TCCA (Trichloroisocyanuric acid - pool chlorine tablets)

[haveagojoe]

I'm planning to use the HCl-TCCA (pool chlorine tablets) method to dissolve my next lot of escrap foils over the holidays. Previously I have used Sodium Hypochlorite bleach but I can't find any locally any more which doesn't contain fragrance and other additives. I'm curious to try TCCA as it seems the Chlorine is released into the solution in a more controlled manner, and I've read that it also avoids the potential problem of bleach neutralizing the HCl. When I've done it with bleach, while successful, it seemed like the Chlorine left the solution rapidly and I have been obliged to add more HCl to complete the dissolution, resulting in a large volume and low concentration of gold in solution.

I have read everything I can find on the forum about the method, it seems that the ideal approach is to drip HCl onto the TCCA in a flask and bubble the resulting Chlorine gas into the metal reaction vessel via a tube. I have seen @kadriver Sreetips do it that way some years ago on Youtube and a few other times since.

Unfortunately I don't have the right glassware to do it that way, but it seems that alternatively TCCA can be added directly to the foils in HCl. So I plan to do that; first crushing the tablet to powder and adding it in small doses while stirring, allowing time inbetween additions for the Chlorine to react. I'm wondering if perhaps it would be better to use small chunks rather than crushing the tablet to powder? Maybe that would help to slow down the rate of Chlorine production?

I'm considering possibly covering the beaker and stirrer loosely with clingfilm which I'm thinking might help to keep the gas in the beaker while still allowing me to stir it. After allowing the Chlorine to off-gas I plan to cement the gold out of solution with copper before refining.

Since most of the threads on this topic are several years old I was wondering if anyone had any updates or tips to share regarding this process? I understand @Yggdrasil favours this method, alongside HCl-H2O2- sadly though even H2O2 is becoming more difficult to obtain here in the UK, apparently 12% is the maximum available now and the pharmacy may ask you to complete a questionnaire

I was not able to find any specfic information regarding waste handling for this process but I understand that it produces cyanuric acid, which Wikipedia tells me is classifed as "essentially nontoxic" and "a component of urine" which is somewhat reassuring but I want to maintain caution since this is a new method for me.

Maybe I'm overthinking it but better safe than sorry, so any comments would be much valued.

 

[Yggdrasil]

I'm planning to use the HCl-TCCA (pool chlorine tablets) method to dissolve my next lot of escrap foils over the holidays. Previously I have used Sodium Hypochlorite bleach but I can't find any locally any more which doesn't contain fragrance and other additives. I'm curious to try TCCA as it seems the Chlorine is released into the solution in a more controlled manner, and I've read that it also avoids the potential problem of bleach neutralizing the HCl. When I've done it with bleach, while successful, it seemed like the Chlorine left the solution rapidly and I have been obliged to add more HCl to complete the dissolution, resulting in a large volume and low concentration of gold in solution.

I have read everything I can find on the forum about the method, it seems that the ideal approach is to drip HCl onto the TCCA in a flask and bubble the resulting Chlorine gas into the metal reaction vessel via a tube. I have seen @kadriver Sreetips do it that way some years ago on Youtube and a few other times since.

Unfortunately I don't have the right glassware to do it that way, but it seems that alternatively TCCA can be added directly to the foils in HCl. So I plan to do that; first crushing the tablet to powder and adding it in small doses while stirring, allowing time inbetween additions for the Chlorine to react. I'm wondering if perhaps it would be better to use small chunks rather than crushing the tablet to powder? Maybe that would help to slow down the rate of Chlorine production?

I'm considering possibly covering the beaker and stirrer loosely with clingfilm which I'm thinking might help to keep the gas in the beaker while still allowing me to stir it. After allowing the Chlorine to off-gas I plan to cement the gold out of solution with copper before refining.

Since most of the threads on this topic are several years old I was wondering if anyone had any updates or tips to share regarding this process? I understand @Yggdrasil favours this method, alongside HCl-H2O2- sadly though even H2O2 is becoming more difficult to obtain here in the UK, apparently 12% is the maximum available now and the pharmacy may ask you to complete a questionnaire

I was not able to find any specfic information regarding waste handling for this process but I understand that it produces cyanuric acid, which Wikipedia tells me is classifed as "essentially nontoxic" and "a component of urine" which is somewhat reassuring but I want to maintain caution since this is a new method for me.

Maybe I'm overthinking it but better safe than sorry, so any comments would be much valued.

I favor the use of Peroxide.
I found some old 30% that I used.
I can buy 49% but only in 20L cans.
When I used TCCA I ground it up and drizzled it into the HCl.
Quite effective this way since the Chlorine is released slowly.

 

[haveagojoe]

I've just finished dissolving my gold foils this way and I must say, it is far superior to bleach. Doing it outside with a gentle breeze, the escaping chlorine was barely noticable compared to the stench that bleach creates. The foils dissolved easily with about 10 minutes of stirring, much more straightforwardly than bleach which can require an extra addition of HCl.

In 250ml of HCl at 10% I used about 10g of powdered pool tablet (half a tablet) which I think was far too much, as there are undissolved clumps of it remaining at the bottom of the beaker even after all the foils have been dissolved. I'm expecting less than 5g of gold so it was definitely overkill, 5g of tablet powder would have been plenty.

My idea of leaving some of the tablet in chunks was not a good one, even though they were small. Next time I will make sure it's crushed down as finely as possible as the chlorine stays in the solution more than adequately. I elongated the solution afterwards with 100ml of water, I'm hoping this will give the remaining bits of tablet some space to dissolve completely. I think it will take several days and then perhaps some gentle heating to drive off the chlorine before I add a few drops of sulfuric and then filter it- I was hoping to do the drop on Christmas day but I think that might be too soon. Overall though I was very impressed by the action of the tablet and will do it this way from now on.

 

[haveagojoe]

After settling there seems to be a lot of white sediment, I think there must be some kind of filler in the tablet which doesn't dissolve in the HCl, or perhaps just very slowly. So I decided to go ahead and filter the solution, I figure that should help with releasing the chlorine too. I'll just run it through once to get the bulk of the solids out, then add the sulfuric drops before filtering twice through a fresh filter. If I try to double filter it through the first filter it will take forever. Then I'll put the first filter inside the second filter and rinse through with water.

 

[haveagojoe]

 

[HarryLee1506]

Can this method be used for gold ores?

 

[Yggdrasil]

Can this method be used for gold ores?

Can you elaborate a bit on the pre treatment and composition of your ore?

 

[haveagojoe]

I changed my mind about cementing with copper, after driving off the chlorine with heat I went ahead and dropped the gold out with SMB- which was 10 years old(!) but worked perfectly fine. The gold powder is extremely fine, I think because my solution was quite dilute.

Now onto washes; my first hot water wash has drawn the powder together nicely and improved the colour somewhat; there is a powdery film floating on the surface- is it safe to assume this is not gold and that all the gold is at the bottom of the beaker? In the past I have poured this off into the stockpot but it occurred to me that it might settle to the bottom if I give it more time beween the washes.

 

[BGDOCK]

Could be very fine gold , when I do ewaste with HCl and bleach . The gold drop has s tiny amount that floats. And some that clings to the sides it’s scarlet colored , I try to knock it down with a couple of sprays from the water bottle . Any left over floaters get poured into the stock pot for later recovery . Any thing still clinging to the sides when I transfer to a smaller beaker to clean up the gold powder is wiped up with a Colton ball .

Good luck don’t forget to sent a gold button picture

 

[haveagojoe]

Could be very fine gold , when I do ewaste with HCl and bleach . The gold drop has s tiny amount that floats. And some that clings to the sides it’s scarlet colored , I try to knock it down with a couple of sprays from the water bottle . Any left over floaters get poured into the stock pot for later recovery . Any thing still clinging to the sides when I transfer to a smaller beaker to clean up the gold powder is wiped up with a Colton ball .

Good luck don’t forget to sent a gold button picture

Thanks, I don't think there will be much to show, my heart is sinking as the gold seems to get smaller and smaller with each wash, I think I'll be lucky to get a gram at this rate. I kept the washwater in a seperate beaker, I think I'll have to rework it and try to get some back. I didn't have this problem with bleach, I used bleach which had no additives but I think maybe there's something in the tablet which is making the very fine gold float- although I would have thought after 3 hot water washes and one HCl wash whatever it is would be cleared out by now.

 

[Shark]

Often those floater have some sort of base metal attached to them. I have seen this fairly often where pgm's were involved at times as well. Given enough time and/ or some heat they will settle. They will also float back up soon as disturbed.

 

[HarryLee1506]

Can you elaborate a bit on the pre treatment and composition of your ore?

Pyrite ore with a content of 25g/ton... I used the cyanide method but it was not very effective.

 

[Yggdrasil]

Pyrite ore with a content of 25g/ton... I used the cyanide method but it was not very effective.

Pyrite must be roasted to break the Sulfur bond.

 

[Deano]

The general nomenclature of sulfide ore covers several iron sulfide , copper sulfide, copper iron sulfide and other base metal sulfide minerals such as antimony sulfide.
The treatment methods vary depending on which actual sulfide is present in the ore.
A gold grade of 25ppm is high for a non-upgraded ore, it is more likely to be either a float or gravity concentrate.
In general a concentrate will be more difficult to cyanide successfully than run of mine material, an oxidation step of some sort will be required.
This oxidation step can be thermal, chemical or bacterial depending on the grade and proven size of the ore resource.
If you are effectively at hand mining scale then alkaline oxidation of the sulfides is the simplest and cheapest way to oxidise the concentrates.
It is worth trying to cyanide run of mine material milled down to 85% <75 microns, start with 1% sodium cyanide solution in a 24 hour bottle roll at a 4:1 liquor to solids ratio.
Often cyanide fails because the sulfides use up the oxygen in the leach liquor, get a handheld dissolved oxygen meter to check the DO level at at least 6 hour intervals.
All of the DO meters you can get online are of similar quality, surprisingly good, so you buy on price.
Chlorine leaching of the cons is an expensive way to go, apart from the health hazards associated with it.
Chlorine leaching of head ores is usually not viable unless you have an exceptionally high grade deposit.
Deano

 

[HarryLee1506]

Pyrite must be roasted to break the Sulfur bond.

Oke I understand. Thanks sir

 

[HarryLee1506]

The general nomenclature of sulfide ore covers several iron sulfide , copper sulfide, copper iron sulfide and other base metal sulfide minerals such as antimony sulfide.
The treatment methods vary depending on which actual sulfide is present in the ore.
A gold grade of 25ppm is high for a non-upgraded ore, it is more likely to be either a float or gravity concentrate.
In general a concentrate will be more difficult to cyanide successfully than run of mine material, an oxidation step of some sort will be required.
This oxidation step can be thermal, chemical or bacterial depending on the grade and proven size of the ore resource.
If you are effectively at hand mining scale then alkaline oxidation of the sulfides is the simplest and cheapest way to oxidise the concentrates.
It is worth trying to cyanide run of mine material milled down to 85% <75 microns, start with 1% sodium cyanide solution in a 24 hour bottle roll at a 4:1 liquor to solids ratio.
Often cyanide fails because the sulfides use up the oxygen in the leach liquor, get a handheld dissolved oxygen meter to check the DO level at at least 6 hour intervals.
All of the DO meters you can get online are of similar quality, surprisingly good, so you buy on price.
Chlorine leaching of the cons is an expensive way to go, apart from the health hazards associated with it.
Chlorine leaching of head ores is usually not viable unless you have an exceptionally high grade deposit.
Deano

Wow amazing... I will try, tks mr.Deano.

 

[haveagojoe]

So after struggling a bit with the washes I decided to cut my losses and melt the powder up after just a single refine, and to my surprise the result was quite remarkable, a nice shiny button which even has the beginnings of a pipe on top! The only problem is that it's firmly stuck to a piece of crucible- the crucible cracked so I threw the whole thing into water to quench it at the end.
Any recommendations of how I can release it? I'm thinking I could just soak it in some dilute sulfuric for a while and hopefully the borax will dissolve away and free it.
There are also a few specks of gold which didn't coalesce with the main button, I will have to try to retrieve those too somehow.

 

[Yggdrasil]

So after struggling a bit with the washes I decided to cut my losses and melt the powder up after just a single refine, and to my surprise the result was quite remarkable, a nice shiny button which even has the beginnings of a pipe on top! The only problem is that it's firmly stuck to a piece of crucible- the crucible cracked so I threw the whole thing into water to quench it at the end.
Any recommendations of how I can release it? I'm thinking I could just soak it in some dilute sulfuric for a while and hopefully the borax will dissolve away and free it.
There are also a few specks of gold which didn't coallesce with the main button, I will have to try to retrieve those too somehow.

View attachment 66270

I think you plan will release your button. Especially if it is the Borax that creates the problem.
It will free the other prills to most likely.

 

[haveagojoe]

I managed to free it with a bit of determination... 2.5g on the scale, I'm very happy and quite amazed how well it came out without the second refine. Thank you to everyone here for the help and advice along the way!

 

[Shark]

Gold!

Congratulations.