Gold bearing solution split?

[Desertcik]

Hi,
something odd has happened to my gold bearing solution after adding SMB, it split in to two phases. I didn’t neutaralize excess nitric, because I thought the amount I used was just right(yet I’m not sure of that). Does anybody have a clue what might be happening here , and how to fix this mess?
Best regards.

 

[butcher]

Where did this gold-bearing solution come from?
What type of other metals or nonmetals could you also have in solution?
How pure was the gold before you put it into the solution?
What have you done up to this point?

SMB or SO2 is not selective for gold, especially when nitric or nitrates are involved, it can also reduce copper, silver and lead and mercury are insoluble as chlorides...

All I can tell is something is precipitating from solution.
The more details you can provide, the more clues of what is happening.

 

[Lino1406]

Tell the exact details of how you got this gold bearing solution

 

[Desertcik]

So step by step: I Inquarted some old 14k jewelry with silver, then dissolved the alloy in nitric acid. Then I dissolved leftover gold with aqua Regia. This is just diluted AR.
At the begginig of gold drop process it was all fine as I had added SMB in pinches, the problem appeared when i dissolved the rest of demanded SMB in destilled water and poured it into the solution.

 

[Desertcik]

Update:

 

[butcher]

So was the solution concentrated?

Silver as AgCl2 dissolved in solution (formed in the high concentration of chloride ions) will reduce to insoluble AgCl (white salt) when the solution is diluted.

Did you dilute solution and let it sit overnight to remove the insoluble silver, prior to adding SMB and diluting solution?

Before I could finish my post you have posted an updated picture with better-looking results.
I will ask the question anyway.

It could have been silver chloride, now with your precipitated gold???

 

[anachronism]

As Butcher said, it helps when you get a better pic- it's just funny when it happens whilst you're typing a helpful response. 8) 8) :lol: :lol:

As Butcher also said- that later pic looks pretty good to me.

 

[Desertcik]

Well I didn’t leave it overnight, but I did filter it after diluting. For me it looks like only Gold powder participated out but still i have never seen such fenomen before.

 

[butcher]

Give it a good washing, (Search getting Gold pure and shining Harold as the Author).

It might have been some silver chloride, or maybe just the SO2 gases in the lower part of the solution giving up electrons stirring things up down there?

 

[butcher]

Just a thought, the phase solution separation may have been where the lower phase was gassing SO2 attempting to reduce the gold, while the upper phase of the solution may have been trying to re-dissolve the gold...

Stirring the solution may have mixed the separation?

Have you tested the solution after precipitating the gold?

 

[Desertcik]

I will proceed with washing the gold powder, also separate both liquid phases and test them.

 

[g_axelsson]

Just stir the solution.

It's easy to form two layers if you don't stir your solution. I get it often and you could often see a zone of heavy liquid below a more dilute layer and where the gold redissolves. Different density creates separate layers with different chemistry.

Here is one I did once. Gold in solution in the top layer with enough SMB to reduce the gold at the bottom. Solid gold at the bottom.


An easy way to create a density gradient is to use gravity filtering with the stem of the funnel leading down into the liquid. You can actually see the filtered liquid flowing up from the funnel to the top of the liquid when you wash the filter with water in the end. The gold chloride solution is really heavy compared with water and doesn't mix easily unless you stir it.

Göran

 

[Desertcik]

Just stir the solution.

It's easy to form two layers if you don't stir your solution. I get it often and you could often see a zone of heavy liquid below a more dilute layer and where the gold redissolves. Different density creates separate layers with different chemistry.

Here is one I did once. Gold in solution in the top layer with enough SMB to reduce the gold at the bottom. Solid gold at the bottom.
AR-dual-layer.jpg

An easy way to create a density gradient is to use gravity filtering with the stem of the funnel leading down into the liquid. You can actually see the filtered liquid flowing up from the funnel to the top of the liquid when you wash the filter with water in the end. The gold chloride solution is really heavy compared with water and doesn't mix easily unless you stir it.

Göran

I have just finished whole process, apparently you are right.

 

[Shark]

I have seen it several times as well. Here is a shot of one of mine, scroll down and read GSP's reply about it. It might help with future drops.

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=61&t=26820#p284715

 

[Desertcik]

Thanks for your answears, you all have made me not freak out with my future drops!

 

[anachronism]

Thanks for your answears, you all have made me not freak out with my future drops!

Don't ever freak out. Remember you still have your gold until you throw it away :lol: :lol:

Joking aside that is one of the facts you must always remember.

Jon

 

[g_axelsson]

Don't ever freak out. Remember you still have your gold until you throw it away :lol: :lol:

That has a whole new meaning for me nowadays. :mrgreen:

Göran

 

[butcher]

Just thinking of the gold I've missed, couldn't find in all of the big holes I dug so deep, didn't know was under my nose and left my hands, washed out the end of the sluice with the tailings in the fast-moving water downstream, that might have been under the iron nails or bullets I found metal detecting, well I just freak out.

When I put gold I finally had in my hand into a solution I made sure I understood enough to be able to get it back (one way or another), there is no way it would get away from me now. No need to freak out, although I have stood there at times scratching my wooden head trying to figure out what was going wrong, here again gaining an understanding of the principles, we can figure out the problems as they raise their ugly head...