# My First proper Refine and some Questions.



## IntelGold (Mar 2, 2013)

Hi, Hope you can help me out as i am not sure what to do next..?
I have added some pics of my efforts so far which i think went well.








This is the final Result and i hope when i melt it down it will be of good purity.  I did not skip any steps so should be good. Just waiting on a Crucible for my melt. It weighs in at 2.2 gram, can i expect a button of 2.2 grams at the end or will some be lost in the melting process??
Before this refine i tried just melting down some foils i had without refining. My question, is there a way of using the AP process to refine the small lump of impure gold i have??
Heres a pic of it, weighing 1.7 Grams.


Thanks for any help and for all the information on the site which helped me greatly with my first proper refine.
Thanks, Ben.


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## jeneje (Mar 2, 2013)

Nice job, on proper processing. Look forward to seeing the button.
Ken


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## IntelGold (Mar 2, 2013)

Thanks Jeneje, But still need to know what to do with my impure 1.7 gram gold button??
Thanks.


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## jeneje (Mar 2, 2013)

IntelGold said:


> Thanks Jeneje, But still need to know what to do with my impure 1.7 gram gold button??
> Thanks.



If it were me i would hammer out to a button, making it flat. Cut the button up in small pieces, boil in a NaOH solution to remove dirt and grease, do a wash in boiling water, decant and use HNO3 (nitric) to remove base metals, decant, wash again decant, cover material with HCL and add very small amount of HNO3 (drop by drop) until the gold dissolves. Be very careful not to add to much nitric(HNO3) it will not take much just a few drops. Use heat set on low. allow plenty of time for the reaction to stop, before adding anymore HNO3. Once the gold has dissolved filter through a charman plug, if all the nitric (HNO3) is expelled double the solution with (H2O) water and drop with SMB.

Hope this helps.
Ken


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## butcher (Mar 2, 2013)

it is easier to re-refine the gold before it is melted back to metals.

Do not forget to study Harold's washing proceedure, look for it in getting your gold pure and shinning.


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## FrugalRefiner (Mar 2, 2013)

jeneje said:


> Once the gold has dissolved filter through a charman plug, if all the nitric (HNO3) is expelled double the solution with (H2O) water and drop with SMB.


Ken,

I believe if you double (or triple) the volume of the solution and chill it _before_ you filter, you might eliminate a tiny bit of contamination. Silver is _slightly_ soluble in a strong, hot AR solution. It is less soluble in a dilute, cool solution. Cooling and/or diluting will cause dissolved silver to precipitate and it can then be filtered out before adding SMB.

Dave


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## jeneje (Mar 2, 2013)

FrugalRefiner said:


> jeneje said:
> 
> 
> > Once the gold has dissolved filter through a charman plug, if all the nitric (HNO3) is expelled double the solution with (H2O) water and drop with SMB.
> ...



Thanks Dave, I will remember to chill my AR before filtering from now on. Any help with removing contamination before dropping is a good thing when purity counts.

I guess adding a few ice cubes to the solution should work for chilling after allowing it to cool down..
Ken


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## Palladium (Mar 3, 2013)

Another important aspect a lot of people overlook is filtering. Double filter you solution through the same filter twice to make sure you remove all contaminates. A new filter paper will allow small particles to pass on the first run until the filter bed is packed good. Just because it looks clear doesn't always make it so.


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## IntelGold (Mar 3, 2013)

Thanks Guys, Does the cooling process work on AP method or just AR? If it does i will add some icecubes made from distilled water in future.
Thanks again,
Ben.


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## butcher (Mar 3, 2013)

Ben,
AgCl silver chloride is insoluble in water and many acids.
AgCl is insoluble in aqua regia, nitric acid or HCl.
The silver that made it this far in your process is no longer AgCl.

In aqua regia being a very strong oxidizer and high chloride content, a very small portion of silver, or silver chloride, can be oxidized to a higher oxidation state to form AgCl2, which is soluble in the concentrated solution of gold chloride of HAuCl3, when diluted with several volumes of water the AgCl2 converts back to AgCl and will precipitate as white powder, even though the solutions pH has not changed with additions of water.

Most salts which are insoluble will precipitate easier from a cold solution than a hot solution, some metal salts are much more soluble in hot solutions than cold solutions, concentration can also play a role in how much of a salt will precipitate out of a solution, normally in concentrated solutions we get more of a salt being pushed out of solution, as normally the solution can only hold so much of that metal.
As we see here with silver chloride in this discussion it does not follow this idea, actually it does AgCl will precipitate from the concentrated solution, but with silver chloride some will also convert to AgCl2 and dissolve into solution as a different form of silver salt, but when we dilute this converts back to AgCl and precipitates out.

In the Copper II Chloride leach (what you are calling AP or acid peroxide) the silver chloride is just AgCl and does not oxidize to AgCl2, so the AgCl stays insoluble in this solution, although it may need time to settle out as a white salt, this solution is also normally dilute any way, as water is a big part of the leach, H2O2 also forms water and oxygen in this leach, the HCl acid is about 68% water.

Now just another tidbit Iron chloride or copper chloride, if heated strongly and concentrated it too can dissolve silver chloride by oxidizing it to AgCl2, but when cooled the silver will again go back to AgCl and precipitate, this was one way they would remove silver from gold ore using hot iron chloride solution,(I have only read about the process, and I think they may have been more details, the old article did not mention dilution but just said cooling, so I am unsure if it was diluted any to get the silver chloride to precipitate). 

The way I understand it a very small portion AgCl becomes AgCl2 in high chloride solutions (acid can help play a big part here) but it can also be that only a small portion of AgCl2 is soluble or the solution can only hold so much of it.

I have tried to find more information about AgCl2, but so far there does not seem to be much written about it, or at least in the places I have looked for it.


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## IntelGold (Mar 8, 2013)

Melted my button today.  Weighs exactly 2 gram. Very pleased.


Sat watching tele last night cutting my batch of fingers off memory. My hands took a battering, 3 lovely blisters..lol
Think i will get them in AP solution tomorrow. If my maths are correct i should get around 4 grams from them, we shall see....!


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## jmdlcar (Mar 8, 2013)

Hi,

Nice button you made there. Can you tell me how many fingers was in that button?

Thanks
Jack


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## jmdlcar (Mar 8, 2013)

IntelGold said:


> Melted my button today.  Weighs exactly 2 gram. Very pleased.
> 
> Sat watching tele last night cutting my batch of fingers off memory. My hands took a battering, 3 lovely blisters..lol
> Think i will get them in AP solution tomorrow. If my maths are correct i should get around 4 grams from them, we shall see....!


Hi,

How many fingers did you cut off of memory last night?

Jack


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## IntelGold (Mar 10, 2013)

Hi,
I read somewhere on the site ----
"As Harold explained once, the gold shrinks when cooled and the result is a hole in the top surface of the gold, usually near the center. This hole is called a "pipe." The pipe is squarish as it meets the squarish crystals. The pipe doesn't appear unless the gold is very pure. The deeper it is, the purer the gold, it seems. On occasion, there will be two pipes"
If you look at my picture i have a nice pipe running in the center of mine, can i be certain by this that my gold is very pure?
Thanks.


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## IntelGold (Mar 10, 2013)

Hi Jack,
I used around 130 but they where mixed and of different quality. I off nearly 300 the other night, so should get a button around the 4 gram mark. I think i will keep an exact record in future so i know what i should be getting from what i process.


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