Non-Chemical IC cons for resabed01

[rusty]

Well, my concentrates arrived back home Monday. There's about 1100g from the chips I sent, roughly 10% or a bit less.
I'm itchin to start processing the cons but I have a few other things I'd like to clear off and finish first. I'm also waiting on a set of beakers I ordered. Plus we're still waiting for nicer weather here. It's snowing again tonight :x .

I was thinking of mixing it well and starting a 100g test batch. Then I can see what percentages of base and precious metals I have. Playing around with a magnet there seems to be a fair bit of iron in there and I'm guessing lead too. We'll see when I get out the acids. I'm still mulling a process over in my head. Been reading Hokes book again to get some direction from her and refresh my memory. the first time I read her book it didn't make much sense. Now that I'm reading it again 3 or 4 years later it's all clicking now.

Thank you very much for running the chips through your centrifuge, Rusty.

Your welcome, yea your probably going to have excess garbage as this was not my material and had given it a few extra runs through the centrifuge to make sure I had captured all the precious.

The very top layer in the canister is ball mill sweeps.

I recently purchased some random chips from ebay, this jar is what I'm currently working on.

After the ball mill, recovered the concentrates of which went without incineration or a HCL pre-leach.

Straight to 50/50 nitric for silver, after removing the chloride returned the liqueur to the AR in the jar. Any palladium will be recovered later.

The insolubles after settling out last evening, four distinct colors.

Be sure to post pictures as you progress with your journey into the world of concentrates, you will enjoy working them.

Best Regards
Rusty

 

[resabed01]

Well, it's time I started working on these concentrates. Last night I got the heavy lump dissolved into a tub of water and did a separation of the magnetic material.
I did this in two stages. From the concentrates bath I captured with a magnet whatever I could and transferred the mud to a intermediate bath. From the intermediate bath
I did the same, transferred the magnetics out into a 3rd tub for collection. I did this to separate out any material that was non-magnetic that got dragged out from the first bath.
I'd say I got the majority of the magnetic material, not all. The chips were milled superfine which makes a slick, heavy paste when wet.
After a night of settling i poured off the excess water which was pretty clear. I plan on processing these two separately.



The coffee pot on the right is the concentrates, the left is the magnetic material. I started the magnetic material in a HCL leach tonight after I poured off most of the water.
I slowly added HCL not wanting to over do it at first. I kept adding until I had about 50/50. The reaction was started and the pot was self heating and gassing from the reaction.
I'll give it the night to react and I'll tend to it again tomorrow.
The other pot of concentrates I wanted to give it a additional night to settle before I pour off the water.

Nice thing about working with milled material is the particles are so fine and small it takes no time at all for the acids to do their work. Not at all like a crock pot of pins that
will take forever it seems to digest.

 

[rusty]

The slick heavy paste will contain some insolubles and these are going to give you a major problem they will form a heavy layer over the values keeping the acids away. You can either stir or divide your material into several containers so that your bottom layers are thinned out.

I started out with three 20 liter pails, then when I thought the leach had done it deed added the sludges into one pail as i only have one torch. The cons have been on heat all week then over the weekend and more today and still not done.

The precious metals will form a crust under the insolubles which become slimy and runny you can pour these off the crust sticks to the bottom of the reaction vessel you almost need a jack hammer to loosen them up so there is no fear of loosing any.

I've saved the slimes to rework later.

Today while heating my leach fell asleep reading a book when I woke found that most of my leach had evaporated away, this is why my gold chloride crystallized in the filter flask.

For those working incinerated chips you will not experience the heavy crusting of precious metals under the slimes I mentioned above, concentrates is a world to its own.

Do not forget to go after your silver and palladium after the HCL leach, you may have to incinerate before going to nitric.

Heating your coffee carafe be wary of the precious metals crust which has formed on the bottom, they can and will form super hot spots which could crack your pot. I use a stainless steel screen between the pot and hot plate for light heating and a pan full of sand for more vigorous heating.

To heat the 20 liter plastic pail cut the top off an old propane tank, then added a brick to the bottom filling it with water, using a tiger torch to heat the water.

 

[butcher]

When I have powders to heat the ceramic casserole dish is my tool of choice.

Rusty is correct about the powders settled in the bottom of the coffee pot, creating a hot bottom which will crack the glass at the base of the pot.

 

[resabed01]

I know the limitations of the common coffee pots but I appreciate the reminder anyways. I like using them because they are cheap (more like free), easy to handle and transparent unlike HDPE. I generally don't like to heat HCL solutions other than to drive off chlorine or evaporate excess water from wastes. Time is on my side, I have lots of it and normally don't try and speed things up with heat.
There will be times when I go out of town for a week or more and I'll leave the leaches go at their own pace, stirring, decanting or adding more acid when I get around to it. I don't find heating necessary.

I was lucky enough to find a small Pyroceram dish at a Goodwill store for a couple of bucks. This will be my dish of choice for incineration. I just wish I could find a larger one.

One question, when I added HCL to the fraction with the magnetic materials, I got gassing from the reaction. I'm assuming this was hydrogen as the HCL reacted with the base metals. I also got a wiff of rotten eggs which tells me H2S was there as well. It wasn't very strong but still noticable. Is it common to see H2S gas from a reaction?

 

[butcher]

I am not sure where any sulfides would have come from.

Base metals when acidified can give off hydrogen gas in the reaction, if they are above hydrogen in the reactivity series of metals.

 

[johnny309]

Chips cases made from plastic contain sulphur as an hardening agent of the plastic material ....so it is possible to encounter sulphur compounds.

 

[resabed01]

Well, whatever it is.... it's nasty. Trying to avoid exposing myself to the smell

 

[rusty]

Well, whatever it is.... it's nasty. Trying to avoid exposing myself to the smell

I'm surprised no one has mentioned it, you should have treated the cons as you would process bench sweeps - incinerate first.

 

[resabed01]

ooops!... you're right, I never incinerated this batch

 

[rusty]

ooops!... you're right, I never incinerated this batch

It's unfortunate that Harold is not spending as much time on this gong show as he used to put in, his mind is sharp as a tack and he would not have missed making that suggestion to incinerate.

It seems the entire class has fallen asleep.

 

[seanconnrey]

my advice is not to run aqua regia prossece at first because u well lose
silver metal he well be transformed to Agcl and mexid with the powder .

base metal can be taking with hcl

Hcl dose not react with silver in my knowledge

if u want to save your silver u must run hno3 wash but if u have a lot of
Tin u must be carful with Tin past he well cause a serieus problem when
filtring the solution.

 

[rusty]

resabed01 what stage in this project are you, curious how its progressing.

 

[resabed01]

Not much happening with the recovery... been working on other things. Just spent two of my three day weekend working on the son's car, fixed up a few things and general maintenance.
As soon as I get some more days off work I can get back at theses cons and get some leaches started.
I do all my recovery and refining outdoors and right now the mosquitos are fierce and plentiful so there is not much motivation to go outdoors at the moment :x

 

[butcher]

If it isn't the cold rain and snow its the skeeters, well they will not keep me from the lab having fun.
Now keeping the vehicles running does keep me from enjoying the lab. :lol:

 

[resabed01]

Today I wanted to get started on these concentrates. The chips were milled and concentrated but never incinerated yet so I expect there will be considerable resins in the mix from the IC packages. Not sure if these resins would be inert or cause me problems down the road so I decided to start by incineration first.
The cons are milled very fine, any handling causes clouds of dust to be formed so I have to be careful.
Transferred the cons to a ceramic dish and placed in on the BBQ side burner. I didn't think my 1500w electric hotplate would be up for the task. The gas burner throws a great amount of heat. About 20min in med then after I cranked it to high and let it cook for almost an hour and I watched as the powder changed color starting from the outside and slowly work towards the middle. I knew things were getting hot because the piece of steel I used for stirring and breaking up the lumps came back blue from the heat. Never seen a powder "boil" until today. No smoke but a fair bit of smell.
Not sure if what I did was effective or a waste of time/fuel. It's difficult to incinerate that much powder because the oxygen has no way to get down inside the mix aside from me stirring it.

At least I found out the pyroceram dish is up for the task.

Any suggestions on incinerating almost 1Kg of finely milled concentrates?

 

[rusty]

Looking good resabed01, whats next to do.

Wet everything down with a layer of water, mag the fine iron filings out.

You can leave the water to use for your dilute nitric leach, 50/50 water acid when going after the silver and any palladium there could possibly be in there.

Filtering is going to slow you down a tad, try wicking.

Use distilled water on that silver rinse, the distilled water is free of minerals looking to grab some along the way.

I'm using HCL to convert the silver nitrate to silver chloride, then going the scrap iron route to convert this into metallic silver.

Once your satisfied all the silver nitrate has been wicked from the concentrates, proceed to go for the gold using the leach of your choice.


A word of caution, those finely divided powders react violently to acids, I add the acids to my cold and concentrates let the acid work on the cons for a half an hour or more before adding more acid, string at this next addition then when I'm satisfied the acids have taken up some of the metals I add the heat with a very slow paddle speed.

The heavy metals will form a layer under the insoluble mud, so be careful string as not to bring up to much metal into the hot acid at once or you'll have a boil over.

Here's a boil over I had this afternoon, caused by to much paddle speed for too long a duration. You'll not be so lucky should you have a boil over, the reactor saved the day. Didn't loose a gram of values.

 

[butcher]

resabed01,
If you would not fill the dish so full when incinerating you will have more room to stir the powders better exposing them to heat and air or oxygen, of course you would have two batches to process.

 

[resabed01]

resabed01,
If you would not fill the dish so full when incinerating you will have more room to stir the powders better exposing them to heat and air or oxygen, of course you would have two batches to process.

As they say, hindsight is always 20/20. I thought the same after I started incinerating. The volume of the powder seemed to increase as time went on and the heat climbed. As I stirred the texture was much like ash, light and fluffy.

I have two larger sized Corning ceramic dishes here but I'm not 100% certian they are pyroceram so that's why I went with the smaller dish, it's marked. Is there a way to test them? Perhaps placing the empty dish on the burner and cranking the heat up to high? I'd hate to have one of these explode on me sending hot ceramic shrapnel everywhere.

 

[resabed01]

Looking good resabed01, whats next to do.

Wet everything down with a layer of water, mag the fine iron filings out.

You can leave the water to use for your dilute nitric leach, 50/50 water acid when going after the silver and any palladium there could possibly be in there.

Filtering is going to slow you down a tad, try wicking.

Use distilled water on that silver rinse, the distilled water is free of minerals looking to grab some along the way.

I'm using HCL to convert the silver nitrate to silver chloride, then going the scrap iron route to convert this into metallic silver.

Once your satisfied all the silver nitrate has been wicked from the concentrates, proceed to go for the gold using the leach of your choice.


A word of caution, those finely divided powders react violently to acids, I add the acids to my cold and concentrates let the acid work on the cons for a half an hour or more before adding more acid, string at this next addition then when I'm satisfied the acids have taken up some of the metals I add the heat with a very slow paddle speed.

The heavy metals will form a layer under the insoluble mud, so be careful string as not to bring up to much metal into the hot acid at once or you'll have a boil over.

Here's a boil over I had this afternoon, caused by to much paddle speed for too long a duration. You'll not be so lucky should you have a boil over, the reactor saved the day. Didn't loose a gram of values.

Thanks for the advice Rusty. Magnetic seperation was the first thing I did. From the total I pulled out almost 10% of the solids that were magnetic. Some small trace amounts still exist but I don't think there will be enough to cause problems. I'll give it another water wash and go over it with the magnet again before I start leaching. I think my biggest enemy here will be tin. I wanted to do a HCL leach first to remove tin, aluminum and anything else that wants to hitch a ride with the HCL. After that, incineration again before moving onto nitric acid.
Before I start any leaches I want to find a suitable vessel that will be large enough to prevent boil overs as I expect a fairly rowdy reaction. Four litres would be enough, maybe more. I know the coffee pots won't work in this case.