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Chemical Using Zinc to deal with Tin Oxide from dirty Copper Chloride etches- experiment writeup

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The colour looks a bit more normal after filtering, dropping out the lead with sulfuric, and then double filtering again. Maybe it was just the lighting.

I tend to get impatient at this stage and use an excess of SMB rather than off-gassing the chlorine properly. But this time there's no point rushing as I'm waiting for a new crucible to arrive anyway so I'll just wait. I think I ought to cement it really but the excitement of seeing it drop with SMB is very alluring :)
My first solution was practically red, but it was just 10 ish ml and quite concentrated.
 
My first solution was practically red, but it was just 10 ish ml and quite concentrated.
Yea this time I made a bit more of an effort to keep the volume down as my last one was such low concentration that the drop was ultra-fine and took a long time to settle.
 
Your call.
I decided to take the sensible route of cementing with copper and was pleasantly surprised.

In the past I have found cementation to be a slow process, but this time my solution was still warm after driving off the chlorine on the hotplate, and when I suspended a coil of heavy-gauge electrical wire into it, the whole solution turned dark and cloudy almost instantly, nearly as quickly as an SMB drop.

Shaking the coil after a few minutes released a crust of black powder which quickly settled in a layer at the bottom of the beaker, while the solution continued to darken.

I will leave it to proceed for 24hrs but I think most of the gold will have cemented long before then.

I would be interested to hear if others use gentle heat to aid cementation, as I think this is something I will do again in future.
 
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I decided to take the sensible route of cementing with copper and was pleasantly surprised.

In the past I have found cementation to be a slow process, but this time my solution was still warm after driving off the chlorine on the hotplate, and when I suspended a coil of heavy-gauge electrical wire into it, the whole solution turned dark and cloudy almost instantly, nearly as quickly as an SMB drop.

Shaking the coil after a few minutes released a crust of black powder which quickly settled in a layer at the bottom of the beaker, while the solution continued to darken.

I will leave it to proceed for 24hrs but I think most of the gold will have cemented long before then.

I would be interested to hear if others use gentle heat to aid cementation, as I think this is something I will do again in future.
Circulation is important so all the solution comes in contact with the Copper.
 
Circulation is important so all the solution comes in contact with the Copper.
You're right- after about 90 minutes of continued aggitation, the solution is almost clear with only a slight yellow hue remaining, and only black powder at the bottom and on the coil. I'm amazed how effective it was and I will no longer hesitate to use cementation as a first stage recovery method.
 
You're right- after about 90 minutes of continued aggitation, the solution is almost clear with only a slight yellow hue remaining, and only black powder at the bottom and on the coil. I'm amazed how effective it was and I will no longer hesitate to use cementation as a first stage recovery method.
Cementation is a great first step in rough recovery, because it kills residual nitric acid too. Chlorine isn´t very problematic (pool chlorine/hypochlorite), because solubility of gasseous chlorine in HCl is relatively low. And chlorine is very effectively reduced by SMB too.
But if you are refining with nitric, using cementation on copper assure complete de-NOx-ing and also complete gold precipitation.

It is beneficial to heat the solution below boiling point - it not only speed up the process, but also convection in the hot liquid mix it around and effect better precipitation. Not to mention that precipitates from hot solutions "pack" better and particles clumping together means faster clear-up time and settling/decanting.
 
Yup :(

The Control of Poisons and Explosives Precursors Regulations 2023:

The Following Substances Are Classified as Regulated Explosive Precursors:
Ammonium Nitrate 16% N
Nitromethane 30% W/W
Potassium Perchlorate 40% W/W
Hexamine
Nitric Acid 3% W/W
Sodium Chlorate 40% W/W
Hydrochloric Acid 10% W/W
Phosphoric Acid 30% W/W
Sodium Perchlorate 40% W/W
Hydrogen Peroxide 12% W/W
Potassium Chlorate 40% W/W
Sulfuric Acid 15% W/W
I never thought you will be worse off than us... I very much hate the people who regulate what I can and what I cannot. As a veteran in making all kinds of stupid things in my younger years, experimenting with many kinds of energetics... I really do not see how you will use say phosphoric acid or HCl for explosives preparation...

Here, they totally pissed me off by banning regular battery acid. Like, why ? Who ever misused battery acid ? How ?
 
precipitates from hot solutions "pack" better and particles clumping together means faster clear-up time and settling/decanting.
Yes, this was what surprised me the most, the cemented gold is granular rather than dusty, much larger clumps than I have seen before.
Chlorine isn´t very problematic (pool chlorine/hypochlorite), because solubility of gasseous chlorine in HCl is relatively low.
Well I'm not sure, I seem to have encountered a problem:

After cementation, I let the solution sit for about 18 hours and then drove off the residual chlorine with heat on the hotplate for an hour. I could not smell any chlorine after this.

I decanted the solution from the cemented gold, and then boiled the gold in HCl. The colour improved, going from black to a nice brown which I would normally recognize as a sign of improved purity. Initially the HCl showed no colour change. However, after I left it to cool, the HCl began to turn yellow.

I decanted it off, and in the decanted yellow solution I placed a fresh piece of copper. Black powder began to cement out onto it! So the yellow colour must have been gold going back into solution again!

I added fresh HCl to the cemented gold, and again it began to turn yellow!

I can't figure it out. Perhaps I had not sufficiently driven off the chlorine after cementation, or perhaps there is something in the tablet to keep it in solution and prevent off-gassing. (I imagine that could be beneficial in swimming pools)

The only other possibility I can think of is that rinsing my beakers in tap water left a tiny amount of chlorine residue which allowed the gold to be redissolved.
 
My new crucible won't be here for another week, so in my impatience and in the spirit of experimentation I opted to melt up the cemented gold in a potato :p

Produced this rather sorry-looking little fella, just over 1g:

ugly nug.jpg

The potato crucible works but not very well, the gold refused to melt properly to a liquid, it just glowed dull red and gradually came together in a lump. I think a lot of heat was being wasted in cooking the potato, I just couldn't get it hot enough. I'll melt it up again with borax when my crucible arrives.

All good fun and my 1oz goal is a small step closer :)
 
My new crucible won't be here for another week, so in my impatience and in the spirit of experimentation I opted to melt up the cemented gold in a potato :p

Produced this rather sorry-looking little fella, just over 1g:

View attachment 67515

The potato crucible works but not very well, the gold refused to melt properly to a liquid, it just glowed dull red and gradually came together in a lump. I think a lot of heat was being wasted in cooking the potato, I just couldn't get it hot enough. I'll melt it up again with borax when my crucible arrives.

All good fun and my 1oz goal is a small step closer :)
Budget/DIY heat-resistant materials for small sample melting (not great, some not even good, but usable in desperate situations):

Cement - regular powdered cement for making concrete is naturally heat resistant - as it is dead-burnt at temps exceeding 1300 °C. If you press the powder into some old tin can and make smooth bowl shape using some spoon or whatever, you can melt things in it. Yes, it is "fragile" and easily disturbed, but it works OK. You can mix it with silica sand (regular playsand - but dry it first to avoid popping) and then after shaping it, sprinkle some borax on top of everything.
Do not use any water in the shaping process.
Borax tend to glue the surface together, but be gentle with it and use as little as necessary to make good glazy surface. Otherwise it will be very viscous and bead of metal will "drown" in the viscous borax-cement-silica goo (nothing terrible, but inconvenient).

Magnesia firebrick - used for lining furnances/stoves etc. In the old days, in public/industrial spaces, large electric heating units were installed. They weighed nearly 100 kg each, because they had dozens of magnesia bricks inside - which retained the heat and evened out the temp peaks :) (old soviet block stuff..., maybe not applicable to UK). This was a good source of MgO bricks, which can be cut with angle grinder to appropriate size and holes ground into them using masonry drillbit in the regular (not impact) drill. Prone to thermal cracks when not heated evenly, but withstand temps exceeding 1900 °C.

Silica glass - in "emergency" cases, you can use chips of silica glass for melting small samples of gold etc. All halogen and high power lightbulbs are made of fused silica (due to temperature resistance. If you happen to have some in hand, you can prop it into some sand and use it as miniscule crucible :D (what I will say, sometimes desperate situations require desperate solutions)

High density charcoal - coconut shell charcoal is usable for this purpose, but you need to properly heat it red beforehand to avoid sparking and spitting. It comes in little cubes used for smoking shisha. If forming ash is the problem, you can sprinkle some borax during the melting to keep it down. Advantage is - when the thing lights up, it adds some heat from the bottom of the charge and aid melting :)
 
Budget/DIY heat-resistant materials for small sample melting (not great, some not even good, but usable in desperate situations)
Good to know!
I was just messing about though really. A small quartz silica crucible is only £4 from China, but takes a while to get here.

I added some SMB to the yellow HCl wash solution and a small amount of gold precipitated. So I then added that solution containing dissolved SMB to the main solution which I had cemented from, and after a few hours it turned black. It seems like cementing did not get all the gold out. It's taking a long time to settle as it's very fine.

It will be nice if I can recover a little bit more from this batch, I will probably just add it to my next batch of foils to dissolve again.
 

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