) * 125) - 125

Thanks to GSP for helping me figure that one out.

Using these numbers you can now more accurately guess how much nitric acid you are putting into the HCL to prevent excess nitric additions.
Thanks - that IS helpful! I'll copy & paste it with my Poor Man's AR instructions documents.
 
dtectr said:
I may have misstated some of the above - if so, I invite anyone to correct my errors.
The only thing I'd suggest is that the advice about the ratio for AR isn't true. The ratio isn't critical----any amount of either constituent will create some AR, and it will do work until it has been exhausted. In order for more work to be done, the acid that is deficient can then be added to continue dissolution once again, until one of the acids is again depleted, or all of the metal has been dissolved. Said another way, one need not make AR with a 3:1 or 4:1 ratio---and, indeed, neither of them may be correct because we often work with acids that vary in concentration beyond the ideal formula. (I'm basing my comment on volumetric measurements).

My policy has always been to use an excess of HCl, which does no harm, and is not expensive. That way you are assured of using up all of the nitric, so when action ceases, it's safe to assume that nitric is the acid that is short. The addition of a few drops will tell the tale---action picks up once again, assuming the solution is heated.

Harold
 

Latest posts

Back
Top