Refining Gold from Gold Filled Jewelry

[butcher]

Oneal,
keep reading Hoke's book, you will never know when the light comes on, sometimes it comes on and we did not even realize when it did, You have really learned alot in a very short time.

 

[Oneal58]

Hi Butcher, thanks for those words of encouragement. They were surely needed at absolutely the perfect time, appreciate it buddy.
When things fall into place, as my first half-dozen refines did you get the big head, as I did. This aspired me to move onto bigger goals before I was ready to make that jump.
This last refine or 2 has put me back in my place and made me realize how little I still know. How much more time I need to spend studying and reading instead of counting my nuggets.
As we say in the South, these last 2 refines have beat me as you would a Red Headed Step Child.
Beaten right now, but not broken. I will get this sorted out!
Thanks Butcher,
Oneal

 

[Oneal58]

Well, I must be losing my mind here? I finally got back out to the old house today and try and get some work done. I had 2 lots of refined gold, one sitting in AR and the other I had tried to cement with Metabisulfite and no drop took place. I have one lot sitting in Metabisulfite and the other solution in AR. I had tested both these lots last week just to see how strong a reaction I got. I even loaded a picture of the postive test on both the Platinum and Gold mix in an earlier post. This was my largest refines so far. I expected at least half an ounce out of these last 2 lots.
I go back out today and test with stannous again, no results/negative. I made up some new Stannous and tested again, same results, negative? I made up another batch of Stannous while scratching my head and tested the lots again. Both test negative now for gold or either platinum.
What in the world could this be? What could be causing this? I don't remember reading in Hoke's anything about results such as this. I know for a fact I had gold in these lots and now I get negative test results on both lots? I am going to try and drop the last lot with Ferrous Sulfate, the one that has the redish color tonight. Even though the solution is testing negative for PM's. I know I had PM's in the lots only 4-5 days ago.
I am at a lose here. Has anyone ever heard of such a thing happening with their refines. I know that the gold is in these solutions but my test tell me it's not there anymore.
Does anyone know what could have happened to the PM's in these lots. I know that there still in solution. I just get a negative result when I test for PM's.
Any help would be appreciated.
Oneal58

 

[butcher]

Oneal,

Lets just stand back and look at this, sometimes when we get up too close we cannot see something right in our face.

Some of the chemical reactions take time, many times we may mix A chemical and B chemical and think we should get a reaction in a few minutes, when actually it can sometimes take time for these reactions to complete (depending on condition) minutes, hours, days, weeks, or more, also sometimes we may not have enough of chemical B or too much of chemical B, this can also change conditions of our reactions,
I have neutralized, chloride metal salts and got fairly close to neutral, expecting to see a clear salt water, only to see a colored solution that would not settle for day's, then I would add just a few drops of HCl, and watch what sit for days, precipitate in just a few minutes.


Do we have gold in solution, our stannous test say's none we can detect, are there powders maybe gold precipitated? Maybe we still have nitric in solution (or oxidizer)? Maybe there is gold and our stannous is not working?

Lets start to try some things.

Take a tiny piece of gold we do not need much at all (memory finger, filings off old gold ring, or chain, could be used), put this in small jar or test tube and dissolve some gold into solution, I would use HCl and bleach, (but aqua regia would also work), we will need heat to evaporate the oxidizer bleach or (nitric) whichever we used (bleach is just easier).

Now we have some gold in solution we can check our stannous with, while we are at it we can use a white spoon or spot plate and add a few drops of this solution to a crystal of ferrous sulfate to see if we get a brown ring in the spoon around the crystal, if these show up the gold, we have proved our test solutions will work.

We can repeat these test with the solutions you are scratching your head over, now is our stannous working? Maybe it works on the test solution from the test tube above, but not the solutions in the little house (your lab) we suspect have gold, but we still think these solutions may have gold in solutions, and we know our stannous chloride is good, lets take a small sample of the solutions we think have gold and put these in a test tube's one tube for each one of our solution's we wish to test, now lets heat these just incase we still have an oxidizer like nitric acid that may be re-dissolving our gold when we try and test them, (here is also where I may use a prill of urea, I know I always say urea is not needed, but that does not mean it can not be useful in a few places), now that we have de-noxed we can try and retest these solutions, lets try both stannous and ferrous sulfate.

If we find gold in solution we can take the liquid from the white spoon that ferrous sulfate crystal precipitated the brown gold out around the crystal, dip a Q-tip into the liquid and test it with our stannous to see if we may have Pt or another reaction to stannous chloride.

If our gold was there It is still there, we just need to find it, if these tests do not show us where it is, we may just have to stand back and look at this again.

It is good to see you feeling good enough to get out some, try and not to over do it, do not stress about the gold, these little gold Ion’s are just sneaky, sometimes they just want to play hide and seek with us, we just have to get the right tools to find them.

 

[Oneal58]

Hi Butcher, thank you for your post. I will do just what you suggested, spot plate and also test tube test. I am headed back over now to start on it. When I have results I will let you know what they were. More than likely be tomorrow, it will be too late when I finish up tonight to post results.
I have thought this through many times, step by step, and just can't figure what happened. In my earlier post, the lot that I posted the picture of earlier that showed red mixed in with purple. I added the Ferrous Sulphate, about 2 grams of (fresh) Ferrous Sulphate to drop the gold and leave the Platinum which I strongly believe is mixed in with it. Again, nothing happened, negative drop, negative test with stannous. Take a look at the picture I loaded a few post back. This is the very same solution, same corningware dish, I changed nothing other than wait another 3-4 days.
The first gold drop attempt on the lot I put the metabisulfite in, I tested it after I attempted to drop the gold. The results on the solution back about 4 days ago was so purple it was almost black. But now I get a negative when I test?
I haven't been back but just a few minutes. I went to Ace Hardware and bought fresh HCL and fresh Rooto Sulphuric. I had used a few drops of another sulphuric, (different brand) on these last 2 lots but that was the only change I made. The sulphuric is professional brand (pure sulphuric) but it is a dark color, not like the Rooto brand I have been using which is clear in color. But that is the only change I can think of verses the previous 7 refines.
But, it's just like you said, do the test, back off and see what the results are and what needs to be done to correct it, then proceed.
One thing I do remember that was different than the others was when solution was being filtered. I had a build up of white powder in the filter paper that I hadn't seen before. I will load a picture of this later. I assumed the very white powder was lead. It came after I added a few drops of the dark sulphuric? It floated to the top of the solution and when poured off to filter turned white in the filter paper. It was not sticky or gel like, more like a paste or regular paint.
Wait a second, I will run out there now and get a picture of the white powder before I start the test. I will post it now.
The paste was very white like paint, when I folded the filter paper I believe the tin, copper, Etc;. dust covered it. But it was very white, just like dried white paint. But it was the very first time I have seen it before in any of my refines. Picture is below.
Thanks Butcher,
Oneal

 

[ryan6342]

hi everyone this may not exactly be on topic, first time posting here. if you burn your leftover filters and notice green flames, is that the gold leaving to go play with the atmosphere? or is my gold all still in the bottom of this ash pile?

 

[Geo]

green flames are normally copper.

 

[ryan6342]

green flames are normally copper.

thanks whew.
so would the gold burn away as a color?

 

[butcher]

copper will give green flames to a fire.

Many metals will color flames, this is one way metals can be identified, with flame tests seeing colors in the fire.

Gold if it is a chloride salt can burn into the chlorine gases formed (I never noticed a color to the fire or smoke but have noticed yellow on surfaces that cooled, and when tin involved noticed it condensed to a violet purple color.

Silver chloride salts are also volatile, and your silver will burn up in the white smoke.

Gold is hard to oxidize, so if it is a metal it will not go up into smoke as far as I know, silver also does not oxidize easily (it will actually absorb quite a bit of oxygen into the melt and can spit it out on cooling.

many base metals can put off vapors of metals in the gases, almost all in our lungs are not good for us, some are especially dangerous, or deadly never breath any fumes of these metals, especially from electronic scrap, not only the metals but there are many toxic chemicals in circuit boards and things like heat sink greases, and materials the components are made from, also many metals we do not normally discuss.

Ore can also be a very dangerous material to incinerate or roast; these rocks contain some dangerous acidic fumes or other toxins like arsenic.

 

[Oneal58]

Hello Butcher and Everyone, just back on line. Been in hospital for a while, severe (diverticulitis infection). I thought I was a gonner for sure?
I did get my testing done on my solutions though as Butcher advised. Found that my solutions were barron. Just a little gold in one of them but just a dusting.
Anyway I had a lot of material left in my reactin vessel that just would not dissolve. By reading here on the site and Hoke's I finally figured out that my gold was still in the reaction vessel locked up with a heavy coating of silver chloride. I really did try and kill 2 birds with one stone and put a silver alloy in with this lot. So there was a lot of silver in this refine. I guess that's why this was my first experience with this problem.
Anyway, I boiled the material in ammonia hydroxide for a while and low and behold there it was. All my work was revealed to me! This sure has been a learning experience for me and I have learned a ton from this.
I want to thank all of you for your help.
Has anyone ever experienced this? Am I right to think that too much silver in the refine caused this? Or did it have to do with the prolonged boilings with nitric that played a part in this? Or did the homemade Nitric play a part as well?
I did my very best to dissolve this material and I am hard headed but I couldn't get it to dissolve. So, I don't know why this happened for sure and would love to know if anyone has the answer?
One more question, I contacted a Refinner today that said if my gold was .999 he would pay me 99% of spot. He also said if the gold was in Karat form he would pay me 98% of spot? This refining is sure a lot of work for 1% profit to refine it. Is this the going price or is this just because he doesn't know me. I even offered to shot it but he said that wouldn't help the price even if it was .999 pure. He would just put all the shot back together and refine it again to assay it?
But, I have to remember, most of what I have has came from gold filled, gold plated, rolled gold Etc;. Just wanting to check in with everyone to see if this is the going rate for .999 pure gold?
Thank everyone for their guidance in advance.
Oneal58

 

[nickvc]

I'll leave a full answer to Butcher who has been advising you all the way on your material and may I say doing an excellent job, only a fool would ignore his comments in my opinion.
The reason your material didn't dissolve is I fear down to your unexpected illness when you couldn't get back to work quickly or remember what was what. The silver had not digested fully in the nitric so when you put it into AR you got the hard silver chloride covering which prevented the acids working on your gold, go back to the nitric dissolution now you have removed the chloride and finish off that part and you should be good to go.
Terms for gold scrap or refined scrap are pretty good these days so the offers you had do not surprise me but remember much karat scrap isn't plum so an offer of 98% is one I'd take if he will accept the marks as 10 , 14 or 18 karat although I expect the payout will be based on a melt and assay, this is where some doubt can start to creep in as to actual returns...
With your gold filled again I'm sure the only way he will buy is on melt and assay again a grey area and in this case a big one, not all refiners or buyers cheat but many will and do, so unless you melt the material yourself and have an assay done how do you know what exactly your trading...

 

[Oneal58]

Thanks nickvc,
I completely understand. Years ago I was selling to a refiner. I would test each one of my pieces of karat gold and knew what I had. When the check came it would not be what I had figured it should be? This happened time after time after time. I am not accusing, I know their are honest refiners out there who wouldn't be able to sleep at night if they did anyone wrong. But I can also see the reasoning why a refiner would prefer the karat gold in raw form and refining it himself. Look at the countless thousands of people who send in their gold in not having a clue as to what they have to begin with. It would take a refiner who was saved, sanctified and filled with the Holy Ghost not to be tempted to stump their toe every now and then. And then it would tempt the best of us not to watch the filtering real close, Etc.
So, I am like you, I would rather refine it, knowing what it weighs exactly, and also what karat I am near. I can say then, hey, I know better. I have told the refiner not to melt my gold, just to drill them if he has to assay the gold.
It just doesn't make sense to pay $1 more spot price for refined pure gold than raw karat gold. Look at the time and expenses, labor, acids, utilities, and all the other overhead, The list goes on and on that's involved to refine the karat gold. So, you have to ask the question, WHY? I am open here for someone to give me their opinions on this. Maybe it will help me understand better, why this is?
Thanks nickvc for your post.
Oneal58

 

[Oneal58]

Butcher, where are you at Buddy, my friend. I need and would appreciate a little help if you have time.
I came across about 86 grams of karat gold, some 10K some 14K. For some reason I wanted to try a different method of refining than the nitric, inquartration method. I guess because of all the trouble I had on the last refine.
I used (AR) from the start with my homemade nitric and HCL on the karat gold. I figured the amount of nitric and HCL to use and put the lots on low heat. The karat gold dissolved completely in about 1.5 hours with constant agitation. The 14K dissolving before the 10K did, that surprised me? The solutions came off the burner jet black, I diluted with distilled water and the solutions turned a dark green color. I tested the ph and both lots came in around 2 on my litmus paper. From what I have read I think I need to take this down to less than 1ph? These refines ended up being a large amount of solution. I iced the solutions down good, covered and left overnight. White powder has settled on the bottom of containers. This suppose to be mostly silver if I have read correctly. I know you are not a supporter of UREA to neutralize a solution. So would you drive off the excess nitric from solutions by heating and condensing the solutions down? Then using your method of evaporations, adding several HCL additions, few drops of Sulfuric additions. Also, to drop the gold, the solutions are a deep green color, tells me that it contains copper for sure. Would you use ferrous sulfate or sodium metabisulfite to do my drop since I processed with (AR) this time?
Butcher, this process has went far too easy and quickly. Would you tell me why this approach isn't used more on karat gold than the nitric/inquartration method? Up until this point and this refine I thought (AR) suppose to have a hard time dissolving karat gold? I am confused now and am waiting on the other shoe to drop on this refine also. On the 14K material, rings, necklaces, pendants, etc:, was dissolved in less than an hour, took longer on the 10K? I thought it would be the other way around? I have read that I could use a little UREA to lower the ph and drop the gold through the green solutions with ferrous sulfate without dragging the copper, lead, etc; down with it? Then that would be the end of it after the use of Harold's making gold pure process. Why not sodium metabisulfite, would that drag down other metals as well in the green solutions? That sounds far too easy and I know there is a reason why not to do this?
I know I am missing something here, but I just can't put my finger on it? Why isn't this supposeably easier quicker method used to process karat gold, I know there are good reasons. I kind of hate to hear them but I need to understand, why? I know you don't use this method for good reasons, that's what has me concerned, what you are going to tell me?
Can you give me a hand old friend?
Oneal

 

[jimdoc]

Why isn't this supposeably easier quicker method used to process karat gold, I know there are good reasons. I kind of hate to hear them but I need to understand, why?
Oneal

Because getting rid of the base metals should be your first step. Now you have everything in your solution to contend with.

Jim

 

[Oneal58]

Hi Jim, thanks for your post.
I am under the impression that by using ferrous sulphate I can drop the gold through the green solution witout dragging down too much of these other metals? Then by using Harold's making gold pure process get rid of the metals I did drag down? Is this right or wrong?
Thanks, Oneal

Why isn't this supposeably easier quicker method used to process karat gold, I know there are good reasons. I kind of hate to hear them but I need to understand, why?
Oneal

Because getting rid of the base metals should be your first step. Now you have everything in your solution to contend with.

Jim

 

[jimdoc]

Why isn't this supposeably easier quicker method used to process karat gold, I know there are good reasons. I kind of hate to hear them but I need to understand, why?
Oneal

Because getting rid of the base metals should be your first step. Now you have everything in your solution to contend with.

Jim

I failed to mention the problems that silver will cause with your new method.

Jim

 

[goldsilverpro]

Butcher, where are you at Buddy, my friend. I need and would appreciate a little help if you have time.
I came across about 86 grams of karat gold, some 10K some 14K. For some reason I wanted to try a different method of refining than the nitric, inquartration method. I guess because of all the trouble I had on the last refine.
I used (AR) from the start with my homemade nitric and HCL on the karat gold. I figured the amount of nitric and HCL to use and put the lots on low heat. The karat gold dissolved completely in about 1.5 hours with constant agitation. The 14K dissolving before the 10K did, that surprised me? The solutions came off the burner jet black, I diluted with distilled water and the solutions turned a dark green color. I tested the ph and both lots came in around 2 on my litmus paper. From what I have read I think I need to take this down to less than 1ph? These refines ended up being a large amount of solution. I iced the solutions down good, covered and left overnight. White powder has settled on the bottom of containers. This suppose to be mostly silver if I have read correctly. I know you are not a supporter of UREA to neutralize a solution. So would you drive off the excess nitric from solutions by heating and condensing the solutions down? Then using your method of evaporations, adding several HCL additions, few drops of Sulfuric additions. Also, to drop the gold, the solutions are a deep green color, tells me that it contains copper for sure. Would you use ferrous sulfate or sodium metabisulfite to do my drop since I processed with (AR) this time?
Butcher, this process has went far too easy and quickly. Would you tell me why this approach isn't used more on karat gold than the nitric/inquartration method? Up until this point and this refine I thought (AR) suppose to have a hard time dissolving karat gold? I am confused now and am waiting on the other shoe to drop on this refine also. On the 14K material, rings, necklaces, pendants, etc:, was dissolved in less than an hour, took longer on the 10K? I thought it would be the other way around? I have read that I could use a little UREA to lower the ph and drop the gold through the green solutions with ferrous sulfate without dragging the copper, lead, etc; down with it? Then that would be the end of it after the use of Harold's making gold pure process. Why not sodium metabisulfite, would that drag down other metals as well in the green solutions? That sounds far too easy and I know there is a reason why not to do this?
I know I am missing something here, but I just can't put my finger on it? Why isn't this supposeably easier quicker method used to process karat gold, I know there are good reasons. I kind of hate to hear them but I need to understand, why? I know you don't use this method for good reasons, that's what has me concerned, what you are going to tell me?
Can you give me a hand old friend?
Oneal

Most of my life I haven't inquarted unless absolutely necessary. Instead, I dissolved the jewelry directly in aqua regia. Even with keeping it near boiling, it took at least 3 to 4 hours and often longer. From several things you said, it sounds like you didn't have karat gold to start with. It just doesn't go nearly that easily or that fast. One reason people inquart is that direct dissolving. Are you seeing a strong yellow color within the green color? Use a stir rod and drag some solution up along the glass above the solution. If this doesn't appear yellow, you have a problem.

 

[Oneal58]

Hi goldsilverpro, thank you for your post.
You are the reason I tried this refine with (AR). I follow your post and spend time on your site and see you use this method.
Goldsilverpro I tested each and every piece of this karat gold. Unless my chemicals are giving me a false reading each and every piece was either 10K or 14K? I have been testing gold for many years the same way so I am pretty sure that it was karat gold I dissolved.
I may have mislead you on the condition of the gold before it went into the (AR). I cut each and every piece up into tiny pieces with my lineman's pliers. I also took my anvil and flattened each and every piece of it, so it was very thin. I then cut into even smaller pieces and made bends in the pieces that were big enough so they would not lie flat on the bottom of the vessel. The (AR) tore into these pieces with a vengeance.
With me standing beside the two heating elements agitating vessels constantly. I guess that's why it only took around 1.5 hours to dissolve the gold.
I do have the yellow color in the solution, it's just masked by the green color. When the solutions came off the burners it was black, it turned green only when I added distilled water to dilute and cool it.
Goldsilverpro, I have a couple of thousand $ in these refines so I am nervous and want to be cautious. I am just at the point that I am not sure as whether to use ferrous sulfate or sodium metabisulfite or some other method to drop the gold.
I see you offer a book on refining. Does your book have this process in it? Since you have been using this process for years any guidance would be appreciated from you here. It seems you are one of a very few that does this process.
In the meantime if this process is in your book I could purchase it as well.
I need to finish these refines up the right way. It's just that I don't know what the right way is right now. I have looked for a couple of days on the web and can't find the last steps. I have trouble watching videos with my computer for some reason I haven't figured out yet.
Would you give me the link to the book that has this process in it, it would very much appreciated.
Thank you for your post and any guidance you could give me from here.
Thank you, Oneal


Most of my life I haven't inquarted unless absolutely necessary. Instead, I dissolved the jewelry directly in aqua regia. Even with keeping it near boiling, it took at least 3 to 4 hours and often longer. From several things you said, it sounds like you didn't have karat gold to start with. It just doesn't go nearly that easily or that fast. One reason people inquart is that direct dissolving. Are you seeing a strong yellow color within the green color? Use a stir rod and drag some solution up along the glass above the solution. If this doesn't appear yellow, you have a problem.[/quote]

 

[goldsilverpro]

Oneal,

My book does cover that process.

If you haven't thrown anything away, you still have all the gold and there is always a way to get it - Always! I'll help but I have to first absorb your posts. You write very well but, in the future, please break stuff into more paragraphs with spaces between them. To me, this is very important when you have a lot of details. On one long paragraph and no spaces, my eyes glaze over after about 8 lines. Need some white area.

The way you prepared that stuff, I will agree that 1.5 hours is very possible.

 

[Oneal58]

Thanks Goldsilverpro, will do. I just get in a hurry sometimes and take my mind off what little communication skills I do have.

Thank You in advance for any guidance.
Oneal

Oneal,

I'll help you but I have to first absorb your posts. You write well but, in the future, please break stuff into more paragraphs with spaces between them. To me, this is very important when you have a lot of details. On one long paragraph, my eyes glaze over after about 8 lines.