SUCCESSFULLY PAST HOKE PAGE 44 - THEN A BUMP

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INDY864

Well-known member
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Dec 4, 2010
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After two evaporations to remove the nitric, filtering, raising the ph to 1.0, I was really siked. I had a beautiful golden brown solution. I studied the handbook online, and Steve's video. I added the SMB. It turned black. Then it turned back to the golden brown. Then nothing. It didn't drop.
Should I slowly reheat the solution to concentrate it and add more SMB? Kinda stuck.
 
you can neutralize nitric with smb but it will take much more than necessary. did you test to make sure you have gold in your solution? nitric acid boils at 121 degrees C, just cover your glass pot with a watch glass or i have found a glass dinner plate works good too untill the solution gets thick and no more NOx fumes are present.
 
Geo said:
you can neutralize nitric with smb but it will take much more than necessary. did you test to make sure you have gold in your solution? nitric acid boils at 121 degrees C, just cover your glass pot with a watch glass or i have found a glass dinner plate works good too untill the solution gets thick and no more NOx fumes are present.
Covering to evaporate is counter productive. The point is to evaporate, not evaporate and condense.
Evaporation should be conducted at a temperature below a boil, so values are not lost. It's all in Hoke.

Harold
 
Do you have any urea? Even if you don’t use it for neutralizing the excess nitric you can still use it for testing purposes. After you evaporate your solution down and add more hcl you can add a peril of urea and if you observe fizzing you still have free nitric.
 
Harold_V said:
Geo said:
you can neutralize nitric with smb but it will take much more than necessary. did you test to make sure you have gold in your solution? nitric acid boils at 121 degrees C, just cover your glass pot with a watch glass or i have found a glass dinner plate works good too untill the solution gets thick and no more NOx fumes are present.
Covering to evaporate is counter productive. The point is to evaporate, not evaporate and condense.
Evaporation should be conducted at a temperature below a boil, so values are not lost. It's all in Hoke.

Harold
maybe thats why i could never get it to work right for me. it would eventually evaporate but it took forever. thanks for clearing that up.
 
Thanks guys,
I am dealing with a small amount of gold I am refining from mining. It is very pure. I have had a reaction that puzzles me.
After adding SMB, the liquid turned black, then brown, then light brown, then 14 hours later to a pale lime green.
Does anyone have any input?
 
INDY---

If nothing but gravity separated gold is dissolved in aqua regia, and SMB is added, there is nothing in there which will produce all those strong colors.

:?:
 
Indy---

Oh, I thought you said that after dissolving the gold, your solution was a golden brown. If you had just, as you described it, "very pure gold" dissolved, your resultant solution should be yellow or, if lots of Au, orange. With a little contamination, maybe light brown.

After adding SMB, the solution should go from yellow or orange, to clear, and there should be tan power on the bottom of the container. With a little contamination, the solution could be greenish or bluish or brownish, but it should be light colored and transparant.

Those dark colors you described don't sound right, if you started with "very pure gold," and real SMB.

What was the actual color of your dissolved solution, and how transparant was it?

Is your SMB sodium metabisulfite or sodium metabisulfate?
 
Indy---

Sorry, I guess the "black" threw me. I just reread, and see that it ended up "pale lime green."

You can simply hang some solid copper into the solution, and cement out all the PMs, then refine it over again, limiting the amount of nitric this time. That would be a good way of getting sight of your gold again, so it's not "lost."

Let it sit overnight, then test the solution with stannous chloride. If any PMs are still in solution, decant the solution and leave the copper hanging in it for a week or so. In the meantime, you will have your gold in solid form, to prove it's not "gone."

If you actually started with gold ore, you should probably do this as step one, anyway, as a recovery process, then refine the powders.
 
eeTHr said:
Indy---

Sorry, I guess the "black" threw me. I just reread, and see that it ended up "pale lime green."

You can simply hang some solid copper into the solution, and cement out all the PMs, then refine it over again, limiting the amount of nitric this time. That would be a good way of getting sight of your gold again, so it's not "lost."

Let it sit overnight, then test the solution with stannous chloride. If any PMs are still in solution, decant the solution and leave the copper hanging in it for a week or so. In the meantime, you will have your gold in solid form, to prove it's not "gone."

If you actually started with gold ore, you should probably do this as step one, anyway, as a recovery process, then refine the powders.
Thanks eeTHr,
Hoke says on page 45 that the gold solution, if mainly gold, is a yellowish brown. That is what I am going by. I just got my tin wire to make stannous chloride. i don't mind doing stupid stuff if I am learning. I think I am dealing with too small a gold result. I have saved my nitric wash. I started 2 threads by mistake. I did a hcl, water 3 times, nitric, water 3 times, wash then A/R. BUT I KEPT THE NITRIC WASH! Figured I might lose some gold in the wash. (My ADD is kicking in).
All that said, I am going back and starting to test everything with stannous chloride. I had ordered some tin wire from Israel. I got started without the tin and I paid for it. BUT the learning is priceless. Oh Yeah, the SMB is SULPHITE.
indy
 
Indy---

Since this has evolved from a refining problem into a recovery problem, you would probably be best helped if you posted in the Prospecting, Mining, Ore Concentrates & Geochemical part of the MINING & METAL DETECTING section of this forum.

There are some very knowledgeable people who could help you with your initial recovery from the ore, which can be very different from refining processes.
 
eeTHr said:
Indy---

Since this has evolved from a refining problem into a recovery problem, you would probably be best helped if you posted in the Prospecting, Mining, Ore Concentrates & Geochemical part of the MINING & METAL DETECTING section of this forum.

There are some very knowledgeable people who could help you with your initial recovery from the ore, which can be very different from refining processes.
Thanks! I never thought of that. That's exciting. THANKS AGAIN!
 
Geo said:
Harold_V said:
Geo said:
you can neutralize nitric with smb but it will take much more than necessary. did you test to make sure you have gold in your solution? nitric acid boils at 121 degrees C, just cover your glass pot with a watch glass or i have found a glass dinner plate works good too untill the solution gets thick and no more NOx fumes are present.
Covering to evaporate is counter productive. The point is to evaporate, not evaporate and condense.
Evaporation should be conducted at a temperature below a boil, so values are not lost. It's all in Hoke.

Harold
maybe thats why i could never get it to work right for me. it would eventually boil down but it took forever. thanks for clearing that up.
If you understood the level of contempt I have for people that discuss evaporation by speaking of BOILING, maybe you'd rephrase your comments.

Why in hell do you suppose people keep evaporating too fast? Could it be because people like you insist on talking about boiling, when they shouldn't be?

Can you say *evaporate*?

Harold
 
Thank you.

I strive for the use of proper terminology on this forum. When falsehoods are repeated endlessly, those that don't think clearly assume that what they read can be taken literally. That creates a never ending source of people that have the same problems, time and again, and it could all be eliminated by people giving proper instructions at the outset.

None of us are perfect, in particular, me, but we all must strive for excellence in conveying our messages, otherwise no one benefits.

If you must use evaporate and boil in the same sentence, they should be separated by the words DO NOT.

Harold
 
Harold_V said:
Thank you.

I strive for the use of proper terminology on this forum. When falsehoods are repeated endlessly, those that don't think clearly assume that what they read can be taken literally. That creates a never ending source of people that have the same problems, time and again, and it could all be eliminated by people giving proper instructions at the outset.

None of us are perfect, in particular, me, but we all must strive for excellence in conveying our messages, otherwise no one benefits.

If you must use evaporate and boil in the same sentence, they should be separated by the words DO NOT.

Harold
harold,
You took me to task several months ago about boiling. I have taken it to heart. However I have made the mistake of leaving the sample on what I thought was a low temp only to find it boiling. I get confused with LazerSteve's video. He boils his solution. But it's not Nitric or A/R. He does boil HCL. I'm learning not to boil regardless.
INDY
 

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