Refining Gold from Gold Filled Jewelry

[Geo]

i dont see a problem with dissolving those at the same time in the same solution.the problem arises when you go from a hcl solution to a nitric solution without first incinerating the material.or from nitric solution to hcl solution for that matter.you cant rinse acid from your material,for instance,if you used AP to process gold plated items and you wanted to insure the base metal was gone it wouldnt be wise to go straight to a nitric acid wash because as you know nitric acid and hcl acid make AR.your expecting to wash your foils to remove any base metal left and instead you dissolve a portion of your gold.if you didnt know that in advance you may neutralize and discard the solution containing your gold.and if you had dried and weighed your foils after rinsing with water thinking you removed the hcl and then washed in nitric you would be wondering where your gold went.

 

[philddreamer]

"Could someone tell me why It's a bad idea to run my gold powder that I got from the sulhuric cell through with the values recovered from the nitric treatment of the gold filled jewelry?"

I don't think its a bad idea, if I'm recovering the gold, not refining it. I've done it, & noticed no problem. Someone please correct me if I'm wrong.

"I know that HC/Cl of the powdered gold has been recommended. I am fine with that, I just would like to know (why is it best) to use HC/CL on the sulphuric cell powder and the AR on the values from the nitric process. This is just so I can understand why? Thanks to anyone who will answer. Oneal58"

HCl/Cl is mostly recommended because is cheaper than AR & the chlorine is easier to get rid of before trying to precipitate. It's a process the noobs can learn to "handle" quicker. Also, some folks can't afford the nitric or can't find it; HCl & bleach are very easy to find, so its the easiest alternative to AR. Keep in mind that HCl/Cl takes longer to digest the gold.
We all have a preferred process for dissolvong gold, mine is AR. HCl/Cl when I'm cleaning filters, or dissolving gold from chinaware...

Take care!

Phil

 

[butcher]

Oneal,
You could do these separate for less trouble, or combine them.

Here are some things to consider helping you to make the decision.

Much of what I chose next would be decided on how much base metals I may have in these powders from the two different processes I used earlier.

I would most likely wash both recovery’s of gold well and mix them together, but realizing that there could be traces of nitrates in the mix,(this could be dealt with), after a good wash of the powders you could incinerate the powders and avoid that trouble of nitrate's.

Now do I have tin that may give me trouble? If so a boil in HCl, then dilute and settle and decant then hot water wash settle decant repeat till clear, and re-incinerate (if going back to nitric wash later).

Think about this is if using HCl/bleach you do not want to evaporate too much or you will have salts to deal with (not that big of deal).

Which process I chose next would have several factors to think about, how much base metals are left? HCl/bleach is easier but I would not be able to do another wash with nitric acid to remove these base metals, (unless I wanted to deal with traces in this solution later, not that big of deal, but do I want to go there?).

I could go to another nitric wash and then aqua regia, but here I will have to eliminate the nitric acid by slow evaporations, and this is harder for beginners to deal with and precipitation is also harder for beginners (as they may still have nitric in solution) which way or process do I choose?

After incineration you could use HCl with small additions of bleach used to put gold into solution this is much easier to deal with (than aqua regia), but if you still had some base metals that your washes may have missed, they would also report to this solution, as long as there was not that much base metals the process will work fine and I can do another refining for purity.

Or after incineration you could heat in HNO3 70% and water 50:50mix, then go to aqua process (more difficult) which way do I choose?

I think HCl/bleach would be my choice.

 

[Oneal58]

Hi kadriver,
I have the black powder now out of the sulphuric cell. I also have the foils from my first nitric acid treatment of the gold filled jewelry. I can't seem to get any answers on some of my questions on the forum. I hope you can help me.
I have the black powder from the sulphuric cell and the foils from the nitric bath of the gold filled jewelry.
Do I use 2 different type processes here, 1 for the black powder, (HCL/CL) and 1 for the foils, (AR). Then decant and drop the gold>
Is the answer to the question is that the gold black powder from the cell is too pure (high karat) for the AR to attack?
Will a nitric bath for the black powder help any, I might have dropped some silver and other metals along with the gold when stripping with the cell?
Am I missing any steps in the process?
Is this the best route to take with each. Could you tell me why the 2 different processes is recommended? I need to know this , just for me, for the sake of knowing it?
Thanks Kadriver,
Thanks, Oneal58

Oneal58:

I recall having to allow the acid in my stripping cell to settle for several days like Phil pointed out.

Eventually you could see through the acid and the black material had collected on the bottom of the cell.

The acid was not crystal clear, it was still dark, but transparent.

I have saved a bunch of gold plated jewelry that has been accumulating. I may have to get the sufuric acid stripping cell set up and get it running again.

I think December 2010 was the last time that I ran it.

Back then I was too green and anxious to have to wait for the black gold powder to build up in the cell - let alone the idea of having to wait for it to settle.

Since I have gained a little more experience, hopefully I have gained some patience.

thanks - kadriver

 

[Oz]

I am going to skip any answers to your questions and ask instead why I see so much of your processing (in your first picture) that looks like your primary work space is occupying indoor living space. None of this is worth your health or that of your family’s.

 

[Geo]

Oneal58

i wish you the best of luck.i hope you figure all of this out and look forward to seeing your first gold button.i will not clutter your thread with my useless post anymore.

for all the other members, if there are any that can and are willing to help Oneal58 please try and help him figure out this puzzle.

 

[Oneal58]

Hi Geo,
Please forgive me if I have offended you in any way. If I did I didn't mean to. I very much appreciate your post and look forward to each and every one of them. I check my computer many times a day for post on the questions that I ask. I am still learning how to use the site. After taking another look at previous post on this thread I see where you have answered this question that I had been trying to get an answer to. I am very sorry, honestly. Please don't stop posting and helping me. You have been in there for me for many, many post and I apppreciate you trying to help me. But I have had a couple of heart attacks and they have changed me. I have a tendency to get tunnel vision and overlook things, such as your post to answer the question I asked. It wasn't because I didn't seek your advice or want your advice, it was just that I didn't see it. Please don't leave me hanging here. I need everyone here on this forum and the last thing I want to do is offend anyone. If I offended you, I am sorry. Will you accept my apology, it is heart felt.
I need to say when I asked kadriver the question, it was because I didn't know where else to turn. It seemed as though nobody was reading my post and some of the questions I asked I could not get answers to. I drove to meet with Kadriver and know him. He is the person who gave me a lot of material to get me started. When I thought no one was looking at my post I had no where else to turn but to someone who I thought would help me and I knew.
But thank each and every one of you. If I have not thanked all of you in every post it was just an oversight and I am sorry.
Oneal58
As far as my working space it is an old house that my mother lived in. It is on my porperty and I started to tear it down last year. The termites have done a number on it but I still use it for storage. I would not dare bring this operation inside around my grand's or my wife.
Member's on this site, please do not take me wrong, I really don't know how I sound to others reading what I post. I may sound arrogant, selfish, dumb, I just don't know? But I know one thing for sure, I need each and every one of you. Your help is not taken for granted or unappreciated, no matter how it may sound on these post. Thank each and every one of you for your help and your post. Please don't take me wrong, I am not that way.
Thank You, Oneal58
A

Oneal58

i wish you the best of luck.i hope you figure all of this out and look forward to seeing your first gold button.i will not clutter your thread with my useless post anymore.

for all the other members, if there are any that can and are willing to help Oneal58 please try and help him figure out this puzzle.

 

[Oneal58]

Hi Butcher and everyone who has been helping me. I truely appreciate it.
After close inspection of the material that came out of the nitric bath I can see that there are still pieces of grey metal on a good bit of the gold. I went ahead with the advice to combine the 2 and give both the sulphuric cell values and also the values that needed a little longer in Nitric. I have got the material in the nitric bath now. It's cold here today and I have had to heat the nitric to get a reaction.
Question 1- The color of the first bath in Nitric was a dark bluish geenish color. The color of this batch is almost a black color? Is it becasue most of the copper has been dissolved in the first nitric treatment?
Question 2-Butcher you said that I would have to evaporate the nitric by slow evaporations. Can I evaporate in the same flask as I am giving the material the nitric bath in?
Question 3-Do I dilute in some way by adding the nitic with values to water and then evaporate many times this way? After several evaporations do I evaporate down dry? That is once I am sure all the nitric has been evaporated?
Question 4- Then go with the AR or do I need to recover, incinerate and then go to the AR treatment
P.S.
Question 5- I did not do the HCL Boil for tin before the nitric treatment. Somehow I overlooked this. Can I do the HCL Boil for tin when I get all the Nitric out, then incinerate and do the HCL Boil for tin?
I know Butcher you said this was the hard route for beginners. But I am in this for the long haul with everyone's help. I want to tackle the process that I will be using on a regular basis from here on out.
Am I in line here or am I leaving out something?
If anyone wants to reply to this post I welcome it.
Thank you butcher, and everyone!
Oneal58
P.S., I left out the HCL boil for tin. Can I do the HCL boil for tin after I get all the nitric out before the AR??

I very much appreciate your post. I can't figure out why these post was not on my page untill this morning.
Butcher I just want to say I very much appreciate your help. I am seeing things more clearly now. Without you and the members of this forum I could not go on, on my own. Thank you Butcher for all your help. You have been there for me from the beginning and I appreciate you. I will follow your advice, Thank You,
Oneal58

Oneal,
You could do these separate for less trouble, or combine them.

Here are some things to consider helping you to make the decision.

Much of what I chose next would be decided on how much base metals I may have in these powders from the two different processes I used earlier.

I would most likely wash both recovery’s of gold well and mix them together, but realizing that there could be traces of nitrates in the mix,(this could be dealt with), after a good wash of the powders you could incinerate the powders and avoid that trouble of nitrate's.

Now do I have tin that may give me trouble? If so a boil in HCl, then dilute and settle and decant then hot water wash settle decant repeat till clear, and re-incinerate (if going back to nitric wash later).

Think about this is if using HCl/bleach you do not want to evaporate too much or you will have salts to deal with (not that big of deal).

Which process I chose next would have several factors to think about, how much base metals are left? HCl/bleach is easier but I would not be able to do another wash with nitric acid to remove these base metals, (unless I wanted to deal with traces in this solution later, not that big of deal, but do I want to go there?).

I could go to another nitric wash and then aqua regia, but here I will have to eliminate the nitric acid by slow evaporations, and this is harder for beginners to deal with and precipitation is also harder for beginners (as they may still have nitric in solution) which way or process do I choose?

After incineration you could use HCl with small additions of bleach used to put gold into solution this is much easier to deal with (than aqua regia), but if you still had some base metals that your washes may have missed, they would also report to this solution, as long as there was not that much base metals the process will work fine and I can do another refining for purity.

Or after incineration you could heat in HNO3 70% and water 50:50mix, then go to aqua process (more difficult) which way do I choose?

I think HCl/bleach would be my choice.

 

[Oneal58]

Hi Oz,
I am working out of a old house that I was going to tear down. It was where my mother lived and most the house has been damaged by termites. I appreciate your concern but I would not dare bring this type process into my home around my grands and my wife. I have even told my grands when they see Pops in the old house to not even come close to it. That it is really dangerous and could kill or hurt you or me. They are 9 years and 4 years old. I have instilled a fear of them going near the old house, which was my purpose. I wouldn't trade 1 of my grands, wife for all the gold in the world. You see, I have already lost my son due to a farm accident and a brother that got electrocuted. So, I realize what family means, it is my job to keep them safe. So, don't worry, protecting my family is priority #1.
Thank you Oz for your concern and thank you Oz for your many post. I really appreciate you and all your post. I appreciate and am thankful for everyone on this site. I can't say this often enough. Thanks to everyone.
Oneal58

I am going to skip any answers to your questions and ask instead why I see so much of your processing (in your first picture) that looks like your primary work space is occupying indoor living space. None of this is worth your health or that of your family’s.

 

[Oneal58]

Hi Phil, thank you so much for your postings. You are very much appreciated, I can't say this often enough. All of you on this site is very much needed and appreciated. Not taken for granted but really appreciated. I am very thankful for each and every one of you.
Thank you Phil for your many post!
Oneal 58

"Could someone tell me why It's a bad idea to run my gold powder that I got from the sulhuric cell through with the values recovered from the nitric treatment of the gold filled jewelry?"

I don't think its a bad idea, if I'm recovering the gold, not refining it. I've done it, & noticed no problem. Someone please correct me if I'm wrong.

"I know that HC/Cl of the powdered gold has been recommended. I am fine with that, I just would like to know (why is it best) to use HC/CL on the sulphuric cell powder and the AR on the values from the nitric process. This is just so I can understand why? Thanks to anyone who will answer. Oneal58"

HCl/Cl is mostly recommended because is cheaper than AR & the chlorine is easier to get rid of before trying to precipitate. It's a process the noobs can learn to "handle" quicker. Also, some folks can't afford the nitric or can't find it; HCl & bleach are very easy to find, so its the easiest alternative to AR. Keep in mind that HCl/Cl takes longer to digest the gold.
We all have a preferred process for dissolvong gold, mine is AR. HCl/Cl when I'm cleaning filters, or dissolving gold from chinaware...

Take care!

Phil

 

[Oneal58]

Hi Everyone, I just want to say that I don't know what happened to my postings. It seemed I was asking the same question trying to get an answer to and I had no responses? I don't know if my computer was updating correctly or what had happened? I just did not see the many post that all of you had put up for me. I still can't figure out why I didn't see the many answers I had gotten. Was the site updating correctly yesterday? I truely can't see how I overlooked them, but it happened. And I am sorry if I made any of you feel that I wasn't taking your advice.
When I wrote kadriver last night to ask him before I went to bed I honestly did not see the many post that I had received on the question. I thought everyone had either stopped reading my post or abandoned me, honestly!
I want to thank each and every one of you from the bottom of my heart. I don't know what I would do if you weren't here to help me. You take your time and energy to answer these post. Not because you have to or in some cases even want to. You do it to just help. That's a quality that few have and it does not go unrecognized. You are not taken for granted and you are appreciated, each and every one of you.
Thank You from the bottom of my heart for your help.
Oneal59

 

[Oneal58]

Hi Everyone,
I am right in the middle of a Nitric Evaporation and know that I cannot bring the solution to a boil, (Hoke's) I can no longer see brown fumes comming from the solution.
Question 1- Does this mean all the nitric has worked off. I have the amount of water left in the beaker. This has taken all afternoon. I have kept the container covered the whole time. Venting through a wet cloth.
Question 2-I need to treat the solution for tin, can I add HCL now while the solution is warm? There is about 300ml of solution in the container, how much HCL to add if this is the right thing to do? Or do I wait to treat with sulphuric during the AR process?
Question 3- Once treated do I decant, filter, wash, incinerate and then go with AR?
Am I on base?
Thanks to anyone who has the time to answer.
Oneal58

 

[Geo]

i have a question.when you say evaporating nitric are you talking about from an AR solution?

is this the process you were doing of removing base metal with nitric acid?

If so there is no need to evaporate the nitric as that is only needed in an AR solution. If you add hcl acid now you will create AR and dissolve your gold. IF this is a process to remove base metal with nitric acid and all the base metal is dissolved and your left with gold and perhaps some salts now is the time to turn off the heat and let the solution cool. Test with stannous chloride to make sure theres no gold in your solution. Dilute your solution with tap water 50/50 and reheat to a slow boil to dissolve the salt. Turn off the heat and let everything settle. Decant as much solution as you can without pouring out any foils or solids. Add water and return to the heat and bring to a slow boil. Repeat this until the rinse water is clear,do not add hcl acid. You should be left with clean gold foils and powder. Now proceed to the refining stage.

 

[goldenchild]

Since it sounds like you've done your homework I will offer my help.

1. No brown fumes usually mean no more nitric but then again there could be some left in solution. You're supposed to periodically add HCL to an evaporating solution to drive off nitric. More specifically when the solution becomes more viscous. HCL is actually exhausted letting no more nitric evaporate out of solution, hence the additions of fresh HCL. This is even more evident when an AR digestion comes to a halt but there is plenty of nitric still in solution. An addition of fresh HCL will start it right back up. Don't go overboard with evaporation. The HCL doesn’t have to be like maple syrup before fresh HCL additions. This is one of those things you will learn from experience.

2. Its highly advised to get rid of the tin before you digest with AR or you will end up with a big mess. Remember tin reacts with gold chloride to get that nice purple color. No imagine digesting tin and gold at the same time. An excess of HCL doesn't hurt so in an evaporating solution of say 300ml I would say to add 25 to 50ml of fresh HCL at a time. And yes you can and should add HCL while solution is warm. BE CAREFUL! Hoke states that a small amount of H2SO4 is added to the AR solution to hasten the expulsion of nitric and to drop any lead that may be in solution.

3. Once you are finished with steps 1 and 2 let the solution completely cool and settle. Some will chill the solution and others dilute with water. Decant and filter your solution. Precipitate and wash thoroughly. Follow steps 1-3 again if necessary.

P.S.
Learning to use just enough nitric to complete a digestion will make step 1 a breeze.

Edit
After reading Geo's post I have to now point out that 1-3 is AFTER you have recovered your gold.

 

[kadriver]

Oneal58:

I just finished a 2.4 troy ounce pure gold bar and shipped it out to the refiner today. i worked late last night and got back to it early this morning - self inflicted pressure. I called and got a price lock on the gold bar before it was refined and ready to go! So I was under pressure to ship it out by the end of the day today so the refiner would get the gold by tomorrow (Friday).

Anyway, I have briefly read through your posts here and this is my experience:

I have processed gold filled scrap only one time using HCl/CL. It was when I first ordered the DVD from lazersteve. I did it for the experience and I have not done it since. I have plenty of nitric acid and the AR treatment is something I am familiar with. AR=aqua regia

You can use AR to dissolve the gold filled foils. You can also use AR for the black powder from your sulfuric cell. I don't see any reason why you can't use HCl/Cl for either type of these materials also. I don't think it makes a difference.

I am currently in the middle of a gold filled recovery and refinement myself. I started with 260 grams of gold filled watch covers and jewelry.

I started by incinerating the gold filled scrap to redness. Then I added distilled water and then nitric acid (about 850 ml each).

I put it all in a coffee pot with a lid and "cooked it" for several hours.

I then let it sit for a day or so. Once settled and cool, I filtered off the liquid, allowing the "purple mud" the go into the filter at the very end. I took the clear filtered liquid which was dark blue, and neutrailzed it with Urea.

I put the filtered liquid in a large beaker and added a coil of copper wire to cemented the silver from the solution - there was about 1 ounce or so (estimate) of cemented silver in the liquid - it is still cementing as I write this.

I rinsed all the fine material from the coffee pot into the filter, but kept the foils and shells of gold in the coffee pot. There was a pale purple mud about 1/8 inch thick in the filter. I saved the filter, just left it in the buchner funnel.

I then re-treated the gold foils with some more (about 200ml total) dilute (50/50) nitric as some of the base metals had not dissolved completely.

Also, I found a chain I had saved from a previous batch from some months ago. The chain was saved because it still had base metal that was not dissolved. I added this chain to the foils in the coffee pot with the second 50/50 nitric treatment.

More red fumes came from this reaction confirming that base metals were present.

I cooked the batch this time for about 2 hours until no more red fumes were present and the solution was boiling vigorously. the solution was black this time - I think because of the chain, it may have had iron - I don't know.

Oneal58, I am pretty sure there is lead and tin are in my batch of gold filled scrap. I say this because of what I found in the filter paper from the first filtering of the liquid from the coffee pot - a pale purple paste that looks like lite purple silver chloride. I am thinking that this is tin and lead mixed with some colloidal gold and gold powder. The gold can be recovered from this mud according to Harold.

I would guess that there is a good chance that your gold filled batch also has these contaminates. Therefore, it is probably not a good idea to mix your two batches together - although I read where you have already done so.

A while back, Harold had written a post where he recommended that gold filled foils, mud, and everything should be sent to the filter - this is one of the only times that it makes sense to put all the material into the filter.

Once in the filter, Harold stated, that the whole batch should then be incinerated, filter and all - to get the gold mud - then the incinerated material should be treated (boiled) with full strength HCl.

Boiling in full strength HCl will get rid of the tin and lead that are sure to be present from gold filled scrap.

Once the treatment with HCl is complete, wash with water several times, then treat with aqua regia and proceed as usual with filtering and precipitation of the gold.

I hope I have not mis-quoted Harold on this. I have this process printed out and in a notebook at my shop and just happened upon it as I was reviewing.

The foils from the second cook are still sitting in the coffee pot in that black liquid. Tomorrow I plan to pour eveything into the filter as Harold recommended. Foils, gold mud, and anything else from the reaction vessel. Then I will let it dry and incinerate the whole mass - filter and all. Then treat by boiling it in HCl. Once complete I will wash with distilled H2O (Tap is probably OK here) and then dissolve in aqua regia.

I will let you know how this batch turns out. I am curious to know how it will turn out myself as this will be the first time I use Harold's process on this gold filled batch. i am hoping for good results.

I have done gold filled batches in the past were I rinsed out all the purple mud into the filter, then saved the filter. The foils were not allowed to go into the filter. I rinsed the foils in the coffee pot with plenty of hot water, then dissolved the foils only (no mud and no incineration).

The resulting gold bead came out OK, but it was not very pure and had a silvery coating on top, but it tested at least 22k. I think it weighed about 3 or 4 grams. i sold it on Ebay as 22k Gold and got about 80% of spot price for it with a positive feedback from the buyer.

I hope this is helpful to you. Aslo, I hope I did not mis-quote Harold on the process I wrote about above in this post!

kadriver

 

[butcher]

Oneal,
Everybody here wants to help< and all are giving good advice.
I see several problems, one you’re just learning and may not grasp the whole picture,
Some are giving advise based on the long wording in your questions, and then we may get mixed up on where you are or where your planning to go, so it seems with so many of us giving you directions (in this confusion) you will start getting pointed into many directions.

This way of helping you is confusing you and us.
Normally it is better to follow one person’s advice that know exactly what you’ve done and can just tell you what to do next.

You get a broad view with many members helping but it can also get confusing.

So lets get all on the same page or maybe let one person help here.

First we either need to make the questions and answers simpler.
Know exactly where you’re at and which way you wish to go.
Understand each step that has been taken.
And the direction we plan to go.
And we need to get all our answers pointing the same direction.

Please explain where you are please making it simple.
Explain your plan on process you intend to take.

The members helping can give better steps to take,

Oneal then you still may get a couple of different advice, so members need to know which plan your going with and the next steps, some of us may choose a different route so some answers may differ.

Hope this helps
This is a good thread for many to learn from, but can also become one to confuse them.

 

[Oneal58]

Thanks Geo, I need to let you know right where I am, how I got there and where I was trying to get to. I want to get on the same page with everyone. I might have mislead you and others on where I was and what I was trying to do plus which route I have taken and why. I will post tonight and try to explain what I have done to the best of my ability. Then you will know where I am. And would appreciate any advise on where I need to go from here. I feel that some may think I am going the HCL/CL route. I didn't go that route for the reasons I will post.
Thanks Geo, a new post will follow. I am sorry for the confusion I have caused.
Oneal58

i have a question.when you say evaporating nitric are you talking about from an AR solution?

is this the process you were doing of removing base metal with nitric acid?

If so there is no need to evaporate the nitric as that is only needed in an AR solution. If you add hcl acid now you will create AR and dissolve your gold. IF this is a process to remove base metal with nitric acid and all the base metal is dissolved and your left with gold and perhaps some salts now is the time to turn off the heat and let the solution cool. Test with stannous chloride to make sure theres no gold in your solution. Dilute your solution with tap water 50/50 and reheat to a slow boil to dissolve the salt. Turn off the heat and let everything settle. Decant as much solution as you can without pouring out any foils or solids. Add water and return to the heat and bring to a slow boil. Repeat this until the rinse water is clear,do not add hcl acid. You should be left with clean gold foils and powder. Now proceed to the refining stage.

 

[Oneal58]

Hi Butcher, I think I have not been clear on what I have done, how I got there and where I am trying to get to. I will be making another post tonight just to let everyone know where I am and try to find out where I need to go next. I will be posting to the best of my abilities where I am. Post will follow.
Thanks Butcher,
Oneal58

Oneal,
Everybody here wants to help< and all are giving good advice.
I see several problems, one you’re just learning and may not grasp the whole picture,
Some are giving advise based on the long wording in your questions, and then we may get mixed up on where you are or where your planning to go, so it seems with so many of us giving you directions (in this confusion) you will start getting pointed into many directions.

This way of helping you is confusing you and us.
Normally it is better to follow one person’s advice that know exactly what you’ve done and can just tell you what to do next.

You get a broad view with many members helping but it can also get confusing.

So lets get all on the same page or maybe let one person help here.

First we either need to make the questions and answers simpler.
Know exactly where you’re at and which way you wish to go.
Understand each step that has been taken.
And the direction we plan to go.
And we need to get all our answers pointing the same direction.

Please explain where you are please making it simple.
Explain your plan on process you intend to take.

The members helping can give better steps to take,

Oneal then you still may get a couple of different advice, so members need to know which plan your going with and the next steps, some of us may choose a different route so some answers may differ.

Hope this helps
This is a good thread for many to learn from, but can also become one to confuse them.

 

[Oneal58]

Thanks Kadriver, I need to let everyone know where I am, how I got there and where I was trying to get to. I want to get on the same page with everyone. I might have mislead you and others on where I was and what I was trying to do plus which route I have taken and why. I will post tonight and try to explain what I have done to the best of my ability. Then you will know where I am. And would appreciate any advise on where I need to go from here. I feel that some may think I am going the HCL/CL route. I didn't go that route for the reasons I will post.
Thanks Kadriver, a new post will follow. I am sorry for the confusion I have caused. Look for another post to explain where I am.
Oneal58

Oneal58:

I just finished a 2.4 troy ounce pure gold bar and shipped it out to the refiner today. i worked late last night and got back to it early this morning - self inflicted pressure. I called and got a price lock on the gold bar before it was refined and ready to go! So I was under pressure to ship it out by the end of the day today so the refiner would get the gold by tomorrow (Friday).

Anyway, I have briefly read through your posts here and this is my experience:

I have processed gold filled scrap only one time using HCl/CL. It was when I first ordered the DVD from lazersteve. I did it for the experience and I have not done it since. I have plenty of nitric acid and the AR treatment is something I am familiar with. AR=aqua regia

You can use AR to dissolve the gold filled foils. You can also use AR for the black powder from your sulfuric cell. I don't see any reason why you can't use HCl/Cl for either type of these materials also. I don't think it makes a difference.

I am currently in the middle of a gold filled recovery and refinement myself. I started with 260 grams of gold filled watch covers and jewelry.

I started by incinerating the gold filled scrap to redness. Then I added distilled water and then nitric acid (about 850 ml each).

I put it all in a coffee pot with a lid and "cooked it" for several hours.

I then let it sit for a day or so. Once settled and cool, I filtered off the liquid, allowing the "purple mud" the go into the filter at the very end. I took the clear filtered liquid which was dark blue, and neutrailzed it with Urea.

I put the filtered liquid in a large beaker and added a coil of copper wire to cemented the silver from the solution - there was about 1 ounce or so (estimate) of cemented silver in the liquid - it is still cementing as I write this.

I rinsed all the fine material from the coffee pot into the filter, but kept the foils and shells of gold in the coffee pot. There was a pale purple mud about 1/8 inch thick in the filter. I saved the filter, just left it in the buchner funnel.

I then re-treated the gold foils with some more (about 200ml total) dilute (50/50) nitric as some of the base metals had not dissolved completely.

Also, I found a chain I had saved from a previous batch from some months ago. The chain was saved because it still had base metal that was not dissolved. I added this chain to the foils in the coffee pot with the second 50/50 nitric treatment.

More red fumes came from this reaction confirming that base metals were present.

I cooked the batch this time for about 2 hours until no more red fumes were present and the solution was boiling vigorously. the solution was black this time - I think because of the chain, it may have had iron - I don't know.

Oneal58, I am pretty sure there is lead and tin are in my batch of gold filled scrap. I say this because of what I found in the filter paper from the first filtering of the liquid from the coffee pot - a pale purple paste that looks like lite purple silver chloride. I am thinking that this is tin and lead mixed with some colloidal gold and gold powder. The gold can be recovered from this mud according to Harold.

I would guess that there is a good chance that your gold filled batch also has these contaminates. Therefore, it is probably not a good idea to mix your two batches together - although I read where you have already done so.

A while back, Harold had written a post where he recommended that gold filled foils, mud, and everything should be sent to the filter - this is one of the only times that it makes sense to put all the material into the filter.

Once in the filter, Harold stated, that the whole batch should then be incinerated, filter and all - to get the gold mud - then the incinerated material should be treated (boiled) with full strength HCl.

Boiling in full strength HCl will get rid of the tin and lead that are sure to be present from gold filled scrap.

Once the treatment with HCl is complete, wash with water several times, then treat with aqua regia and proceed as usual with filtering and precipitation of the gold.

I hope I have not mis-quoted Harold on this. I have this process printed out and in a notebook at my shop and just happened upon it as I was reviewing.

The foils from the second cook are still sitting in the coffee pot in that black liquid. Tomorrow I plan to pour eveything into the filter as Harold recommended. Foils, gold mud, and anything else from the reaction vessel. Then I will let it dry and incinerate the whole mass - filter and all. Then treat by boiling it in HCl. Once complete I will wash with distilled H2O (Tap is probably OK here) and then dissolve in aqua regia.

I will let you know how this batch turns out. I am curious to know how it will turn out myself as this will be the first time I use Harold's process on this gold filled batch. i am hoping for good results.

I have done gold filled batches in the past were I rinsed out all the purple mud into the filter, then saved the filter. The foils were not allowed to go into the filter. I rinsed the foils in the coffee pot with plenty of hot water, then dissolved the foils only (no mud and no incineration).

The resulting gold bead came out OK, but it was not very pure and had a silvery coating on top, but it tested at least 22k. I think it weighed about 3 or 4 grams. i sold it on Ebay as 22k Gold and got about 80% of spot price for it with a positive feedback from the buyer.

I hope this is helpful to you. Aslo, I hope I did not mis-quote Harold on the process I wrote about above in this post!

kadriver

 

[Oneal58]

Hi Everyone, this is Oneal58.
I am going to try and tell everyone exactly where I am right now. I think I have not conveyed to everyone exactly where I am at, how I got there and where I would like to try to go. I am sorry for this confusion. It is totally my fault.
I will first explain how I got here. As all of you who have been helping me know I worked about 5 days on the sulphuric cell stripping gold plated Jewelry. I ended up with a small amount of black powder from the cell. I diluted the sulphuric down in steps and washed the black powder several times in distilled water.
Where the confusion is coming in at is that I had gold filled jewelry I was working on during the same time. I spent 1600ml of Nitric on 3/4 lb of gold filled jewelry dissolving the base metals from. I decanted/filtered and saved the dark blue greenish solution and put it in a big crock for later processing.
After taking a closer look at the material out of the Nitric Bath that held the (gold filled items) Jewelry, I saw that the material still had some grey metal in and on the gold filled items.
Step1- Here is what I did, I put the black powder from the sulphuric cell in with the partially dissolved gold filled material from the nitric bath into the same beaker.
Step 2- I added 200ml of water and 200ml of Nitric to the gold black powder from the sulphuric cell (plus) the material (foils attached to metal) into the same flask, (all material in 1 flask)
Step 3-I started warming the Nitric to get a reaction started. Once the reaction started I covered the container and let the solution sit on low heat while covered. The solution vented dark brown vapors for 45-1 hr. and then stopped fuming. I continued heating the solution on low heat to make sure that I drove off as much nitric as possible.
Step 4-I stopped right there, took the flask off the heat, covered it and put it up to cool.
This is where I am at right now.
I believe I have all the base metals dissolved and am waiting for the solution to cool.
I know I probably have tin and maybe lead still in solution due to the purple color I got from the wash water when I washed it before I put the 2 together.
I want to go with the AR recovery method, I know it's harder on a beginner but this is the method of choice I hope to use in all my recoveries in the future.
I hope this will let everyone know where I am in the process and where I would like to go with your help.
I apologize to everyone for not being clear where I was at and where I was headed. I must pay better attention trying to inform you of where I am in a process and where I want to go to. I have got to be able to know where I am before I can relate to you for you to be able to help me.
Thank all of you for your help, this would be impossible for me if it wasn't for you. I am sorry for the confusion.
Oneal58
Oneal58