AP CU saturation help needed...

[JH123]

This continues where Crow Kings Pirahna thread stops..

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=37&t=13461

We intended to saturate the solution and added copper til it would no longer consume it. Our bucket sat for 3 weeks and evaporated away from nearly 3 gallon of solution to half of that while we were busy with other matters, becoming quite thick before we got back to it. We added more HCL perhaps not enough as we now have a black color to the solution yet a beautiful turquoise colored film and paste when we try to strain, the bottom of the bucket contains a fist sized glob of this copper in a clay like form.

Is this typical of a staurated w/ copper AP? Should the amount of copper in a saturated solution be so thick that it will not strain through filters or have we not replaced ALL of the evaporated HCL that would bring it back to a strainable solution w/ all the copper in liquid form?

We are still trying to locate any gold within it since we think a possibility of up to 8 grams of AU are lost. We managed to gather 5-6 filters with material for testing with Stannous. Is it possible to identify AU purple stain when dealing with this much CU?

With the CU covered filters in hopes of finding some gold, what would you recommend for us try with those filters? Joe

 

[butcher]

I will use old copper chloride solution, sometimes cooking it down thick dissolving copper, iron, and other base metals, I will usually strain pins in a bucket with holes drilled in bottom (see Lazersteve's idea for the foils bucket strainer), to separate the copper chloride gold foils and some of the other chloride powders from the pins, the un-dissolved pins, eye glass frames or whatever, is returned to the corning casserole dish, and the decanted solution is also returned to the dish, and more solution added, the jar of chloride powders are washed in new HCl boiled and hot water washes, solution added to un dissolved pins, then these powders are washed in caustic soda solution to neutralize the powders (help to form oxides and possible somewhat hydroxide of the metal powder, and the salt water solution rinsed in hot water, (the caustic washes and salt water washes to into the waste stream and any powder that settles from these solution are added back into the possible value to be treated stream.

These neutralized powders are dried and incinerated, (in another corning casserole dish on the second hotplate burner, the incinerated powders are washed in boiling HCl, a little water added (not much and the powders settled still hot but not moving from boiling, the HCl wash goes into the other dish to help dissolve the pins, the incinerated powders are then wash in boiling water several times this water also goes to help dissolve the pins in other dish, these powders are now dried and incinerated again, after this I can use nitric to remove any silver palladium and base metals involved (using copper to cement the values from this solution, the remaining powder is my gold and possible PGMs if involved and can be dissolved for these values, in aqua regia or the HCl/bleach or the HCl/ concentrated peroxide method of my choice.

The cooking down of the copper II chloride solution to dissolve pins will end up becoming an acidic solution of copper I chloride, and if iron, or if kovar is involved the solution can be an iron chloride and copper I chloride in solution, strong heating with iron solutions can also from solid iron hydroxides, the thick green/brown/black solution if water or dilute peroxide added precipitate some copper salts, if HCl added these salts will dissolve, iron chloride will stay in solution easier than copper salts, except t for the iron hydroxides (which are very hard to dissolve into any acid including aqua regia, these iron hydroxides can be converted to iron metal powders or other iron salts by several methods if needed).

Hope this helps with your questions.

 

[crow king]

Thank you for replying Butcher. Our dealing with the AP method mirrors your answers you gave. The CU in transition from II to I readily changes with contact from either H20 and HCL. Enough HCL and it should return to Copper II Chloride. And allow for any recovery of cemented gold in solution.

Can you tell me in your opinion when gold is in solution in AP, does it require total saturation of CU before all AU is cemented or does AU cement out as soon as copper II is introduced into the solution borrowing ion for ion?

Can you tell me when a test with stannous is done on AP does the CU affect the reading?

 

[butcher]

Gold chlorides can be dissolved in solution in solution along with copper II chloride solutions, if the oxidizer is strong enough to keep the gold in solution, (adding more copper can push out the gold from this solution as a black powder, which would plate to any remaining un-dissolved copper metal, or if the metal remaining is dissolved and the oxidizer not supporting keeping the gold in the copper II chloride solution will fall to the bottom of the vessel as black gold powder, usually with the white powders of copper I chloride, silver chloride, lead chloride and sodium chloride, if these are involved (mixed with these other salts gold powders can and these salts can look brown in highly acidic solution and turn white when washed with water).

Edit to add: I have made several posts on how to deal with these white powders and how to tell what they are and how to separate them, also have several posts on how to deal with colloids or tin in the process, but I have not discussed that here.

The stannous test will indicate gold in solution, as long as there is not too much oxidizer that would re-dissolve the gold back into the solution of this test, and as long as the gold is actually dissolved gold chloride and not the colloidal gold being held in solution, (colloidal gold is reduced to gold metal and will not react with the stannous chloride test).

Copper I chloride (solution) usually will not hold gold in solution, if the solution is clean of organic material and oils, and if tin is not involved, this is the dark brown solution before rejuvenating your copper chloride leach, gold will be the powder in the bottom with the other chloride salts (diluting this solution with water the copper I chloride powder will precipitate and solution change back green), but if this dark brown copper chloride has organics involved or tin in solution it can hold a considerable amount of gold, as colloids, these will not precipitate and cannot be tested for with stannous chloride (this can be where someone can lose a lot of gold tossing it with their waste), colloids are hard to deal with, filtering is usually very slow and a major pain, high heat and high acidic conditions can help, and incineration of powders along with boiling HCl treatment will also help, it is much easier to remove these problem before you leach this material than to have to recover during your leaching process which is not an easy task and can easily result in losses of valuables, without your knowledge where your loosing gold that you worked so hard to get.


The stannous test can be done with copper in solution the green color of copper does not effect the reading too much, but again keep in mind oxidizer, or colloids can effect what you see or do not see.

 

[JH123]

Since the date of this original post we have not attempted anything else with this bucket. We had used a 5 gallon bucket plastic strainer 200 mesh to filter some of the thickened copperI upon looking at that filter this week we see the edge of the filter is coated with gold in black powder form as well as gold colored flakes. So perhaps a leprachaun hasn't stole our gold. My plan is to rehydrate the copperI with 25% HCL and then filter out the gold.

BUTCHER said "Copper I chloride (solution) usually will not hold gold in solution, if the solution is clean of organic material and oils, and if tin is not involved, this is the dark brown solution before rejuvenating your copper chloride leach, gold will be the powder in the bottom with the other chloride salts "

BUTCHER said "I will use old copper chloride solution, sometimes cooking it down thick dissolving copper, iron, and other base metals"


What gets me is I thought I had filtered this before we let it sit for a month and evaporate dry. The AP was as much saturated at that moment with cu as it is now, though it went to copper1. Could this be what you spoke of in my quote of yours above? That I had an organic material, oil, or tin holding my gold, or am I misunderstanding what you wrote? Is there any way that when the AP returns to a saturate of CU2 that the gold would not be in its blackpowder form or could the change from CU2 to CU1 expell it from being insolution, or am I wrong with assuming from my 2nd quote of yours that the disolved base metals will not return to their former selves where they can "hold" my gold while in solution in refrence to your 1st quote? Which would mean my AP in CU2 form wasn't really completely saturated, which gets me back to the question does it require 100% saturation or does the ion for ion I stated above hold true in this?

Also this is the bucket that when we added the plastic housed card slots in, it ate some of the plastic and left a film on the bottom of the bucket. Also when we were trying to saturate this AP with copper we kept the bubbler running full time. Would this be an oxidizer that could have held the gold insolution?

 

[butcher]

JH123,
I have not gone back and read all that we have discussed, and my memory about what was said is not good, I did catch that you had a dirty solution of copper and other base metals with tin and plastics, so I will just give this advice based on that.

If you have dry or very concentrated powders or solutions neutralize them with NaOH solution the sodium hydroxide will help to neutralize the acids and powders, and will form NaCl and water in solution, which can be washed out, the remaining powder will form base metal oxides and hydroxide a in with the gold powders, wash out the salts in hot water washes till solution is clear.

Then you can dry these powders on low heat In a corning, or vision ware dish on hot plate or some other suitable vessel, (almost the whole process including incineration can be done in this vessel on the hot plate, a gas flame hot plate is best for incineration along with a handheld torch, but I like the heat control of an electric solid burner hot plate for dissolving and washing powders, decant solutions from the well settled powders, using your suction bulb tools and then you do not have a need to remove powders from the dish almost the whole process, unless screening out clumps or un-dissolve elemental metals), incinerate the powders once dry, this will improve the condition of the material, where most of the base metals will oxidize, tin and copper salts can then be more easily dissolved in boiling hot HCl, washing.

In the process of the hot HCl wash (after incineration), if you are picking up a lot of copper salts, the first solutions will be dark brown to almost black dissolving the copper as copper II chloride and copper I chloride into solution, as you remove this copper and base metals the solution will change to a lighter green almost blue color use the hot HCl washes until you see that you have removed most copper salts (dilute the HCl wash before decanting with just a little portion of water (not too much water as we really do not want to precipitate the copper I chloride, which we pick up in solution at first, we also want to let powders settle well first before decanting ,or removing this solution to another vessel, also keep in mind we may have traces of values being carried over in with the decanting so keep this in mind to check the for them later, before decanting your solutions of dissolved metals you should lower heat so that the boiling action does not keep fine powder stirred up in solution when you decant, the idea is to only remove dissolved metals and leave un-dissolved powder, but the idea is also to decant the solution while still as hot as possible so more metal salts are dissolved in the solution and also other chlorides like lead are removed in the process, wash until color of solution indicates you can not remove any more metal with acid or water rinses used, with boiling hot water rinses the lead salts can be removed.

Harold and I have posted much more details on this process, and you can also find details in Hoke’s book,.

After the incineration and HCl treatment, what to do next can depend on what other metals you have in the powders, which materials you processed originally.
I did notice you stated this material is from HCl acid peroxide (copper chloride leach), so I assume electronic materials are involved, and you would not have a large volume of silver to deal with, (in this case I see no need to neutralize, rinse and re-incinerate for a nitric treatment) and washing in the hot HCl till color of solution indicates most base metals are removed should clean the powders up fairly well, if you had no un-dissolved base metals or elemental copper metal involved you can try and dissolve a small portion of these powders in a test tube using HCl/Bleach the color is a good indication of whether your powders are clean enough to dissolve the bulk of values, or if this test is too green, or dark brown Etc. and it would be best to go back and remove more base metals first, if very light green or yellow in this test tube you may then decide to put the larger batch of gold powders into solution as dissolved gold.

Also consider you may need to refine these powders twice after this process of removing the base metals.