# A golden edge on the end of the year



## g_axelsson

Hi all!

It's been a long journey to get to this point... I'm sitting and playing with my 52 g gold button. 8) 

It started so many years ago, long before I found GRF, almost 30 years ago. I was a teenager and scrapped relays and switches for silver when I discovered something golden in a TV. It was also the time when a schoolkid could buy acids in the nearest paint shop. Soon after I had some nice golden foils and water in a small flask.
Fast forward 25 years. I still got the bug, collecting both silver and gold scrap. processing fingers with nitric and melting into quite dirty gold. I had some ideas about how to refine it but I hadn't put any plan into work, and it was a good thing. Because in 2007 I discovered GRF and joined as member #1059. GRF wasn't as big then as it is today but there were already a lot of information. Not soon after I got my first brown powder of refined gold in an erlenmeyer flask and I was all :mrgreen: 

Since then I have learned a lot, tested different techniques and materials. Sometimes made a mistake but always recovered. Every time adding to my pot in the flask, gram by gram. At first I told myself that I would stop at an ounce, but when I got there I had several batches going so I just continued. Finally this summer I felt ready to re-refine my gold and make that big button.

I started with 53.9g gold, calculated the amount of acid I needed for approximately 4:1 ratio ( 205 ml HCl and 51.2 ml HNO3), then measured up even more HCl (125 ml) as it doesn't hurt and 25 ml HNO3, thinking half a batch of acids is a safe starting point. After a while and some heating the reaction seemed to come to a stop. I poured off the auric chloride via a filter into a flask. Realizing that almost all gold had been dissolved I only added a bit of HCl and only 3 ml HNO3 and it was enough. 54g gold took only 150 ml HCl and 28 ml HNO3! 8) 

Two months ago I brought the gold chloride, beakers, SMB, some sulphuric acid and filters to my parents, showing them how to drop the gold from solution to metallic powder.
The powder I brought back home for final wash (HCL, ammonia and water, never saw any discoloration of the washing liquids) and drying.
I went to my parents over the holidays and I brought the gold, a beaker from Steve and some borax and finally on Christmas day I melted the gold while my dad watched. We managed to melt it using only LPG and air but it took a while.
Sadly, there seemed to be some scrap falling off the fire bricks when melting since I got a bit of discoloration of the borax in one spot and a slight oxide discoloration of the gold button.  
I guess I'll re-refine it again when I got another 50g of gold to add to it.

So... here are the pictures from start to finish. Ok, I start with the button. 8)

52.5 g final button. My red gold 18k ring looks like copper in comparision. 



This is where I started, 53.9 g gold powder dropped with SMB.



Dissolving gold in aqua regia.



HAuCl4 250g/liter. I just love that orange color!



Dropped a second time and dried.



Continued below...


----------



## g_axelsson

Starting the melt.



Almost there...



I made it! I wasn't sure it would be enough heat.



The melting dish afterwards. Only discoloration of the borax in one spot.



Fernlike crystal pattern on the bottom, up to a cm in size. Some small patches of borax still hanging on even after pickling in diluted sulphuric acid.



Ok, let's bring on the comments! I can take it!

Happy new golden year! 

Göran


----------



## Harold_V

Göran,

Well done!

A point to ponder. 

Hard to say what has contributed to the appearance in the first picture, but the frosty surface is an indicator that there may be a contaminant of sorts. When your gold is quite pure, it should yield a shiny surface. 

I refined for more than 20 years. I never got tired of watching gold precipitate. It was often a spectacular display, as I used SO2 from a cylinder, and did my precipitation in large, tall vessels (when re-refining). Imagine watching a solution quickly flash to what could best be described as bronze paint, with millions of tiny gold particles in suspension and quickly moving about. 

Harold


----------



## Smack

Cool art work in that button, I see lots of pine trees.


----------



## CBentre

30 years in the making, great story and well done. Looks like I have another 28 1/2 to go. I'll tell you one thing though, if I ever do tackle that art it will be well worth the wait. Looks awesome!


----------



## g_axelsson

Thanks!

I'm suspecting that a small piece of iron dropped down from the top brick at the end of the melt. If the contamination was there from the beginning I would expect it to discolor the borax all over the dish. I should have brushed the fire bricks with a wire brush, my dad uses them for support when he welds.
I was quite disappointed when I didn't get that mirror surface. But part of the disappointment is offset by the cool crystal forms, triangles of crystal surfaces. You can actually see the cubic structure of the gold crystal. 8) 

I'm already started on the next batch... 1.1g in the flask already. 8) 

Harold, once I got SMB down (dissolved in water) to the bottom of the gold chloride, creating small SO2 bubbles that left tracks of precipitated gold going up towards the surface. It must have been something like that when you used SO2 gas. It sure is a "magical" feeling to drop the gold.

Göran


----------



## butcher

What great way to end the old year, and begin the new year.
Thanks for sharing, and for the pictures, I know this was exciting for you doing it, but I kind of get excited just seeing the pictures of what you have done.


----------



## Harold_V

The characteristic pipe is also missing from your button. Your explanation of iron contamination may explain why. 

I've seen a pipe pulled so deep it looks like a cliff--and the color within the pipe is breathtaking. Happens only with *very* clean gold. 

When working with refined gold, everything must be clean---even the torch. The slightest thing can ruin a lot of hard work. 

Harold


----------



## butcher

Well ruined or not that is a darn pretty 52.5 g gold button, any one should be proud of, besides with about 8 grams more, we can watch Göran change it into a beautiful pure 2 troy ounce gold button.


----------



## goldsilverpro

In my experience, the presence of a small amount of Pt group metals can produce that fern-like crystal pattern.


----------



## artart47

Mykert bra Goren!
What a feeling of accomplishment ,eh! Gold powder sitting there for 30years. I could never do that. I get so affraid that it might get broke and the powder would get lost. Plus, I love seeing it in the melting dish turning into a button.
If you already have another 1.1grams, then we should be seeing your 2 oz button before long!

You can melt without the fire brick. Get a handfull of the insulation that they use around the ductwork for restaurant exhaust hoods or in boilers. just lay it in the surface set your melting dish on it and then pack the insulation around the outside af the dish. you can melt two ounces with a map-gas torch and no air or oxygen. that way the heat stays in the dish and you don't have anything over it that can fall in.
Beautiful work! I like the pattern it has.
artart47


----------



## its-all-a-lie

The crystal pattern was explained before by Lou, if I remember right he said it was a sign of very high purity, meaning .9999+. Every bit of gold I have refined has had this same pattern when melted. The only time I have achieved a pipe in any of my gold, or silver, has been when allowing it to cool under a flame lacking oxygen. This bar was refined twice today from gold filled material and weighs just over 26 grams.


----------



## Harold_V

Oxygen has nothing to do with a pipe forming. It's the result of very pure gold shrinking as it cools (in the process of solidification). The final freezing creates the deep pipe as the center solidifies and shrinks. In the process, the pipe is formed. It can be avoided by continually heating the entire surface of the gold, so it cools from the bottom up, and shrinks uniformly, cooling very last at the center, at the surface. In such a case, the surface ends up concave, but with no pipe. 

I strongly disagree with the notion that the crystal formation shown is the result of very pure gold. When gold is extremely pure, it forms a huge crystal structure, with the surfaces within the crystal boundaries being very shiny. I witnessed that routinely. In all my years of casting ingots, I never once managed to achieve a surface such as that which was shown. If pure gold was the reason, I'd have experienced that surface routinely, and commercial ingots would be fraught with the pattern. They NEVER are. 

I defy anyone being able to create that pattern with pure gold. It just doesn't happen. And, I tend to agree with GSP---I had a small ingot submitted to me to be included with a lot I refined. It was obvious by the color and surface condition that the submitted bar was not pure, in spite of the fact that it was marked as such (anyone can stamp an ingot). The small ingot (about a half ounce) was re-processed, resulting in a solution that tested positive for platinum. It takes very little of the wrong contaminant to cause gold to form that small crystal pattern, which also accounts for the lack of a pipe. The material freezes before it can form, as it has a narrow liquidus state, due to the contamination. 

Harold


----------



## g_axelsson

Thanks for all the comments!

That could explain my crystal patterns and lack of pipe.
Firstly I let the button cool slowly by just backing off the flame. Secondly, some of the gold came from dental materials, I dropped a couple of grams of gold from a solution that looked like amber afterwards. I also processed my stock pot and it had some PGM:s in it. So there is a high probability of PGM contamination.

But there is some base metals in it too, as the unprotected surface got an oxide cover when I removed the torch. Unless palladium can oxidize a bit even when mixed up in a lot of gold.

Anyhow, this gives me a perfect opportunity to try out a small Wohlwill gold cell. I just need to extract gold for the electrolyte and then I'm in business. :mrgreen: 

Göran


----------



## goldsilverpro

When I had my last refinery, most all the gold was torch melted with acetylene/O2 and cast into 10 oz bars in a preheated graphite mold. I never kept the flame on the bar after pouring. The purer the gold, the deeper the pipe and the larger the squarish crystals (sometimes as large as 1/4"). When really pure, there was a slight separation between the large crystals, especially those nearest the pipe. I reworked any gold that was discolored (usually reddish), exhibited a fernlike crystal pattern like the photos above, or that with no pipe or squarish crystals. I probably ended up reworking about 5% - 10% of the bars. If the gold wasn't too much off-purity, I remelted with small alternating pinches of niter and borax in an attempt to make it acceptable. This usually worked.


----------



## glondor

Inside the "pipe"


----------



## g_axelsson

Glondor, that one is just extreme! 8) 

I guess that the niter and borax trick doesn't work when dealing with PGM contamination.
Anyhow, I think I will try to remelt it next time I get back home to my parents.
Thanks for the tip, Chris.

Göran


----------



## moose7802

Looks like glondor picked that gold out of the dish before it completely solidified and squeezed it a little to hard. I have had the same thing happen, I just re melted it. But that does look pretty cool glondor! 

Tyler


----------



## Harold_V

Glondor's pictures are a perfect example of what I've been talking about. Note the large crystal pattern on the surface, and how shiny the gold is within the boundaries. Also, I had commented on the extreme beauty of the gold within the pipe. This one is an exceptional display of the enriched color. 


Harold


----------



## necromancer

Harold_V said:


> Glondor's pictures are a perfect example of what I've been talking about. Note the large crystal pattern on the surface, and how shiny the gold is within the boundaries. Also, I had commented on the extreme beauty of the gold within the pipe. This one is an exceptional display of the enriched color.
> 
> 
> Harold



how would you rate this Harold ?

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=61&t=20404&p=209000#p208960


----------



## g_axelsson

Harold_V said:


> The characteristic pipe is also missing from your button. Your explanation of iron contamination may explain why.
> 
> I've seen a pipe pulled so deep it looks like a cliff--and the color within the pipe is breathtaking. Happens only with *very* clean gold.
> 
> When working with refined gold, everything must be clean---even the torch. The slightest thing can ruin a lot of hard work.
> 
> Harold


Now, this is a pipe!



It was sooo beautiful, sitting in my hand in the morning sun... 8) 
The central pipe consists of a flat surface with raised edges that have sunk straight down. At the edge you can see fern like crystal growth in several places. In the picture you can see it at 4 o'clock. 

And this is the back side, a golden moon. A thin surface of borax remains, but is only visible when looking through a pocket lens.



Re-refined with inquartation... will add more in a while.

I'm happy now!

/Göran


----------



## jason_recliner

Göran, that is amazing. I tip my hat to you sir.


----------



## Anonymous

Nice one Goran, I take it that's from the Pentium Pro haul?

By the way recently GSP alluded to the fern pattern on your original pic showing the presence of PGMs in the gold. 

Jon

edit:

"Postby goldsilverpro » June 13th, 2015, 1:53 am

Usually, in my experience, fern patterns indicated PGMs. When I got a fern pattern, I re-did the gold. Too low melting temperatures can produce ferns."


----------



## g_axelsson

Just as you wrote, Jon, I remembered that GSP wrote somewhere that a fern like structure and a frosted surface could hint of palladium contamination and I started to suspect that it was what I had in my original button. So I wanted a method that could eliminate any palladium before precipitating the clean gold. Inquarting filled that goal.

So I brought out my cemented silver powder and started to melt 150g (probably with quite a lot palladium) and added the gold in the end. The molten alloy was poured into water and made some quite spectacular cornflakes. Some of the pieces were gold colored so I suspected that I didn't get a good mix. Another melt, mixing well and pouring it into water again... now I got a large piece among all others as I poured too fast. I definitely need more practice.


Anyhow, I started to run out of time but thought that I should try to treat it with nitric, any pieces that didn't dissolve I could remelt with some more silver. I still had pieces I suspected was high in gold.
I started treating the alloy with nitric (diluted down to 30%) but the reaction was quite slow so I put it on one of my coffee maker hot plate. Still slow to react so I took out a borrowed hot plate and increasing the heat slowly until I get a modest reaction. After a few hours the reaction had died down, so I exchanged the acid for fresh and ramped up the heat again.


The third time the reaction slowed down with a lot less color in the nitric so there probably were a lot of acid left. Now I washed off the brown clumps with water and boiling. With a spoon I tested the consistence of the gold and it just broke apart with no hard centers, it seemed the dissolving of the silver was perfect.


After a few boiling water washes I added hydrochloric acid and was greeted by a silver chloride cloud that disappeared within seconds. Then small bubbles appeared from the gold, remaining nitric had formed aqua regia and started to dissolve the gold.
I added some more nitric, keeping it low so I would have excess HCl. When the reaction (heated on a coffee maker hot plate) died down I poured off the gold chloride, diluted it with two parts water and filtered it with my vacuum filter equipment, first time I use it. It worked great and really fast compared to gravity filtering. The filter took a purple tone from silver chloride.


Second batch went the same way. Then the third batch with the left over gold started to slow down even when I added a bit of nitric acid. I thought it could be some pieces with undissolved silver that became inert in the AR.



... to be continued ...


----------



## g_axelsson

So I started to pour off the final gold chloride and I realized the pieces were just fluffy silver chloride clumped together. With the spray bottle I could disintegrate the clumps and there were no solid metal left. The nitric had penetrated every piece of my inquarted gold. The silver chloride ended up in the filter paper.


As I had used extra nitric in the last step I got a perfect opportunity to test sulfamic acid to destroy the excess nitric. I was surprised by the modest reaction, maybe I didn't have that much excess, I'll do some experiments some other times.
To precipitate the gold I used SMB and it happened without any drama, a thick layer of brown compact mud formed on the bottom of the beaker.


Then I went on to wash with HCl and water until I got no change in color.


Then drying and melting. When the button started to solidify and the pipe formed I realized I had manage to raise the purity and it was pure magic to see the pipe with the red glowing metal inside the button.



... well, that's all. :mrgreen: 

Göran


----------



## g_axelsson

spaceships said:


> Nice one Goran, I take it that's from the Pentium Pro haul?
> 
> By the way recently GSP alluded to the fern pattern on your original pic showing the presence of PGMs in the gold.
> 
> Jon
> 
> edit:
> 
> "Postby goldsilverpro » June 13th, 2015, 1:53 am
> 
> Usually, in my experience, fern patterns indicated PGMs. When I got a fern pattern, I re-did the gold. Too low melting temperatures can produce ferns."


Thanks!

No, this is the gold from the start of this thread. I haven't had time to do anything with the processors yet, not even sorting them. My company have taken off this spring (AV installations and programming) and I've spent whole weeks out of town. The few hours during weekends have been spent to try to keep up with all fun scrap that's flown in lately... A car load of servers, several lasers and other equipment from the university, a +/- 10V 100A computer controlled power supply, two 5 Mbyte hawk disks and a full cabinet for a mini computer from 1978, all keepers except the servers. 8) 
Now I have one week in Norway (vacation) and one in Denmark (work) then maybe I can find some time to process the CPU:s.
I have a vision of processing the CPU:s during summer and creating a number of buttons like the one above.

Göran


----------



## glorycloud

Very nice work Göran!!


----------



## Silver Sliver

Beautiful!


----------



## MarcoP

For sure your holidays are going to be great after this satisfying achievement


----------



## FrugalRefiner

Very nice Göran!

Dave


----------



## Palladium

Very nice!


----------



## maynman1751

Nice job Goran! Beautiful button! 8) :mrgreen:


----------



## Barren Realms 007

Nice looking button there. You should be proud of it.


----------



## g_axelsson

Thanks everyone, I really like my new button and I have a hard time putting it away. I just take it out again and again, just for looking at it. I can't get enough. :lol: 

Göran


----------



## solar_plasma

You could wear it on a chain around your neck. Very nice! I hope to make my 12g button this week.


----------



## machiavelli976

g_axelsson said:


> The molten alloy was poured into water and made some quite spectacular cornflakes. Some of the pieces were gold colored so I suspected that I didn't get a good mix.



Not necessarily. Could be the result of an known phenomena called float zone diffusion which is used as a purifiyng method of metals and metaloids , named 'zone melting' .

It happens on gold inquarting recovering process when the pouring is done near the water surface. To avoid this , needed to be poured from a distance which allow cooling and pre cristalization of the falling drops.

I one , prefer to cool slowly as a long bar and cut it than in small pieces or thin slices .


Anyway , nice job !!


----------



## g_axelsson

machiavelli976 said:


> g_axelsson said:
> 
> 
> 
> The molten alloy was poured into water and made some quite spectacular cornflakes. Some of the pieces were gold colored so I suspected that I didn't get a good mix.
> 
> 
> 
> 
> Not necessarily. Could be the result of an known phenomena called float zone diffusion which is used as a purifiyng method of metals and metaloids , named 'zone melting' .
> 
> It happens on gold inquarting recovering process when the pouring is done near the water surface. To avoid this , needed to be poured from a distance which allow cooling and pre cristalization of the falling drops.
> 
> I one , prefer to cool slowly as a long bar and cut it than in small pieces or thin slices .
> 
> 
> Anyway , nice job !!
Click to expand...

I learned a new thing today! Thanks, that could explain what I saw. I could still see some shiny surfaces in the nitric bath but they disappeared at the end. Probably so thin that they crumpled when the silver behind dissolved.

Göran


----------



## machiavelli976

You can see shiny surfaces of the flakes also if the inquarted gold has quite much undissoluble (regarded to nitric) PGM's , like platinum or rhodium .

In such situations , it may happen that nitric digestion to be unable to crack the flakes or chunks of the alloy , even if the acid penetrates the whole structure . So said , you'll got parted flakes of almost intact initial shape but of course much lighter in weight and with some shiny , slightly dull aspect .

It happened to me even to exagerate alloying ratio like ten to one , let's say... The unreacting PGM's keep away the gold to disintegrate in that grinded-coffee like, status .


----------



## malfeces

That is just beautiful! Good work!!! I can only imagine how heavy that must feel in your hand.


----------



## g_axelsson

It is a nice feeling. 8) 

Göran


----------



## Tndavid

Just read this. Beautiful story with a wonderful end result goran!!!!


----------



## butcher

Bump this thread, Eye candy for sure, beautiful in the liquid state or the metal and just gorgeous as metal.


----------



## archeonist

This post makes me want to create a new button this christmas!


----------



## g_axelsson

I have some plans for silver this year, though I have enough gold powder to make a big sister for this one.

Göran


----------



## AuPure

Can't wait to see the silver.

I really wish I had enough material to make even one button that big. It took me over 6 years of cherry picking stuff here and there and I still probably won't even come close to 1/2 an oz. 

All of you make me so jealous :mrgreen:


----------



## g_axelsson

That button contained gold from scrap that I saved for 30 years. When I visited Jon this summer I finally refined some gold plated pins I collected between 1984 and 1988.

So a mere six years is nothing to complain over. :lol: 

Göran


----------



## AuPure

g_axelsson said:


> That button contained gold from scrap that I saved for 30 years. When I visited Jon this summer I finally refined some gold plated pins I collected between 1984 and 1988.
> 
> So a mere six years is nothing to complain over. :lol:
> 
> Göran



:shock: 

Now I really don't feel so bad. I guess after reading so many posts on here from so many members I just assumed all of you got truck loads of scrap at a time. :lol: 
(Of course I'm exaggerating)


----------



## butcher

These metals are considered valuable for more than just their looks.
Because these metals are so hard to get makes them so valuable.

Besides my truckload of gold was just way too heavy for my old bald tires, after the tires blew, I had to leave that old truck on the side of the highway, Oh well, maybe I can buy some electronic scrap from eBay and some overly expensive chemicals and get another truckload of gold, I can dream can't I.


----------

