Need help with HCL/Cl process-Please!

[Ignatz61]

I am having a very difficult time getting my gold to drop from 5 gallons of diluted auric chloride. ( I expect it to contain about 1.25 oz of gold)
I know I have some copper in it as it is blue in color. I will refine it again once I get a parcipitant.
I watched Steve's video and have read Hoke and Ammen and I just can't get it to work right.
In a beaker with 500ml of the AuCl I tried SMB ( after letting it sit for 2 days) nothing happens. My PH is around 1. I raised the PH with baking soda and as it got closer to 7 the top of the fizzing foam would temporarily turn brown. Encouraged by this I continued to add baking soda.
Finally, I got a dark brown solution and after a while a brown powder settled to the bottom. I checked the PH that this happened at, it was 7.
I was under the impression you needed a slightly acidic solution?

Can someone tell me if I raise the PH to 7 will I jepordize anything?
I am using paper strips so my PH numbers may not be exact.

Thanks for all the help, I rely on this forum often.
John

 

[Harold_V]

I'm troubled by your comments about blue color. If you have that much gold in solution with copper, it won't be blue, it will be green. I am of the opinion that you do NOT have gold in solution, that if you started with gold it precipitated long ago.

I suggest you add HCl to get the pH back to acidic, then test with stannous chloride. You make no mention of having done so. Did you?

If not, by now you should know that it is not wise to process without constantly checking your solutions so you know if you have gold, or not.

Harold

 

[butcher]

might just add HCl to a portion and test it if batch is large,this way you know before using alot of acid.

 

[Ignatz61]

Ok,
Here is what I did.

I put clean never used scrap 14K goldfilled wire (2 lbs 14oz) in HCL/Cl. The wire fizzed and when it was copper colored I took it out. I did this in several batches but combined the solution into one bucket. The HCL/Cl turned yellow at first then green then blue upon diluting with tap water.
See Picture #2
I have not changed the PH of the bulk of my solution only small test batches. It is still ph ~1. My stannous chloride testing is --well I need some practice. I don't have enough confidence to believe the reading yet.

If the solution is barren then what is the brown precipitant I get when I use SMB at PH 7? Could it be copper?

Also I put 1lb 2oz of the same wire in my sulphuric cell and (while I am not done yet) I have a nice amount of black sludge about the same amount that yielded 1.41 oz 18k gold (touch stone test).
So I know the material has a fair amount of gold.

So now I am wondering if the gold did not strip off but was discolored by the hcl/CL?

I also put 2 stainless steel plates in a small beaker of my blue solution and connected to 12V 1amp power source. The solution turned green as copper plated out on the Cathode. Iwas a wierd soft spongy coating but deffinately copper. SMB turned it brown but so far no precip.

 

[butcher]

if you did not dissolve the metal completely you may not have much gold at all in solution. when you dissolve the copper and gold both will dissolve but gold in solution will plate back to copper still not dissolved. if you pulled that out then that can be where your gold went.
and in the plating part you did you can also plate out the gold and copper both.
too much Sodium metabisulfite will precipitate copper, and copper can be brown to black, or even a white powder depending on the chemistry, at PH 7 you can start to drop all kind of metals, it has no acid to keep them dissolved some may stay till PH9,or more, and some will redissolve as hydroxides. at higher PH.

I would sit my solution aside untill I understood what I needed to do.uneducated expieriments dont get your gold, if you have understanding of principles then expierimenting can prove effective,
try making a known solution of gold, and some stannous chloride, then do these expiriments to get to where you can find gold in solutions, do not discard your solutions, till you find it and can test them.
the picture with blue liquid is copper in solution but seems dilute by color, the gold dissolved is plating back to the copper in bottom of bucket.

 

[Oz]

I agree with Butcher that you should take the time to become confident with stannous testing for gold before proceeding.

You can get some reasonably pure gold for making a control solution in a test tube by recovering some foils from fingers in AP. It takes very little gold in a test tube with the dissolving acid of choice that will keep well. Stannous does not always keep so well but whenever you make it you can test its effectiveness against your standard gold solution from foils, if it reacts with it then you know that it will perform properly.

Stannous is one of your best friends allowing you to “see” into your solutions. Without it you are hard pressed to be able to know when solutions are barren and safe to discard.

 

[Ignatz61]

Thanks guys,
I will make a standard and practice with the stannous.
I am also going to run the wire from the HCL/Cl solution in my cell to see if it has the gold still on it.

I read about gold cells in Ammen's book. It uses HCL as an electrolyte so I figured I woul give it a shot. The first plated piece I put Nitric acid on to see if it was copper or gold or a combo. The plating disolved completely so I am convinced it was all copper. I guess that will need testing now to see if there is gold in it now that the copper is out of the way.

 

[Harold_V]

My stannous chloride testing is --well I need some practice. I don't have enough confidence to believe the reading yet.

Then you shouldn't be attempting to refine. That's like taking a cross country trip in a car when you don't know how to drive. That makes no sense to me------and it shouldn't be making sense to you. You should make every effort to avoid instant gratification in this venture. You must understand the fundamentals if you intend to enjoy success.

Concentrate on testing until you understand it, and read Hoke until the book makes sense. No one can predict what is happening, or has happened------it's up to you to determine where your gold is. As each person second guesses your predicament you'll be lead down countless paths, all of which can be avoided by you doing your part first. You can do that easily if you'll read Hoke until you understand how to test.

Once you do, you'll be able to determine where your gold is and come up with an effective way for it to be recovered.

All of these processes are so simple if readers would take the time to learn them before jumping in with both feet.

Harold

 

[g_axelsson]

...
too much Sodium metabisulfite will precipitate copper, and copper can be brown to black, or even a white powder depending on the chemistry, at PH 7 you can start to drop all kind of metals, it has no acid to keep them dissolved some may stay till PH9,or more, and some will redissolve as hydroxides. at higher PH.
...

I'm starting to see what I did wrong at my last refining run ... at which pH should you drop the gold?
The white powder copper is what I probably got the last time I tried to refine gold. What is it exactly and how do I get rid of it? My white powder survived an acid wash with HCl.

/Goran

 

[qst42know]

Ignatz61

HCL/CL is a dissolve everything process. By pulling any base metals out early the bulk of your gold likely went with it.

Your scrap wires from the HCL/CL with cemented gold on it will not act predictably in your cell.

Adding nitric to these wires without destroying the HCL by incineration first will not prove it is just copper either.

Jumping from one incomplete process to another incomplete process will only add to a significantly large volume of hazmat waste. And you won't have anything to show for your efforts.

Even your blue solution bucket looks to have wires in it.

Slow down! Chose one process and learn to run it to completeness.

I hope you have studied the health effects of the poisons you are toying with. Nothing from your photos indicate that you have.

 

[Ignatz61]

Yes, I agree I need to progress more slowly.
Yes , I agree I need to get a better handle on testing and basic reactions.
In fact I am making a gold standard solution and fresh stannous chloride.

I am aware of the dangers involved with these chemicals and processes .
I have a fume exhuast, a resporator and I am in a separate building far from any living spaces.

That said, Thank you for your concern and guidance. I am fascinated with refining and sometimes get ahead of myself.

The HCL/Cl process ---I knew it was a "dissolve all" process. I was hoping to short cut it to dissolve only the surface ( gold and a little copper), as a way to refine all this gold filled wire I have. Thats why I pulled the wire out once the reaction slowed. Now I know better.

The blue solution does test barren! With fresh stannous and a standard to compare to I can verify that my method was a flop!
I still have all the wire. Any suggestion on how best to get the gold off of it? I promise to take it one step at a time.
Thanks again for all the help.
John

 

[Oz]

Ignatz61,

I am glad you now have a gold standard solution to test your stannous with and have made progress in using it.

I would have been amazed if you told us you had found gold in solution with your blue bucket. In your picture you have what looks like undissolved base metal, if so your gold that did make it into solution would have precipitated out on the base metal as a black powder.

Stannous will not detect this black elemental gold, only gold that is dissolved in solution. Beware you do not throw the baby out with the bath water. This is why it is so important to be able to use stannous to “follow” your gold.

 

[butcher]

thanks fellers you explain things well, thats what I was trying to do :shock:

 

[qst42know]

Ideally the sediment and half processed wires should be incinerated to destroy any HCL present. The remains treated with nitric to finish removing the base metals. And then dissolve in HCL/CL.

You could rescue the unfinished wires and sludge using HCL/CL allowing it to completely dissolve this time. Be aware that it will likely not drop clean from this dirty solution and will need refined a second time.

Your plated wire seems better suited to run in the stripping cell. A cell strips the surface only.

Me personally, I would not work over a carpet. Cardboard or thick paper is easier to ash to recover spills. Alternately working in the lid of a storage container can contain small spills and drips for recovery. For safety cover any other buckets of solution you are not working on.

 

[Ignatz61]

Qst42know- I thought about redoing the HCL/Cl and letting it dissolve everything also.
I think now I am going to go back to the Nitric acid for this batch but the cell seems a better choice for me with any new wire. I do like the fact that nitric is clean. By that I mean what is left is pretty pure gold. But the wire is a pain to cut up into small pieces.
What I like about the cell is I generate very little waste solution, and I have been getting very clean parts coming out of it.

I don't work on carpet, I just moved a bunch of stuff out of my way and set the blue bucket down for the picture, otherwise I slide it under the bench top. The other buckets contain dry parts that have been stripped and are waiting for me to have the time to go through looking for any spots that were missed, some I found have more gold inside so they are waiting for me to come up with an easy way to crack them open.
I actually work on a concrete top with a hard plastic on the floor. Spills are wiped up and the paper towel saved with the filters. When I dilute the acid from the cell I do work in a big glass jug inside a big tray just in case. An exhuast hood is mounted on the wall. It works good but I am working on a fume hood. The Nitric and HCL/Cl work I do outside.

 

[qst42know]

No offence intended. I would rather mention safety issues than hear of someone injured or worse.

Anyhow is your plated wire on a spool?

If it is you could rig a submerged plastic wheel and reel it slowly through a stripping cell. Just a thought.

 

[Ignatz61]

None taken

I like the way you think! I had a similar idea for processing photographic negatives. Feed them like a sheet of paper in a printer only nice an slow!

Anyway here is a picture (blurry) of the rats nest I am dealing with.

The problem is I need yield data and so far things keep going wrong or taking too long....

My Gold filled Karma is still bad. I tried to melt my sludge from 1 lb of wire put through my cell. My little electric melter is broken so using the big furnace - little crucible- spilled gold I can get most of it back after cleaning the furnace but this means back to the drawing board for accurate yield data.

 

[qst42know]

What is the scale of your wire ball?

Just a guess but that's what happens when a chain former runs too long unattended?

I hope you refined the material from the cell. In which case you can weigh the dry powder without melting.

 

[Ignatz61]

yeah, Thats the powder that was spilled in the furnace.

The wire is around 1/16" diameter

 

[qst42know]

If I had to prepare this for a cell I would drive a large spike nail through the center. Then with a hay hook or something like one I would pull and stretch this into as near a flat sheet as I could. Tamp it with a mallet and then run it in the cell. In it's present form the inner wires would be fairly well shielded.