# Lovely gold AR with no SMB reaction



## das schnellste (May 4, 2013)

I am pulling my hair out right now because I have followed the process 3 times now and I am getting to reaction with SMB. The SC test shows gold in solution, and I dissolved about 4 ounces of karat jewelry with the proper % of silver. I have added a total of 6 table spoons of SMB and still no reaction. I even tried dissolving the SMB in hot water first, for about 2 tablespoons worth. I really don't want to cement and start over again. Is there something I can try that will drop the gold. I have been told to try table salt?? I am willing to try anything right now.


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## lazersteve (May 4, 2013)

Did you denoxx the solution?

Steve


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## Claudie (May 4, 2013)

I see that you are new to the forum, you can learn a lot here.
I am wondering what all is in your solution. Did you use a method that you read about here on the forum or did you use something like Shor chemicals? The more information you give about what you have already done, the more people will be able to help you.


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## Palladium (May 4, 2013)

Glad to see you back around Claudie. Hadn't seen you in awhile and was starting to worry.

On a side note anybody heard from Irons lately?


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## Claudie (May 4, 2013)

Thank you Palladium. 
Irons hasn't been with me, I haven't heard anything from him.


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## das schnellste (May 6, 2013)

My solution has had a minimum of a week to evaporate. I still get no reaction with SMB. I have never heard of denoxx.


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## das schnellste (May 6, 2013)

Claudie said:


> I see that you are new to the forum, you can learn a lot here.
> I am wondering what all is in your solution. Did you use a method that you read about here on the forum or did you use something like Shor chemicals? The more information you give about what you have already done, the more people will be able to help you.



Its a mixture of 14k gold and 18kt gold. There is some placer gold in the mix also. I melted it all together with fine silver and then started with nitric and distilled water. I filtered that solution and rinsed with nitric and distilled a few times. That's when I started the AR. At the end of the reaction is dropped sulphuric in the solution to drop the lead. Then I filtered it and meant to let it rest for 48 hrs. Then I lost track of time and ended up leaving it for about 1 week. The level in the beaker went from 800ml to a little over 700ml. From that point I added the SMB. NO REACTION. Did I let it sit too long? Did I miss a step. I have made it to this point a few times and then cemented with copper and started over, but I don't want to keep going through the process. I know I am doing something right because I keep recovering the same amount of silver and copper from my solution. Where am I going wrong?


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## steyr223 (May 6, 2013)

What brand is your smb?


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## steyr223 (May 6, 2013)

Sorry
Yes if you have gotten to this point a few times
And cemented .(is that this batch or a few prior
Batches)
I guess it makes no difference 

What is your source of AR (hno3+hcl,
pottasium nitrate or sodium nitrate+hcl)

It sounds like someone already gave you the
Answer
You have to much free nitric in your AR
Are you heating the hcl and than adding your
Nitre in consecutively smaller addition ,waiting
Between each one for the reaction to stop
Before adding the next

Heat will do so much more,if your doing it cold
It would take a lot more nitric

For now before you go off and read i belive
Page 44,45 or 55,56 (my phone format is off 10
Pages) of holkes 

Do you have a nugget of gold if so weigh it
And toss it in the AR you will get it back

It will consume the nitric but first tell us 
The question above so we can determine 
How much free nitric you have

Steyr223 rob

Edit i ment to ask how much of each chemical 
Are u using to make the AR exactly. And are
You premixing it or doing like stated above


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## Palladium (May 6, 2013)

Are you sure your smb is good?


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## das schnellste (May 8, 2013)

So if I heat this up and put more gold in it, will the reaction with SMB just happen, or will I need to add more(SMB)? Since it is already in solution, do I need to cement and start over, again?


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## butcher (May 8, 2013)

If the reason your gold will not precipitate from solution is caused by excess nitric acid in solution heating the solution with a button of gold will help, the nitric acid will be consumed when it oxidizes the gold, the gold oxidized gold will join with the chlorides from the HCl in solution.

You may or may not see the solution beginning to turn brown from gold beginning to be reduced, from your previous additions of sodium metabisulfite.

reaction with SMB:
Sodium metabisulfite reaction with water forms sulfur dioxide gas and sodium bisulfite,
Na2S2O5 + H2O --> SO2 (g) + NaHSO3
Gold chloride and sodium bisulfite and water forms solid brown gold metal powders, hydrochloric acid, and sodium bisulfate, along with evolution of a sulfur trioxide gas from the sodium bisulfate which converts to sodium sulfate in solution,
2AuCl3 + 3NaHSO3 +3H2O --> 2NaHSO3 +SO2 (g)
and
2NaHSO4 --> Na2SO4 + SO3 (g)

The SMB may have already reacted in solution as in the above equations, or in a similar fashion, so that it may not be able to precipitate the gold as it would normally, you may not have any sulfur dioxide gas and sodium bisulfite left in solution that it would be able to reduce the gold back to metal.

I would concentrate the solution with heat and the added gold button to consume any remaining nitric acid, after concentrated well but not so far as to form salt, dilute solution and let it sit (overnight), if gold precipitates, you will have a brown powder, test the solution with stannous chloride to see if all of the gold has precipitated, if not add more SMB, if no gold has precipitated you may see white powders (silver and possibly lead chlorides) decant the clear yellow solution and filter the clear liquid then proceed to precipitate the gold with fresh SMB (using your SnCl2 testing to determine the end point).


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## das schnellste (May 8, 2013)

Thank you all for your help. I will let you know if it works out.


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## philddreamer (May 8, 2013)

Apply heat in order to evaporate, but, DO NOT BRING TO A BOIL!
Take care!
Phil


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## g_axelsson (May 10, 2013)

Are you sure you are using SodiumMetaBisulfite and not SodiumMetaBisulfate?
Sulfite will drop your gold if your solution is proper denoxed, sulfate will do nothing.

Göran


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## das schnellste (May 14, 2013)

I triple checked and it is "fite" not "fate". I applied heat this weekend and even put a small chunk of placer gold in the AR. There was no reaction to the gold. After about 100ml evaporated, I tried the SMB again and got no reaction still. Then I cemented with copper and for some reason out of the 7 ounces of karat gold that I put in the melting dish, I only ended up with 20 grams after cementing. I hate to say this, but I am giving up. I can pay to have my solutions recovered if that is possible. I am tired of failing at this. Anybody wanna work my solutions and help me out. I also have a 10X20 storage unit full of escrap if anyone is interested.


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## steyr223 (May 14, 2013)

This is just a shot in the dark but

First your 14k to 18k you stated in the first post
Are u sure it was?

Second you had said 4 oz of katat (first post) .
were did the other 3 come from?
I am sorry if i missed something but i pulled
Over on the side of the road to do this.

Third you also mention the proper % of silver
What are your #s .I assumed you inquarted to
Bring down the karat to 6k, otherwise you
Can not get past the alloy that protects the gold
From being dissolved 
Did you have Any solids left after ar or did
You get complete dissolution 

Hope this helps steyr223 rob


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## steyr223 (May 14, 2013)

A few more thoughts

Did your stannous look good after evaporation
(Purple to black) and did it stay 

When i did my first evaporation the 100ml
You spoke of took only a few hours
After 16 more hours i believe only maybe
30-50mls actually evaporates 

But if your stannous yells gold and stays that way
Then it is reducing the gold chloride back
To it's elemental state thus telling us the
Free nitric is consumed

Your questions will be answered by someone
Much more proficient in this subject

Thanks steyr223 rob


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## butcher (May 14, 2013)

das schnellste,

It sounds like you are going to give up even before you get started.
You are getting a lesson in this, that recovery and refining is not as easy as we think it will be (before we actually learn how much there is involved in it).

And that it also does take a lot of study and practice to be able to understand, and gain the skills needed to do recovery and refining of metals.

Gold does not just vanish, if it was in the material to begin with it is somewhere in the materials you processed, whether it was in solution or did not completely go into solution, as long as you have not discarded the powders or solution's your gold is recoverable.

So as long as you have not discarded anything you have not lost anything.

You can quit, or you can use this lesson to get more determined to learn, and spending the time needed in studying.


But what you need is to gain first is the education, to be able to recover and refine, this takes time and a lot of study before diving in and dumping metals into acids and trying something you do not quite understand yet, but seems to you, that it should be so simple.

You are finding out it is not as simple as it first appears.


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## das schnellste (May 15, 2013)

I ended up combining two solutions that I was having problem with in order to free up some glassware in order to try and resolve my issues. Before inquarting I acid tested the gold to make sure it was solid. I cut all of the rings and necklaces and earings and took a chunk of each piece and it dissolved completely in AR. Now I admit, I did this like a newbie idiot and didn't write down my % amounts like I should have. So now I have no clue what my amounts were. I just know that the two solutions combined had 7.242 oz of mostly 18kt gold. there were only a few pieces of 14kt and only one pair of earings that was 10kt.

My biggest problem right now is I am moving to a condo complex in Arizona and I will not be able to have my lab anymore. I have only three weeks to figure out my problems or I have to get rid of my solutions and acids. There is no way I am transporting my solutions in a UHaul in 100 degree temperatures.
Is there anyone out there that can help me by taking this stuff off my hands. I would like to just give this stuff to someone as well as my storage full of escrap and then cut a deal for half the gold produced. If anyone is interested, private message me. I really wish I had time to learn more about this, but right now is crunch time, and I just can't spare the time.

Thanks for all of your help with all of my questions. Maybe in a few years when I can actually buy a house I will be able to build my lab again.


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## butcher (May 15, 2013)

I would make sure the solution is slightly acidic, now you can cement the gold out of solution, use a large clean thick piece of copper, a copper buss bar from an electrical panel is best, but you can use a piece of clean copper pipe, a six inch long piece of 2" copper can be cut long wise with a pair of large tin snips or hack saw, the pipe unrolled and using a hammer flattened out, you also can punch a hole with a nail and a hammer, this gives you a place to hang it with a copper wire if needed, when you add the copper metal to an acidic solution containing the gold, gold will cement out of solution as a black powder, some of the copper will dissolve into solution pushing out, or replacing the gold from solution, when all of the gold is out of solution and there is no more free acid the copper will stop dissolving into solution, after there is no more reaction brush off the copper copper into the solution cleaning the copper bar, you can put it back into solution and if no more black powder forms on the bar the gold should be out of solution, a test with stannous is also recommended, although the green copper solution may mask a slight violet reaction making it hard to tell, when done brush of the copper again, let powders settle, carefully decant solution, dirty gold powders do not settle well or stay settled well, dry the gold and save it to take to Arizona. 

The solution you can add iron to it to replace the copper from the solution cementing it out of solution as you did the gold above, decant iron solution from the powdered copper and dry the copper powders, with the iron solution bring it up to pH 9.5, let it settle decant solution from iron and base metal hydroxide sludge, bring the decanted solution back down to pH7 let it settle again, if anything precipitates, decant the now salt water, which is safe to dispose of, dry the sludge powders, heating the dried hydroxide powders strongly will make the safer oxides for waste disposal.


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## das schnellste (May 20, 2013)

I used a copper heat sink from a CPU. It seemed to work well, but the heat sink disintigrated very fast. I went through three of them. I am drying the powders now and I used aluminum foil to retrieve the copper out of the leftover solution. I realize the solution still has aluminum in it, but I don't know how to get the aluminum out of it, or if I actually need to remove the aluminum from solution.


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## butcher (May 21, 2013)

Add sodium hydroxide to make aluminum hydroxide, and let the fluffy powders settle from the salt water.

Aluminum hydroxide is a very fluffy goop, very hard to dry, Iron is a better choice much easier to deal with.

In the safety section one of the must read topics is dealing with waste, situations to avoid, the elephant in the room is also a very good read.

If you dissolved a lot of copper to cement, this is an indicator you are using way too much acids, there are many posts discussing limiting the acid and about how much acid is needed with how much metals, this will be another topic to study to get a better understanding, to help keep you out of a lot of the problems from overuse of acids, it can also save you some money.


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