Where did my gold go?

xelexo
Advertise with us
Shop deals on ebay
shop deals on amazon
Gold Refining Forum

Help Support Gold Refining Forum:

This site may earn a commission from merchant affiliate links, including eBay, Amazon, and others.
2002valkyrie

2002valkyrie

Well-known member
Joined
Oct 3, 2009
Messages
143
Hi All,
I started with 17g. of 10k and 23.8g of 14k did my inquarting with 42.7g of sterling silver. This should equal 20.995g of refined gold and 67.005g of base metals. I used home made Nitric from Muriatic Acid and Nitric Soda to dissolve base metals then washed my black sponge. For the next process I dissolved the sponge in HCL and Bleach, filtered and then added Sodium Metabisulfite. (I did not dilute in H2O) I after sitting all night I separated it. I ended up with brown mud that totals to 7.8g. I checked the remaining HCL and Bleach with Stannous Chloride and it turns a little brown, I checked my Nitric solution which I also rinsed my sponge into and it turns dark black instantly. What should I do? I have considered using Aluminum to just start over. Anybody got a fix for me?
 
Your first solution was a poor mans AR. if it were me I would put a piece of copper in there and let it cement out the gold and silver,
then start over, use real nitric for parting or try steves new cold nitric process seems it will yeild sulfate free or low sulfate nitric

Jim
 
james122964 said:
Your first solution was a poor mans AR. if it were me I would put a piece of copper in there and let it cement out the gold and silver,
then start over, use real nitric for parting or try steves new cold nitric process seems it will yeild sulfate free or low sulfate nitric

Jim
Click to expand...

Unless it's Chloride free, using Sodium or Potassium Nitrate to make Nitric Acid will dissolve some of the Gold. If the Nitric is dilute, the Chloride will precipitate out as Silver Chloride, contaminating the Gold.

You can check the Sodium Nitrate for Chloride by dissolving a little in distilled water and adding a few drops of Silver Nitrate solution.

The best solution is to buy some good quality Nitric.
 
valkyrie;

2002valkyrie said:
home made Nitric from Muriatic Acid and Nitric Soda
Click to expand...
It should be sulfuric acid and....

A quick way to make poor man's aqua regia is to put, a little at a time, some dry sodium nitrate or potassium nitrate into the container of Au and Muriatic (31% HCl), until after awhile (especially if it's not heated) all the gold is dissolved (that way you don't have much nitric to get rid of before testing or precipitating). That's why the stannous test is black---it's aqua regia, not nitric.

(Plus what james and Irons said). There can be a little bit of chloride in the regular sulfuric-made nitric, too (something about the result of impurities in the sodium or potassium nitrate from the process by which they are made, I believe), so watch out for that as it can suck up a little of your Au if you don't get it out first.

Don
 
I used Hi Yield brand which Catfish had spoke about in the Forum Handbook 1st edition, pg. 21. As for cementing and starting over. What would be the best way?
 
My suggestion was to put a piece of copper in to cement out the silver and gold,
then treat with nitric to remove the silver.
Jim
 
valkyrie;

Also---
2002valkyrie said:
I checked the remaining HCL and Bleach with Stannous Chloride and it turns a little brown
Click to expand...

If you do this test on filter paper and get what looks like a coffee stain, it could be platinum, so don't throw that solution out. (Especially if it is orange as soon as you drop the stannous on it, then turns tan in a little while.)

Don
 
valkyrie;

Here is one way I think you could recover your PMs from the two solutions you now have. I don't know if it's the best way, but it might be interesting to do. See if anyone else has any comments on it---

Treat both solutions as Au + Ag + copper + possible Platinum Group Metals.

With the aqua regia (first solution), get rid of any nitric with urea or preferably by the evaporation process (evaporation produces lots of toxic fumes).

Then dilute with 3 to 5 times water, this dilution with water will drop silver as the chloride form. Let the silver chloride settle and pour off or suck out the Au + Cu (+ PGMs?) solution into a new container, rinse the silver chloride with a little water and add this rinse water to the new solution container. A second rinse, or more may be optimal. There is always some fluid left in the precipitation, to avoid removing the precipitation with the solution. Avoid the use of filters whenever possible, so you don't have a bunch of filter papers to incinerate later.

Keep the silver chloride wet (add more water), save it until you have more or whenever you decide, then convert it to metalic silver using the lye and kayro syrup method.

Precipitate the Au in the new solution container with SMB, let it start to settle for awhile then test a drop of the solution for Au (if you get purple, add a little more SMB), let the precipitation settle for a couple of days, and pour/suck the remaining solution into a third container, rinse the same way again, into the third container. Your Au will remain in the second container.

Test the third solution for platinum and palladium with stannous and/or PGM testers if you have them. If it tests positive for any platinum or palladium, save up the solution, or whenever you want to, use the appropiate precipitation methods for those.

Do the same for the A/C solution, except just warm it for awhile to evaporate most of the chlorine if any is left over.

Don
 
eeTHr said:
valkyrie;

Here is one way I think you could recover your PMs from the two solutions you now have. I don't know if it's the best way, but it might be interesting to do. See if anyone else has any comments on it---

Treat both solutions as Au + Ag + copper + possible Platinum Group Metals.

With the aqua regia (first solution), get rid of any nitric with urea or preferably by the evaporation process (evaporation produces lots of toxic fumes).

Then dilute with 3 to 5 times water, this dilution with water will drop silver as the chloride form. Let the silver chloride settle and pour off or suck out the Au + Cu (+ PGMs?) solution into a new container, rinse the silver chloride with a little water and add this rinse water to the new solution container.

Keep the silver chloride wet (add more water), save it until you have more or whenever you decide, then convert it to metalic silver using the lye and kayro syrup method.

Precipitate the Au in the new solution container with SMB, let settle a couple of days, and pour/suck the remaining solution into a third container, rinse the same way again, into the third container. Your Au will remain in the second container.

Test the third solution for platinum and palladium with stannous and/or PGM testers if you have them. If it tests positive for any platinum or palladium, save up the solution, or whenever you want to, use the appropiate precipitation methods for those.

Do the same for the A/C solution, except just warm it for awhile to evaporate most of the chlorine if any is left over.

Don
Click to expand...

I'm a Noob but I would like to try if it's doable.

Here is an idea I have been tossing around in my head; If I can evaporate the Nitric off, what is stopping me from running it through a condenser and capturing pure Nitric? Or running the fumes through a pipit into chilled Hydrogen Peroxide for a Nitric solution? I know people make Nitric Acid that way but why can't I recycle? I got my eye on a condenser now.
 
valkyrie;

I have seen that discussed on this forum in a couple of different threads. From what I have read, it is doable, but I don't remember the exact recommendations.

Also, I put some edits into my previous post. I hope they help. 8)

Don

P.S. I am thinking about a condenser too, because it keeps the salts and chlorides out of the resultant nitric.
 
I’m not going to go into all the advice that has been given so far but…

If I am not mistaken this is valkyries’s first precipitation. To keep things simple set aside any precipitate you have from SMB precipitation.

Cement all the acidic solutions you have on copper until the solutions give you a negative stannic reaction giving you only precious metals as a precipitate from your solutions.

Combine your 2 precipitations and process as a gold/silver/copper alloy with the possibility of PGM.

You are then starting from the beginning then but with less base metals and the knowledge that your have gained.

I would save all solutions and solids from this first attempt to revisit later when your testing and procedure skills have been perfected some, just to be sure you did not throw out values. I would also use smaller amounts of PMs as you are learning this. 1 gram of gold content is more than enough to see in your beaker, wash, and make a bead from with a torch until you are more comfortable having success several times with smaller quantities before moving on to larger lots.

Keep it simple.
 
Thank you Oz,
Simple, I think I will do that just to get some cash flow going. It is very sound advise.

Oz said:
Cement all the acidic solutions you have on copper until the solutions give you a negative stannic reaction giving you only precious metals as a precipitate from your solutions.
.
Click to expand...

Forgive me but could somebody translate this phrase into a more Southern Alabama lingo for me please... Are you refering to the Stannous Chloride test? If so what should it look like? Anybody got a link to how to read the colors and reactions of Stannous Chloride?

"Wow I read this and wish I had ask questions before I started... I hate learning the hard way."
 
Valk,

You should follow the Guided Tour Link in my signature line below. It will answer your stannous questions and many more.

It always surprises me that so many noob's don't follow the links that have been set up just for them. Anyway, the guided tour will give you a list of reactions, reaction abbreviations and ingredients, safety tips, and much more. It's well worth the time spent reading in the knowledge you'll gain.

Steve
 
I have watched Lazersteve's video again (I have watched it many, many times because I am hearing impaired) I think I heard him say he droped the gold with SMB (Sulfate not Sulfite) I am really confused now because all I've read say's to use Sodium Metabisulfite. My drop looks nothing like his in the video. It took 12 hours to get a milky brownish tan mud and his was a noticable black in a matter of seconds.My acid stayed yellow and his cleared instantly... :?: Thoughts anyone? :?:

This is a link to his video.http://www.goldrecovery.us/goldrecovery/videos/smb.asp
 
The video audio was a slip of the tongue. I haven't had time to remaster the audio portion to repair the discrepancy. It's Sodium Meta Bisulfite.

The reaction will vary depending on concentration of gold in the solution, temperature, free oxidizers (e.g. chlorine, hydroxide, NOx). If you only have a small amount of gold in a large volume of liquid you will get the symptoms you describe.

The persistent yellow tint is likely either chlorine (more green tint), iron ( more yellow orange), or gold with too much oxidizer. The excess oxidizer redissolves the fine gold as soon as it is precipitated.

This is where stannous chloride tests are used to let you 'see' if the gold is in solution before and after adding SMB.

Steve
 
Sorry about that. Yes, I was referring to a stannic chloride test reaction.

As to colors if there are multiple PMs present it can become hard to read without experience. You will notice in Hoke that she recommends acquaintance tests with known pure metals, and if I remember properly even suggests you mix some PMs in different ratios to see the difference.

For your purposes here on your first process any color change you will see on a stannic test indicates you still have values in your solution. For reference, gold by itself can give reactions from light purple (low gold content) to black (high gold content).

Something that is exceedingly important is that you are sure your stannous chloride is functioning properly or you risk throwing out values that you do not see because of bad stannic. A very easy way to be sure of your stannous chloride is to make a gold test solution.

Find a discarded computer card with a gold finger edge, trim the edge off and use AP (HCl with just the smallest dash of H2O2 (hydrogen peroxide) to remove the copper from under the gold platting) until you have the gold foils floating free. Filter out the gold foils and rinse. Put your foils in a test tube and add a small amount of HCl and add unscented household bleach a few drops at a time until your gold dissolves (gentle heat helps). Keep this auric chloride (known gold solution) on hand.

Now every time you wish to test for values in solution with stannous chloride you can first test to see that your stannous is reacting properly by using your “known gold solution” before you trust it to test something more valuable.

As you test with stannous the colors will become more familiar. PGMs get a bit more involved but not terribly. This is also why I suggested you save solids and liquids incase you do have some PGMs in your karat gold.
 

Latest posts

Back
Top