# First attempt at refining - 101 grams



## mlgdave (Feb 13, 2011)

38 grams of 14k, 63 grams of 10k. My first mistake was to think I would unmount the diamonds in the melt (some small melee), they did in fact unmount but now they are stuck in the borax glaze in my melting dish, I guess ill bust the dishes later and use HF unless someone has a trick for me?

Anyways I will post a few replies as I go through the process to the final button which should be about 47 grams.

The 2 blobs of gold were the karat scrap that had stones in them, I premelted them before I inquarted them







Wish me luck!

mlgdave


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## butcher (Feb 13, 2011)

That pure carbon (diamond) will not dissolve in Aqua regia.
why use 999, silver for inquarting, try sterling scrap.
stir melt well with carbon rod and shot before parting in nitric.


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## mlgdave (Feb 13, 2011)

thanks Butcher, I already have the shot in acid and it likes digested, im letting it settle now overnight. I used 999 because I got it for 6 bucks less than spot and it was readily available. 

appreciate the input ads i am just starting out and bound to make a few blunders

mlgdave


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## philddreamer (Feb 13, 2011)

Hi mlgdave!

In case you haven't read it yet, don't crumble the gold "sponges" left over after dissolving the base metals. Otherwise, you'll have to deal with the gold dust when filtering & it's going to be a pain...

Phil


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## mlgdave (Feb 13, 2011)

thanks Phil, didnt know that, I wont crumble them!

I will be filtering tomorrow!

mlgdave


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## mlgdave (Feb 13, 2011)

By the way that big 10k class ring took a crapload of heat to melt, it was white gold so I guess it musta had PGMs in it? 

mlgdave


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## jimdoc (Feb 13, 2011)

mlgdave said:


> By the way that big 10k class ring took a crapload of heat to melt, it was white gold so I guess it musta had PGMs in it?
> 
> mlgdave



Or maybe nickel.

Jim


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## mlgdave (Feb 13, 2011)

ahh yea, will that affect anything or will it just be in solution? Which solution if so? The nitric or the AR?

mlgdave


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## samuel-a (Feb 14, 2011)

mlgdave said:


> ahh yea, will that affect anything or will it just be in solution? Which solution if so? The nitric or the AR?
> 
> mlgdave



Palladium if present will dissolve in the nitric leach.
Platinum if present and considering alloying is consistent will also partially or completely dissolve in the nitric leach. Whatever left will go up in the AR.
Rhodium if present will be left as black/silver powder with the gold.

Dave, have you made your self some stannous chloride test solution? 
To check the nitric leach for pgm's presence:
- you will need to take a sample, few ml. 
- Precipitate the silver with HCL, add until no more white precipitate (AgCl) forms upon HCL addition.
- swab the remaining liquid and test with stannous and see results.
- if test results are un-conclusive, put in the sample a piece of copper pipe for few hours and look for any black powder deposits.

*Test before*, so you will not be chasing a fairytale.



philddreamer said:


> Hi mlgdave!
> 
> In case you haven't read it yet, don't crumble the gold "sponges" left over after dissolving the base metals. Otherwise, you'll have to deal with the gold dust when filtering & it's going to be a pain...
> 
> Phil



That is quite cool to look at, but experience thought me that by doing so, there's a good chance that the nitric will not get a full reach to the alloy, even with boiling.
Same goes to the d. water washes later, by leaving the gold sponges complete it's not likely one will wash all of the silver/copper nitrate solution and will find it (the silver) as contaminate later on at the AR leach.
It's only a matter of patience, few minutes between each wash.


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## mlgdave (Feb 14, 2011)

ok, so having some issues.
I started with 38.5 grams 14k, 63.15 grams 10k and added 93.3 grams of pure silver, melted twice, poured shot and put into a coffee pot with 368ml distilled water and slowly added 368 ml 70% nitric. Boiled for 1 hour and let sit for a few hours. When I went back there were some "copper" colored cornflakes left, and instead of asking on here I thought "ok all that 10k must have left some copper undigested" so I added 50ml more nitric and boiled (and the brown fumes were copius) I let sit overnight and this morning my coffee pot is full to the level of the liquid with white thick crystals and still some undigested shot. The liquid is a nice amber green and thick. 

Next step?

Thanks tons for any input

mlgdave


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## mlgdave (Feb 14, 2011)

Looking closer it looks like all of the stuff did digest. I have a small amount of distilled water to dissolve the crystals. I will check with stannous chloride filter and do the a r.

Mlgdave


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## philddreamer (Feb 14, 2011)

Hi Samuel!
I used to have that problem, but after reading a post from Harold, I realized I was adding enough base metals, but not stiring.
So, by adding enough silver/copper, 75%+, & stiring good the molten inquart with a graphite or quartz rod, the nitric will find its way thru. 

But if a person fails to do these, the results will be just like you mentioned.

In the pic's of my first try following Harold's steps, the results were much, much better than the ones I'd experienced before. 
No gold dust to contend with & a very "clean" AR solution.
I even used my 3oz gold ingot to get rid of the nitric, instead of evaporating. :mrgreen: 
If I would have ran the "drop" thru AR a second time, I would've had .999. It assayed @ .995 when I sold it. 

Shalom!

Phil


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## shyknee (Feb 14, 2011)

mlgdave said:


> Looking closer it looks like all of the stuff did digest. I have a small amount of distilled water to dissolve the crystals. I will check with stannous chloride filter and do the a r.
> 
> Mlgdave


there is no need to filter, just learn to decant and that way you can wash the gold and do the AR all in the same vessel then filter it before you do the drop (precipitate).


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## philddreamer (Feb 14, 2011)

This is when the dust gives you the trouble, @ this point. :shock: 

:lol: 

Phil


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## mlgdave (Feb 14, 2011)

Thanks Shyknee and Phil, I am taking that on, I did decant, washed, boiled and dried the mud, I have 49 grams (I estimated 48.8 grams of pure) I will now do the AR tonight.

Also want to thank Samuel A a TON, he has been guiding me along step by step and I feel a kinship with you and I think when my wife and I decide to do an international trip it will be to Israel!

So far my first experience has been fascinating, exciting and its like christmas to me, cant wait to see the presents!

mlgdave


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## lazersteve (Feb 14, 2011)

Dave,

Be sure you cool your AR solution completely down with ice before you begin the filtration process. This is a trick I learned from 4Metals and I get silver chloride every time, no matter how well I wash and extract the gold sponge after inquarting. Even on the second refining I'll still get a trace of the white powder.

The AR solution may be crystal clear and orange when it's hot, but will quickly cloud up with silver chloride when the added ice begins to melt. This step is the difference between producing two nines gold and three nines five gold or better in my opinion. 

Don't get in a hurry and follow through with all of the steps for the highest purity gold. If you have cloudiness getting through your filter set up, filter the gold solution again until it is 100% free of particulate and cloudiness *before* adding any SMB.

I look forward to seeing your first gold button.

Steve


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## mlgdave (Feb 14, 2011)

Ok, so the reaction stopped and I have a small amount of grey snowflake like fine powder in the bottom of the pot, is this normal?

I wont be using a coffee pot anymore as my new glass labware will be here tommorow, I dont like seeing my AR on the inside of the lid.





mlgdave


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## lazersteve (Feb 14, 2011)

Yes, that is not abnormal when you have contaminates in the gold. 

It's most likely Silver Chloride or other salts if you used sodium nitrate in the poor-man's AR recipe. 

Add the ice (even if it's already room temperature) and you will see more as the clearer portion of the solution clouds up.

Let the powder settle and filter through a good vacuum set up or through a Charmin plug. Yes, Charmin works best.

Steve


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## Barren Realms 007 (Feb 14, 2011)

Add some distilled water to your solution and the water will have a tendency to evaporate befor your solution does.


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## mlgdave (Feb 14, 2011)

thanks guys, my vaccum filter will be here tommorow, it takes for friggen ever with UPS, but that was my only option with the guy I bought from on Ebay, all my labware will be here tomorrow. I will go add the ice and cloud it up, im curious as to how much AU i will recover.

mlgdave


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## samuel-a (Feb 15, 2011)

mlgdave said:


> Also want to thank Samuel A a TON, he has been guiding me along step by step and I feel a kinship with you and I think when my wife and I decide to do an international trip it will be to Israel!



Dave, you are more then welcomed. Your approach to learning the refining process is amazing, patience is a virtue i always say... 8) 

Everything looks good so far. Steve's ice suggestion is spot on, make sure you drain off every little drop of the gold solution from the walls and lid back into the main solution. Whatever spilled out side, wipe off with filter paper or toilet paper and save for later recovery.


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## goldenchild (Feb 15, 2011)

mlgdave said:


> thanks guys, my vaccum filter will be here tommorow, it takes for friggen ever with UPS, but that was my only option with the guy I bought from on Ebay, all my labware will be here tomorrow. I will go add the ice and cloud it up, im curious as to how much AU i will recover.
> 
> mlgdave



You'll be very close to the original 49 grams.


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## mlgdave (Feb 16, 2011)

ok, I did the ice bath and water, and yes I got cloudy, I did a filtration and it was still cloudy, so then I did a 2nd filtration with 2 filters, still cloudy, 3rd with 2 and still not happy, but now the 4th and final filtration with 2 filters and Im satisfied with it being crystal clear. In goes the SMB, stir, let sit overnight (and HOPE I can fall asleep). I havent yet looked for the thread on reclaiming filters (and wet rags that sat on top of the beakers) but I now have 9 filters and the sludge to store and someday reclaim......................










What a freaking trip when I dropped in the SMB, wow, insta mud! 

I will have my first button tomorrow night! 

mlgdave


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## samuel-a (Feb 16, 2011)

Great Dave !

Now the 'fun' part of washing the powder :mrgreen: 

You are probably anxious to melt your gold, but don't neglect the washings phase, this is where high purity is achieved;
Before washing, liquid should be clear and colorless (if still has a greenish hue, it's OK), swab it and test with SnCl

3 x Tap water washes.
2 x HCL washes.
1 x Boil in HCL wash.
3-4 x Distilled water washes.

Don't forget to test HCL washes as they tend turn out positive for gold, specially the boiling one. Keep wash solutions for later recovery.

Can't wait to see your end results. Good luck


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## mlgdave (Feb 16, 2011)

Ok, so I now have my first bar. I did all the washes and started with 46.2 grams of dried powder (I think it was 100% dry) but I wind up with a bar of 43 grams on the dot. I do have about 400 ml of solution leftover (yes the HCL wash tested positive for PM). I have 9 filters in that soloution as well so I know I will recover some gold from that. I estimated 47 grams is what I should get. I will do the research now to find a thread about recovering gold from filters and waste solution that tested positive. 

I made the mistake of trying to polish the surface of the bar by breathing on it and my tshirt and dang its SOFT. Please ANY input here is greatly appreciated, this was my very first go at refining karat scrap. I now have all the proper labware and do know that the coffee pot is not a method I will use again, I have beakers and watchglass covers














mlgdave


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## Drewbie (Feb 16, 2011)

Drooooooool.


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## jimdoc (Feb 16, 2011)

Nice. Got any nuggets that big?

Jim


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## mlgdave (Feb 16, 2011)

I actually do have some nuggets that big! Im happy with the bar and going to trade it for nuggets in fact!

mlgdave


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## jimdoc (Feb 16, 2011)

mlgdave said:


> I actually do have some nuggets that big! Im happy with the bar and going to trade it for nuggets in fact!
> 
> mlgdave



That would be a cool picture with the nuggets side by side with the bar.

Jim


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## philddreamer (Feb 17, 2011)

Good job! 
It paid to do your home work & follow the advise of those with more experience than you, rather than argue with them.

It would be wise to write the steps down for when you do your next batch; there's the tendency of overconfidence & thus forggeting some of the proper steps.
Been there & done that... :roll: 

This is the greatest Gold Refining Forum!

And yes, let's see some pic's of the bar & the nuggets. 8) Sweetness! :mrgreen: 

Take care!

Phil


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## samuel-a (Feb 17, 2011)

First attempt = Slam dunk ! 
Your gold seems very good and clean, in time pouring bars will come second nature for you i'm sure. 

About your possible losses, here's what comes to my mind;
3.2 grams loss is very high and unusual, I have never experienced that much loss, weight wise or percentage wise.
The loss to filters and and HCL washes never summed up more than 0.05-0.1g for me, no matter batch size.

My thoughts are, if you didn't blow off gold powder from the dish or spilled molten gold out of the mold (and i'm pretty sure you didn't), then the 3.2g loss is due to a combination of reasons; (a) not completing the drying process (b) over-estimating of the initial karat scrap. 
That happens... and will happen in the future and as long as i don't deviate more then 4% (up or down) of my initial assessment of the scrap i'm happy.


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## goldsilverpro (Feb 18, 2011)

The dried gold powder from a recent batch I ran weighed 20.65 oz. After melting, shotting, and drying, it weighed 20.61 oz (about 1.2 g difference). It was melted in a clay crucible in an assay furnace. A very small amount of powder was dropped when loading in the crucible and there are a couple of tiny BBs left in the crucible - these should come close to making up the difference.


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## mlgdave (Feb 18, 2011)

as requested, bar beside some nuggets.









mlgdave


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## jimdoc (Feb 18, 2011)

Very nice. That would be a cool avatar, if you didn't already have one.
Thanks 

Jim


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## mlgdave (Feb 18, 2011)

Yea could be a good avatar, I have about 4000 pictures of gold that I have bought, sold, or found, I alos have this picture of my chest that lets you know a little more why my wife thinks Im nuts.............my back is the OUTSIDE of the mine and about 1/2 covered!









mlgdave
ps.probably going off topic now and should start a new thread but does anyone else have gold related tats?


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## Palladium (Feb 18, 2011)

I've said it before and I’ll probably say it again,but just when i think I’ve seen it all. lol That's what you call loving your work there. Nice tat Dave.


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## jimdoc (Feb 18, 2011)

Nice artwork! I have 12 tattoos, but nothing gold related yet. My brother does mine, so it is just getting down to his house when he has the time.
I should have planned out a sleeve before I got started. Now I am running out of space on my arms, and can only fill in the blank spots. Its trying to tie in all the pieces thats tough, because there is no theme. I have been wanting to get a leprechaun guarding his gold with a thompson.

Yours look like they cost you a decent amount of money (or gold), if you don't know an artist.

Jim


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## dtectr (Feb 18, 2011)

Your wife is right ... you're nuts!


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## HAuCl4 (Feb 19, 2011)

Very cool pics Dave!. 8) The tattoos too!. :lol:


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## djui5 (Feb 20, 2011)

Where did you get your vac filter? Nice bar :shock:


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## mlgdave (Feb 20, 2011)

djui5 said:


> Where did you get your vac filter? Nice bar :shock:


I made the sucker! See my post
http://goldrefiningforum.com/phpBB3/viewtopic.php?f=40&t=9271

60 bucks and 6 2 litre flasks included in that $60.00!

mlgdave


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