first attempt at scrap jewelry

[artart47]

Hi friends!
I've been here learning for a couple years and would like to thank my friends that tought my,coached me when I ran into problems or uncertanty and reminded me about 'SAFETY'! You shared your knowlage of this exciting field that I knew nothing about. Refining has brought me so much pleasure! I hope I can help other nubes experience what I have.
Up untill now I've been doing everything with AP for recovering gold and HCl/clorox for refining the gold I recovered. After the last year reading your posts and watching the videos I feel I've gained the understanding of the chemistry and how the materials I'm working with should be attacted. So! I set up and processed my first small batch of 14K and 10K gold jewelry! Inqurting with a silver half dollar, disolved in 50/50 nitric/distilled water digested the gold sponge in HCl/cloroxe and dropped with SMB. Think I did well for a nube getting his feet wet! For any new members, don't attempt to process a material untill you can understand what will be going on inside the reaction vessel and why you're doing it and how to do it safely You see how many posts start with "I need help with the mess I've created...." You want to hold your precious metal in your hand when done and not have you effort end in failure or injury!
My first scrap gold purchase was from a guy who needed money really bad and came to Denney's and asked me if I was the gold guy. He said he wanted $100 for his gold and I bought a small plastic bag full. !0K, 14K, one 18K piece some .925 silver belt buckels,rings and a few silver coins. I don't have my notes with me here but I inquarted the 10&14K stuff and I recall that if I melted the stuff along with one of the silver half dollars, it was supposed to give me a mix of 25% gold/75% silver or whatever other metals were in the alloy.
For nubes; Inquarting with silver.
In order to recover the gold from jewelry alloys you use nitric acid mixed half and half with distilled water to disolve all the metals that aren't gold, thus leaving the gold as a solid that can be filtered out and refined to purity. This process will not work if the gold content is over 25% that is why you must calculate how much gold and how much other metal in the material and then figure out how much silver you need to add to bring the gold down to25% or 6K
I got my nitric recently. I set up outside with a hotplate and a waterbath to place the beaker into so I could bring the reaction beaker to a simmer.
My nitric acid is 67% so I would be mixing it with distilled water 50%/50%. First I pourd the water into the beaker to cover the inquarted gold then, I put the hotplate to medium and brought it to a simmer. Then I added the nitric acid,a couple mililiters every once-in-a-while as the reaction stopped I'd add alittle more with an eyedropper. when I added another mililiter and saw no further reaction I left the beaker covered and on the heat for a couple hours.
For nubes; disolving the non-gold metals,mostly silver or copper with acid.
you will end up with the solid gold in the the beaker and the silver, copper or other base metals disolved in the solution
YOU NEVER DO THIS WORK WITH ACIDS INDOORS WITHOUT A PROPER VENT HOOD SET-UP
NITRIC ACID FUMES WILL KILL YOU AND IT WILL SEVERLY DAMAGE ANYTHING METAL IN THE WORK AREA

After it cooled, I ran the solution thru the same coffee filters four times and rinsed the gold into the same filters.
I disolved the gold withHCl/clorox added ice to double the volume of the solution. after the ice melted, I filtered it again and got alittle more silver and that's where I' at now>

For nubes;
In this post, I'm sharing my first attemot at refining gold jewelry, (something I haven't tried before.)
I explained the reason for each step and what you want to accomplish so that new members can get a basic idea of how it works.
It is not intended to be instructions for how you should try to refine jewelry! There is alot more you need to learn before you ever try this

I;ll add more and let's see how the gold drop turns out, gotta wash it and see what I have

 

[butcher]

Art,
Oh what pretty colors you have there.
I am patiently waiting for the rest of the story.

 

[kkmonte]

OMG Cliffhanger! What are you planning on precipitating the gold with? I'm guessing SMB?

 

[artart47]

Hi!
I'm back! Made some progress yesterday.
Fro nubes;
What was gold jewelry, has been reduced to two solutions and a filter paper. I also have the stones that were in the pieces in a jar for later.
The blue liquid is the nitric solution which contains the silver and the copper that was alloyed with the gold. I can recover the silver later .
The amber liquid is the solution that I dissolved the recovered gold sponge in
The filter paper has a little silver that dropped out of the gold chloride solution (amber) after I added ice to chill it

I Dropped the gold with SMB and let it settle all night. after the gold drops,I always decant the solution into a mason jar so I can test it with stannous chloride (have to make some fresh tonight). Sometimes I get a dusting of gold that drops later. the other picture is the powder after an HCl boil and another water rinse
I believe this may need a second refining to get the lite-tan powder that we all love!

 

[butcher]

Art,
The powder looks good, a second refining it will even look better, with a good wash in Harold's washing procedure (found in the topic getting your gold pure and shining), you will have a very nice lump of gold there.

I cant wait for the next episode of this story,

 

[artart47]

Hi all!
Thanks for the comments and the interest! This is so cool!
Just an update. I washed the powder well with boil in hydrochloric and then distilled water, I ran it again in HCl/Cl, dropped with smb, and I'm doing the "Harold wash" Ill be putting it in the NH4OH boil as soon as I get home.
I'll post some pictures when I get done.
I'd like to ask you opinions. Whenever I go to dry the gold powder, I just give a squirt or two of distilled water into the beaker as drop the powder right into the melting dish. then, I force-dry it by just putting gentle heat onto the outside of the dish and on the powder and dry it right in the dish. never had a problem. do you think this is ok? How do you tranfer it ? I can never seam to get all the powder out of the beaker. Thanks for any info!

for nubes;
In the previous post The gold chloride solution (amber) was treated with sodium metabisulphite(smb). This compound, when mixed with water, makes sulphur dioxide gas in the solution. That causes the gold chlorid to turn back to metalic gold. The gold drops to the bottom but most of any contamenents remain in the solution.
I poured off the solution and washed the gold powder with boiling water then hydrchloric acid .
These washes, continue to clean-up the gold powder.
Now starting with much cleaner gold, I did the refining step again. This time the solution will be much cleaner so the gold I drop the second time will be very pure.
Important! In order to have success at this and to do it safely, you have to learn each of these step and understand them, know the chemicals you're working with, what to do when something goes wrong and how to deal with the wastes that you will produce. and much more!
Hoke's book is the source that will teach you the understanding of refining. You need to be studying our safty section and learning from reading the members' posts before you ever think about pouring chemicals. In the meantime, just keep colecting stuff to refine till you are prepared!
People here will give you help if you have problems. we love to see pictures of your gold buttons but you have a lot of work to do!


I have something beautiful that happened by accident, picture, I just wan't to see if any other members had this happen.
This has to do with this thread and me getting aquainted with nitric acid. (kindda "test drive" of AR)
I want to see the responces and then I'll tell you what I did! I had no idea this would happen!

 

[butcher]

Pictures are a bit fuzzy but that looks like a nice hunk of gold, good job.

I do not put wet gold in my melting dish, as I do not want to crack the dish.

You may get by with it if you dried the dish with heat to drive off all moisture before raising heat on the dish, but to do this the dish would have to have already been pre-seasoned (dried, all moisture driven off with mild heat, then the heat on the dish up to red sprinkle a light glazed coating of borax coating while the dish was red hot), to re-wet the dish after going to the trouble of preparing my dish for a melt, and taking a chance of cracking the dish would not be my choice.

If I only have a tiny bit of gold powder I normally save it up until I have enough for a second refining, where the batch is a little bigger, it is my belief that it it is better to save it up, than try and mess with real small amounts, the (temporary) lose through the process is not as bad when processing bigger batches,

If the gold is pure and your glass ware is clean, and while the gold is almost dry, but still drying you bang the gold into balls, banging the beaker against the heel or palm of your free hand, then rolling the balls around in the beaker while they are finishing drying, they tend to collect most all of the gold from your beaker walls, the gold balls are dried they can then be added to the melting dish, if a tiny bit of gold powder is left behind in the beaker, which really should not be much, use a wash bottle to wash the gold powder to one corner of the tilted beaker, pipette out most of the rinse water, the gold can then be picked up in the pipette transferred to your small collection bottle or a small piece of toilet paper, then with a glass rod you can wipe down beaker with a small piece of toilet dampened by moisture left in the beaker. I have wiped up the small traces from a beaker with toilet paper from the beaker and dried the paper, you can either burn it and melt it or just added it to the other filter papers to get it later.

 

[artart47]

Hi!
I got rid of the fuzzy pictues the guy took with his cell phone and had my daughter take a better one. When my nitric acid first arrived I wanted to try it out before I did the jewelry. Just so I could see how it workes and If I could tell when the nitric was expended and the reaction stopps.
So I put alitle HCl in a beaker, addedabout 2ml. nitric and placed one of my gold buttons in it so I could observe AR.
when I took the button out I coulden't believe what had happened! It looks like the gold has a crystal struture and that the AR had dissolved the gold down to the faces of the crystal planes and then stopped. it dissolved one gram off the 29gram button. I think the pattern is beautiful.
Butcher, have you or anyone else had this happen? are all the buttons structured like this internally? Is it caused by the shock of dropping it into cold water when melting?

Back to the main thread here;
I finished washing the powder, It lightened up alot. I'll have some pics soon!
later artart47

 

[butcher]

Art I believe it has to do with the purity of your gold.

 

[mikeinkaty]

Hi!
I got rid of the fuzzy pictues the guy took with his cell phone and had my daughter take a better one. When my nitric acid first arrived I wanted to try it out before I did the jewelry. Just so I could see how it workes and If I could tell when the nitric was expended and the reaction stopps.
So I put alitle HCl in a beaker, addedabout 2ml. nitric and placed one of my gold buttons in it so I could observe AR.
when I took the button out I coulden't believe what had happened! It looks like the gold has a crystal struture and that the AR had dissolved the gold down to the faces of the crystal planes and then stopped. it dissolved one gram off the 29gram button. I think the pattern is beautiful.
Butcher, have you or anyone else had this happen? are all the buttons structured like this internally? Is it caused by the shock of dropping it into cold water when melting?

Back to the main thread here;
I finished washing the powder, It lightened up alot. I'll have some pics soon!
later artart47

That crystalline pattern is exposed when doing electrolysis on high purity silver. It can be easily buffed out. It also appears on 999+ silver bars when hand poured. To regain that appearance just put it back in electrolysis. At the molecular level when being poured the atoms would be free to align in parallel planes if there was no contamination to disrupt the layering and if it solidifies slowly. During electrolysis it must be stripping or peeling the atoms off along the crystal planes as that probably would be the path of least resistance.

Members here say that the crystalline pattern will command a higher sale value. But, if worn as jewelry, I don't think it would last long.

Mike

 

[midaselm]

great post , im going to attempt my first refining soon too , and seeing how another noobie tries it is great . the crystalline effect looks awesome too . good work

 

[Westerngs]

Basically what artart47 did was etch the surface of the gold to reveal the crystal structure underneath. It is a well known process used to reveal the crystal structure of metals. In this case, the crystal structure does not necessarily reveal the purity of the metal, but rather the rate of cooling when cast.

The crystal structure can be changed by annealing and working the metal to either increase or reduce the size of the crystal.

It is especially useful to know the crystal structure of things such as vapor deposition targets and pellets as it will affect the deposition layer.

LECO corporation publishes (or used to publish) a guide to chemical etchants for different metals and alloys.

 

[artart47]

Hey friends!
Thanks for the answers. I had no idea that a button had a structure like that inside. I learn something new.
artart47

 

[artart47]

hi everyone!
This AR thing is a little different that working with HCl/chlorox. I guess what some of you have said about skill comming in to play.
The gpld powder is from the 10 & 14 K jewelry I began this thread with. I have run the powder twice.
first time the drop with SMB resulted in a very dark brown powder but the color was uniform.
I washed It with boiling water then a HCl boil, a second water boil the house hold ammonia and two more with water. The washes seamed to lighten it, but not the tan you want.
I redisolved it in AR and diluted with4x ice and water. It sat over night. It was amber and very clear with no settled solids. I dropped it today with SMB.
It dropped rapidly, but as the line between the clear, colorless liquid at the top and the gold powder below worked its way down the beaker there was the top inch a band of very dark material that followed the gold down.
The gold powder is the beautiful tan color but there is a layer of the dirty blackish material over it.
I want to eventually master AR But this is a different ball of wax. Ha Ha!
Some things I been thinking....
I had a hard time being able to tell if the material was still reacting as I add nitric or if it was bubbling from heat from the hot plate, I don't believe I used too much nitric.
per-haps i messed up when I was teating the inquarted gold with nitric and failed to get sufficient base metals removed and the're comming back to haunt me now, or could there have been some platinum family in the jewelry and now it comes out with the gold? I don't know!

 

[artart47]

Forgot to mension!
Some of that powder is from an already refined piece i put in to make sure any excess nitric would be used up. It consumed about a gram. ( It was the one with the crystal structure. very pure!)

 

[artart47]

Hi everyone!
I'm back! Well, I been thinking about the problem of the dark film on top of the gold powder. It's been through two refinings and came down with the gold on the second SMB powder drop. it survived the water washes, the boil in HCl, Thought may-be it was some PGM's but hot ammonium hyrdoxide had no effect on it.... so after doing some searching I figure it could be silver that had made it through the AR. That night, I heated the powder in 67% nitric acid just to the point of steaming and after a half hour, bingo! Washed it with boiling distilled water and melted it today!

For noobs;
If your gold has previously been in any chlorine solution, you must be sure all chlorine has been washed out befor putting it in nitric. if any chlorine is still there, you will be creating AR and will put some gold back into solution. even the chlorine in tap water can cause some gold lose. Harold and other members advise incinerating before going to nitric. I also tested the rinses with stannis chloride for gold and they tested negative. Read and understand the safety section before using there acids.

Well, Here are the final pictures!

 

[MEANIE]

AWESOME..and realy shiney , can see your green shirt in the pic ..lol well to me thats what it looks like to me

good job ,,

meanie

 

[artart47]

Thanks Meany!
The green is the reflection of my daughter's cell phone
artart47

 

[butcher]

Nice, it also looks better and is worth a heck of a lot more than that 100 dollar bill.

 

[RoboSteveo]

Great looking button you got there. Good job.