Silver paste ontop of AR

[jeneje]

Hello all,

I have a ?, what is the silver looking paste on top of my AR solution. Here is what i done. I added 2oz of pins, next I added 2cups of hcl and added 1/4 cup nitric. The AR begain to work slowly with very little NOX, I checked it after 1hr and there were flakes of gold on top of the solution, I added 100ml more of nitric and put on the burner at low temp. After thirty more min, I removed it and the silver looking paste was on top.

At this time it is cooling, I just wanted to know if it could be silver or is it something else - before i begain the next step of filtering and denoxing. Any advice would be grateful.

Thanks
Ken

 

[Barren Realms 007]

Did your pins have solder on them or were they clean pins? Could be lead or film of oil.

 

[jeneje]

They may have had some solder on them. I tried to get them as clean as I could. I pre washed in hcl before using AR but may not have washed them good enought.

I just looked and it seems to be drying on top of the solution.

Ken

 

[element47]

I am not an experienced refiner, I am a learner who hasn't touched a test tube or beaker yet. Without any real-world experience, it appears to me you are under-nitric'ed.

And as I read your post, your HCl:HNO3 proportion appears to be 8:1 instead of the 3:1or 4:1 specified as the formula for AR.

Additionally, you haven't specified the concentration of nitric you started with.

 

[Barren Realms 007]

I am not an experienced refiner, I am a learner who hasn't touched a test tube or beaker yet. Without any real-world experience, it appears to me you are under-nitric'ed.

And as I read your post, your HCl:HNO3 proportion appears to be 8:1 instead of the 3:1or 4:1 specified as the formula for AR.

Additionally, you haven't specified the concentration of nitric you started with.

You add your nitric a little at a time and let it work and do it's job until the material is processed.

 

[jeneje]

Barren that is what I did, use a little at a time to help control the NOX fumes. The HCL is 31.45% and the HNO3 is 68 to 70 % if that helps. At this time do I procede with the denoxing or ?

Thanks
Ken

 

[lazersteve]

The solution appears to be dehydrated and saturated with copper, therefore the gray is likely copper I chloride.

Add some HCl to redissolve the copper I chloride.

Steve

 

[Barren Realms 007]

If all of your material is dissloved then yes you can start with the denoxing. You might consider going ahead and filtering the material to remove the gunk on top and if you run across any black powder in your filter reprocess it seperatly.

 

[jeneje]

Barren I checked and I still have material in the bottom, I done as Steve suggusted and added 1/2 cup more HCL and the silver went away but my gold flakes are still on top in the solution I have attached a pic.

Ken

ps. should I re - heat the solution.

 

[patnor1011]

When you will do this next time dont do it like this. I suggest you first start with diluted HNO3 - you can introduce bit of heating. This will dissolve most of base metals before you start dissolving gold in AR.
It will save you a lot of headache and time.

 

[jeneje]

Thanks Pat, I will next time, I am still learning, but I am trying and learning much on the way to success. btw did you get what I sent you.

Ken

 

[eeTHr]

I looks like there is undissolved gold floating, too.

I would add HCl, as Steve said, until the base metals dissolved, up to possibly doubling the volume of liquid (as an approximate guess).

Then add a little nitric at a time, with it on heat but not "boiling," until the gold is dissolved.

If you added only a little nitric at a time, there should not be much excess, so take if off the heat and let it cool. If anything crystalized when it cools, add a little more HCl. If there is any debris in the bottom, like plastic or carbon, decant the solution into another container.

Get a foot or two of AWG #0-0 bare copper "ground" wire from ACE hardware or the like, or copper bus bars, and hang the copper in the solution, and drop out all values. With the wire, you can bend it into a flat coil, that looks like an electric stove burner, just smaller in diameter that the mouth of your container, then bend the wire from the last coil on the outer turn up at 90 degrees, and at the proper height bend a hook to go over the lip of the container so the coiled part will hang suspended in the solution.

Let the copper hang in there overnight, then decant and save the solution, let the copper hang in it again for a week, to get a little bit more values.

Refine the powders left after decanting, in AR. De-nox and dilute, and drop with SMB or whatever you normally use.

Not being a professional, I certainly invite the possibility of better solutions from others more experienced.

 

[eeTHr]

jenege;

If you do as patnor suggested, and get rid of the base metals first, on your next recovery, then you can skip the copper step, as it won't be necessary.

 

[patnor1011]

Thanks Pat, I will next time, I am still learning, but I am trying and learning much on the way to success. btw did you get what I sent you.

Ken

Yes Ken. Thanks.

 

[jeneje]

jenege;

If you do as patnor suggested, and get rid of the base metals first, on your next recovery, then you can skip the copper step, as it won't be necessary.

I will ee, and thanks for your help. Thanks to all who helped with this I have learned yet another step to avoid while contiuning my education on refineing.

Thanks
Everbody.
Ken

 

[lazersteve]

... I done as Steve suggusted and added 1/2 cup more HCL and the silver went away but my gold flakes are still on top in the solution I have attached a pic.

At this point you have a saturated solution of copper chloride mixed with base metals and gold in the bottom or floating around as flakes.

Check out the Modified Poorman's AR method here:

Modified Poorman's Ar

and pick up at step # 9 and continue until all of the base metals are dissolved. Go easy on the nitrate additions so you don't dissolve the gold. It is very important not to over do the nitrate additions or you will have gold in your dirty base metal solution. Be sure to allow your solution to cool before pouring off the dark colored acid after each cycle.

If done right the gold will go into solution on the last cycle and you will have a yellow to slightly lime green colored solution.

Steve

 

[Sodbuster]

What Pat said, "When you will do this next time don't do it like this. I suggest you first start with diluted HNO3"

That will work but do make sure those pins are not brass base metals. You will not want the tin involved with the nitric.

Ray

 

[patnor1011]

I agree, and if they are I would start with HCl and crockpot. Bit slower but this will help with base metals before moving to gold.