Just Finished my FIRST ever GOLD BAR 1.025 Troy Ounce

[kadriver]

When the reaction slowed to a crawl, I used a glass stirring rod and carefully crushed the pieces of brown gold left in the nitric acid.

As soon as i did this the reaction picked back up. I kept crushing the gold mud until there was no more reaction.

 

[kadriver]

I removed the beaker from the heat and this is what was left after i let it settle.

 

[kadriver]

Gold mud after pouring off the silver laden nitric.

I saved the acid to recover the three troy ounces of silver that is dissolved in it.

 

[kadriver]

Here I go doing a second boil in concentrate nitric acid to ensure that all the silver and other base metals are dissolved away from the gold.

All looks well and is going OK for now.

Notice the beaker sitting directly on the coils of the hotplate, disaster is about to strike.

I am new to refining. I learned a costly and important lesson about putting the glass beaker directly on the coil - I WILL NEVER DO THIS AGAIN!

Plus, I am ordering a watch glass to cover the beaker during heating.

 

[kadriver]

The boil was going well. It was a rolling boil, then suddenly it popped and hot acid and gold mud shot about 2 foot straight up.

I was inside watching through a closed window (as I do in all my reactions with heat). I unplugged the hot plate immediately then watched helplessly as the beaker continued to spit hot acid and my gold.

Finally the hot plate cooled and the spattering stopped.

If you are new to this like me, then take note of this mishap and learn from my mistake - NEVER PUT A BEAKER DIRECTLY ON A HOT COIL WHEN BOILING ACID AND GOLD!

Enough said about this - lesson learned.

 

[kadriver]

A close-up of the mess this blunder caused me.

So much for my shiny new hot plate....

 

[joem]

so sorry, now get your metal detector out and start searching under your deck

 

[kadriver]

Here is the remainder of the gold mud being dissolved in aqua regia

Note the corningware dish under the beaker

 

[kadriver]

After about 1/2 hour the gold mud began to look like carrot juice

 

[kadriver]

I slowly added urea to the carrot juice until no mre reaction occured.

Then I added 10 drops of sulfuric acid to remove the lead

I diluted with an equal amount of distilled water and the AuCl looked like orange juice.

 

[kadriver]

Filtering the dissolved gold - note the deep yellow color of the liquid

 

[kadriver]

What was left in the filter paper

 

[kadriver]

here comes the fun part - dropping out the gold with sodium metabisulfite.

 

[kadriver]

The gold began to precipitate before I got done pouring in the SMB

 

[kadriver]

Note the dark brown color like hot cocoa

 

[kadriver]

Pure gold powder at the bottom of the beaker

 

[kadriver]

Stannous Chloride test - there is still gold in the solution.

I added more SMB to get the rest of the gold to drop.

I tested again and the test was clean - all the gold had dropped!

 

[kadriver]

This is what the dropped gold looked like in the bottom of the beaker.

I will let it settle overnight.

Tomorrow I will wash, dry and melt the gold bar.

Thanks for looking - kadriver

 

[4metals]

Nice pictures, are you powering your vacuum with compressed air?

 

[norcalmatt]

Great picture story kadriver. I am sorry to hear about the mishap, but thanks for sharing your mistake. Hopefully you won't be missing too much gold. Any idea's as to why the beaker "exploded". This post will definitely help me with my first refining. Take care.
Matt