HCL/CL Problems

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M

muddle171965

Member
Joined
Mar 2, 2012
Messages
10
I just want to say hi to everyone first and to report back on my my attempt at the HCL/CL process. I had to clean my gold that was from my cell, three more times in HCL with heat and at least a further three times with H20 and then finally once more with distilled water, before there was clean water when everything settled. I then proceeded to two further HCL washes before I tried the HCL/CL process. I used a low heat and what seemed like an endless amount of CL before my powders dissolved and turned a deep orange! I then proceeded to dissolve SMB in warm water and precipitated my values. There seemed to be a fair amount drop to the bottom but to be on the safe side, I left over night to completely settle. I was really sure it all went ok until I checked the solution today. The precipitated gold seems to have dropped out still very black! There also seems to be a lot less than when I started! Can anyone tell me what the difference is between a deep orange solution and a deep yellow one? I presume the deep yellow is the better of thje two?

Thanks for giving me the courage and incentive to get this far and I really enjoyed the process of dissolving my gold even if it didn't go as well as expected!
Leigh
 
First of all you should do your drop in a cold solution. If you think you didn't get a complete drop then add heat. I have run into the same problem with having to use what seemed to be a larger volume of Cl than normal. Before the drop did you make sure that you eliminated the Cl in solution? What did you process in the cell? That's all I can help with. The questions that I asked may help someone with a broader knowledge help you further. John.
 
Hi John and thanks for the reply, I did not realise I had to rid the solution of the CL before I precipitated?! I started off with a cold solution but because it wasn't dissolving, I tried it on a very low heat and then it turned a deep orange and seemed to dissolve. Can you explain what you mean when you say, get rid of the CL in the solution please?
Thanks for your help
Leigh
 
free Cl will either stop the gold from precipitating or cause it to dissolve again back into solution.after you dissolve your gold in hcl/Cl, you should let the solution sit uncovered at least over night if everything went perfect. it sounds like you had to add more Cl than was needed so the wait time would have been longer.if you are in a hurry, you can warm the solution to a steam and keep it there for an hour or longer to drive off any free CL. just be sure not to let the solution boil or evaporate dry. after the heating period, let the solution cool and add at least double the volume of water and then add the SMB.
 
I saved the solution I poured off after the failed precipitation, can you tell me how I get the rest of my values back? Do I need to heat it to get rid of the CL in solution then add double the amount of water as you suggested?
Thanks for your help
Leigh
 
Geo answered for me on your first question, Thanks Geo! 8) Just let your solution rest open for a day or so to allow the Cl to leave and test with stannous. If you get a positive read add a small amount of SMB, stir vigorously and let it settle. See if you get more precip.
Let us know how it goes.
 
This is a test for chlorine.

Heat solution suspected of containing chlorine, to the point of seeing fumes evolve.

Hold a plastic cap (lid) half full of ammonia next to these fumes.

When the gases of these two mixes you will see white smoke of ammonium chloride.
 
Thanks everyone for your time and help, it can be so frustrating at the beginning, i'm sure you all must have been where I am! I have admittedly jumped in at the beginning but then started from the basics, studying safety, Hoke and her teachings and various other books, building my equipment slowly and thought I was ready for my first complete refine! I just wanted everyone to know that I have tried to start slow but obviously missed one simple part of the process but thanks to everyone hopefully I can save any values! So here's a big thanks from me!!!!
Kind regards everyone
Leigh
 
Leigh just remember one simple thing, you only lose values if you either throw them out or boil them off, if you dissolved values they are always there and can be recovered.
 
I personally use a catch barrel that is slightly acidic and containing steel wool to catch values that might be missed.
Dr. Poe
 
thats simple, the steel goes into solution and the values come out. the only problem with this is, if you deal will dirty solutions (contaminated with copper) the steel will precipitate the copper too. i would recommend using copper first to precipitate values.
 
Geo said:
thats simple, the steel goes into solution and the values come out. the only problem with this is, if you deal will dirty solutions (contaminated with copper) the steel will precipitate the copper too. i would recommend using copper first to precipitate values.
Click to expand...

Geo, that's what I thought. I think I'll stick with the way I'm already doing it. Thanks, John. :roll:
 
Dr. Poe said:
I personally use a catch barrel that is slightly acidic and containing steel wool to catch values that might be missed.
Dr. Poe
Click to expand...
That's the stock pot I speak of regularly. It need not contain steel wool. Any scrap steel will suffice. Much cheaper, and every bit as effective.

Harold
 
A couple thoughts :
1. there is ALWAYS lead in the residue from a cell if lead is used as anode/cathode. leaving some sulfuric will form insoluble lead sulfate which will filter easily after HCl/Cl - no need to get rid of all sulfuric
2. I don't recall if you were washing with HCl or not - if not, disregard this. otherwise, nothing else is gained by performing HCl washes - in fact, you could be adding problems. the boiling water washes remove most water soluble sulfates; everything else will be picked up in your 2nd refining
3. usually, for me, when my cell residue is slow to dissolve, its because it is pretty contaminated with base metals. I have either run items too long and/or run my cell too hot. when the residue is pure it takes very little time/Cl. alloy everything to settle/cool well (I add ice) and filter until absolutely clear. follow the above steps to make pure all Cl is completely dissipated.
 
Hi everyone
Just wanted to say thanks for the extra advice, I am in the process of moving house so iv'e not been able to report back on any results! I have heated the solution for an hour then left for a couple of days to make sure all the Cl has evaporated from my solution. I then had problems testing my solution! The solder I had was not testing conclusive so I am waiting for delivery of some decent powder to test properly. I had a very old roll of solder and I think it may have become either contaminated or was just old and possibly starting to deteriorate! Until that arrives, I have put that solution to the side for further testing before precipitating any values. You have all helped me along and I thank you all for that! There is also mentioned above, an answer to a seperate problem iv'e had with a batch of cpu's I processed in Ap. The gold is covered in a grey coating that iv'e been trying to remove for a week now! I don't want to double post so I will leave it at that but just wanted to say thanks for getting me thinking! I have had no internet for the last week so iv'e been constantly studying all the books and literiture iv'e downloaded over the last few months! The generosity of this site and the help given by everyone is invaluable and I for one appreciate the dedication you all have and the he;lp you all freely give!
Thanks to everyone!
Leigh
 
muddle171965 said:
Hi everyone
Just wanted to say thanks for the extra advice, I am in the process of moving house so iv'e not been able to report back on any results! I have heated the solution for an hour then left for a couple of days to make sure all the Cl has evaporated from my solution. I then had problems testing my solution! The solder I had was not testing conclusive so I am waiting for delivery of some decent powder to test properly. I had a very old roll of solder and I think it may have become either contaminated or was just old and possibly starting to deteriorate! Until that arrives, I have put that solution to the side for further testing before precipitating any values. You have all helped me along and I thank you all for that! There is also mentioned above, an answer to a seperate problem iv'e had with a batch of cpu's I processed in Ap. The gold is covered in a grey coating that iv'e been trying to remove for a week now! I don't want to double post so I will leave it at that but just wanted to say thanks for getting me thinking! I have had no internet for the last week so iv'e been constantly studying all the books and literiture iv'e downloaded over the last few months! The generosity of this site and the help given by everyone is invaluable and I for one appreciate the dedication you all have and the he;lp you all freely give!
Thanks to everyone!
Leigh
Click to expand...

The solder will not go bad. The out side might get dirty with grease dirt and grime, just wash that off and make you another batch. Add enough solder when you are making your solution that you have some undissolved in the bottom of your container when te reaction stops. Then filter your solution and test again.
 

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