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Grelko said:
macfixer01 said:
The lids are not made of silver, I believe rjamjb was probably just referring to them as silver colored?

I should have cleared that part up a bit. I meant the copper when he cut the lid, I didn't mean that I thought the lid was silver plated. They just seem to be aluminum plated over copper, some have the small square of gold plating on the inside.

rjamjb said:
I have an outhouse away from any day to day activities/third parties and will undertake this first activity there. There is an outside area I can use safely. Russell

This may seem like an odd question, but I'm just being on the safe side for rjamjb's health.

Does anyone happen to know if the chlorine/hydrogen fumes from the HCL/H2O2 dissolving metals, combined with methane etc, from an outhouse, to become something even more of a toxic mix for your health?

All I know, is that it would be very flammable, especially if the fumes get concentrated, but could it have the potential to self ignite, since an outhouse is a confined space even with the window and/or fan?

Besides that, you would definately want a fan blowing the fumes away from you also "fume hood, scrubber, etc", if you are working inside a small area like that.

Edit - typo


Rjamjb appears to be from the UK. I'm going to go out on a limb here guessing that when he said "outhouse" he didn't mean the same thing as what an outhouse in Pennsylvania is? I'm assuming he just means a separate structure away from the house, such as a shed, and not an outdoor privy. Actually one definition of outhouse is any outbuilding.
 
HI - Yes I'm from the UK and my 'outhouse' is approx 50 meters (150 yards) from any other inhabited building (it is a shed in UK terms about 4meters by 3 meters).

I'm not happy with the safety aspects of running any of the bubbling processes inside now and will not do that. In fact I am going to slow down a bit and go for the hcl with small additions of h2o2 only to start with. Am going to rig up a small covered space open to the air (rain proof) and let it stew for however long it takes.

Russell
 
macfixer01 said:
Rjamjb appears to be from the UK. I'm going to go out on a limb here guessing that when he said "outhouse" he didn't mean the same thing as what an outhouse in Pennsylvania is? I'm assuming he just means a separate structure away from the house, such as a shed, and not an outdoor privy. Actually one definition of outhouse is any outbuilding.

Yes, the way I've heard the word used, was for an outdoor privy, thats why I was concerend about the mixture of fumes. I never knew that it meant "any" outbuilding. So for me, that small building would be a shed or "shanty". I'm learning new things here everyday.
 
Definitely two countries divided by a common language!!!. This really made me chuckle. Outhouse vs privy vs WC vs shed vs Shanty vs...... who knows!!!. Anyway my "one of those" is a wooden construction one room with a couple of windows that I keep gardening gear in!!.

I've been splitting the lids apart with a hammer and putty spreader, slowly for now. By the end of the week I'll hopefully be in a position to share some more pics.

A couple of points - if, as an earlier post says, I'll get about 0.1g gold per 20 chips then I'll be lucky to get about 0.7g out of this batch. I'll count them up, weigh them and post some weight details once I've done the splitting. I'll keep records along the way for others to follow.

I never did get a clear answer as to whether the gold color on the underside of the lids were actually gold - someone mentioned a sulfuric bath for those. Can anyone comment on whether this is the correct approach for that and whether it is definitely gold?. I believe btw, following a bit more research that the lids are copper covered with nickle.

Russell
 
It's gold, look at this search... http://goldrefiningforum.com/phpBB3/search.php?keywords=indium+copper+gold+heat+spreader&terms=all&author=&sv=0&sc=1&sf=all&sk=t&sd=d&sr=posts&st=0&ch=300&t=0&submit=Search

Göran
 
rjamjb said:
I've been splitting the lids apart with a hammer and putty spreader, slowly for now. By the end of the week I'll hopefully be in a position to share some more pics.

I never did get a clear answer as to whether the gold color on the underside of the lids were actually gold - someone mentioned a sulfuric bath for those. Can anyone comment on whether this is the correct approach for that and whether it is definitely gold?. I believe btw, following a bit more research that the lids are copper covered with nickle.

Russell

Get you a wood chisel to that you can place between the copper lid and the fiberglass and tap down on it with a hammer and most of the lids will pop off easily, some you might need to turn over 180 degrees and hit from the other side as well.

If you are going to run the copper tops in a sulphuric cell to deplate the gold from the lid you will want to soak them in 15% HCL solution till the nickle plating comes off ( Depends on how many you have and how hot your solution is for how fast the plating comes off). Then wash the lids with water and let them dry or heat them up to dry them. Then you will be ok to run them in a sulphuric cell to deplate the gold from the lid.

If you try to deplate them with the nickle plating still on them in a sulphuric cell it will cause you to have a mess on your hands that you would rather not deal with.
 
Half of the gold on the heat spreader have been dissolved by the indium solder that connects the die to the heat spreader. This gold will come down as a slowly settling sediment in the HCl bath. Collect any solid leftovers and extract the gold from that too.

Göran
 
Goran, thanks for the comment on the lids. I am reading about the sulphuric bath method atm and will look to progress on this route when I've a better idea of the processes. Will do a little more research on the chips too, to see if I can get a BOM or similar in respect of their constituents.

In respect of the bases I've some progress and some stats to share.

I eventually split all the lids from the bases - see pic.

The bases totaled 180 and weighed 1239g. Each = 6.9g
The lids totaled 180 also (obviously) and weighed at 120 for 2906g (max of my scales). Therefore in total 4359g. Each = 24.2g.
In splitting them apart I lost a little debris but the total weight was in excess of the 5kg I purchased by some way (5.6kg) so I got a few freebies in the batch.

On to the AP solution.
I washed the bases in water a few times to remove debris and gave each one a wipe to remove some of the grey paste that was stuck/smeared on most of them.
I worked out I'd need 1.1 litres of solution to cover them in my bucket.
I worked on a 3:1 ratio of 30% HCL to 3% H2O2.
However I only had 36% HCL and 12% H2O2.
Working backwards and adding water to dilute. I ended up with the following:

................Total ml....HCL 36%.....H202 12%.....H2O
.....................864 ........720.......................144
.....................288......................72...........216

Total ml..........1152........720.........72...........360

As you'll see this comes to a total ml of 1152, just more than I needed to cover and used up all the HCL I had. - perfect.

Pictures in reverse order.
Pic of 180 lids and bases duly separated (hammer and chisel worked just fine - became quite a pro at this towards the end.)

Measured quantities of chemicals - note the H2O2 on the left freely bubbling off O2 (wonder whether the concentration was really 12% after quite a bit of bubbling off over the past few days).

Water addded, then HCL added, then H2O2 added in that order - this pic was taken 1 min after adding and agitating - already seeing a green color.

Lid on pot, in sun will leave it outside agitating every day - from reading I'll need to be patient with this bit.

Note on safety in buying 12% H2O2 - the plastic 1g container is air tight - the H2O2 gives off O2 and slowly expands the container. This happened to mine and after a while the pressure built up so much that the container failed - fortunately with only a pinprick hole - this proceeded to shoot H2O2 about three yards across my garage - fortunately I saw (or rather heard - as the garage floor started to fizz and bubble) this before it had dumped the whole thing on the floor. I've now loosened the top on the plastic container so that it isn't quite airtight and enclosed in another bucket. My advice is NOT to buy this at this concentration if you only need 3% solution.

Russell
 

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Looks like you are on a mission here! I look forward to seeing your progress. 8)

I would suggest that you try and take care in protecting your nice glass table and pretty tile flooring
as chemical spills will occur and will greatly effect their current beauty. :shock:
 
This is a picture of the bases in the solution 2 hours after first adding. Color is a lot darker - I can already see some of the gold dots floating around in the liquid (quite a lot more than you can see in the pic). Much sooner than I'd thought. Weather is warm and bucket has been in bright sunlight.

Man those dots are small. At about 1000 per chip there is going to be 180k of them floating around in that liquid eventually. Still can't see that amounting to a lot of gold though!!

Russell
 

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rjamjb said:
This is a picture of the bases in the solution 2 hours after first adding. Color is a lot darker - I can already see some of the gold dots floating around in the liquid (quite a lot more than you can see in the pic). Much sooner than I'd thought. Weather is warm and bucket has been in bright sunlight.

Man those dots are small. At about 1000 per chip there is going to be 180k of them floating around in that liquid eventually. Still can't see that amounting to a lot of gold though!!

Russell

For that batch it will not be a lot of gold.
 
Latest update.

Well, having been away for a week and a bit I come back to the AP solution.

The color has turned to a very very dark green brown and not so many of the gold spots have come off the chips as I had hoped. It appears very clearly IMHO that the solution has become saturated with Cu and therefore the dissolving reaction of the Copper under the gold spots has slowed significantly.

So, I have two choices - add a good quantity more H2O2 to get the reaction kicking again, or use a bubbler. I am aware that too much concentrate of H2O2 with the HCL will actually dissolve the gold so will not go down the first route.

I have therefore adapted a fish tank air bubbler and am now bubbling air through the solution with the hope/expectation that the small amounts of O2 passing through the solution will keep the copper dissolving.

Will post a pic of the very dark solution in next post.

Oh, a lot of debris has also come off the chips from what I can see - will need to look at separation of that debris from the gold spots in due course.

Russell
 
Hello,

Just an update as it has been a week or so and a request for a bit of advice that I'm on the right track.
I kept the AP with the chips in it for about 8 days outside and gave it a daily mix up. After about 5 days the liquid had turned a very very deep brown (I guess very deep green but it looks brown). About a 1/3 of the gold dots had come off and I think that the mixture had become saturated (with Copper Chloride?) and so the rate that the dots were dropping off had almost ceased.

I did two things.

1. Added about 400mil more HCL 36%. This was on the basis that there would be more capability for the solution to dissolve more copper.

this worked for a while (couple of days), a few more dots dropped off then the rate of dropping stalled again.

2. I put in an air bubbler - this was from a very cheap aquatic fish tank bubbler and there are not a huge amount of bubbles perculating through the liquid. But there are some.

I've now had the bubbler working for about five more days and now about 2/3 of the dots have come off the chips.

Does this seem right in terms of time?. I guess I've just got to have patience, yes? I'm just letting the solution keep bubbling away at the moment.

Secondly, When I was putting in the bubbler I took the opportunity to filter off the debris/dots from the liquid as I transferred everything from one container to another. I then put through a plastic sieve to remove the larger pieces of debris and collected all the dots and small particles. I washed this through with water a couple of times. Then with HCL only a couple of times, then with water again. I then used a magnet which managed to collect some magnetic debris -which with care I was able to separate out and throw away. With the small sample I have I notice three things. First the dots that have come off (excellent !!! Yay). Secondly some dark blackish debris - which I think are parts of the chips that cracked/separated when I broke the chips apart and thirdly a whitish/milky coloured/cloudy particulate in the water. I think that this is a tin based salt precipitated out of the HCL (yes?) (if so then SnCl would be the salt, yes?).

Any comments on my observations so far? Am I on the right track?

I'll keep the posts up - and I'll post a pic of the extracted materials so far so you can see the mix of dots/milky cloudiness/dark matter shortly.

Appreciate the feedback.
 
CuCl is brown, CuCl2 is green. Too much brown in the solution means that there is no free oxygen to oxidize the CuCl into CuCl2. A bubbler was a good choice to add oxygen.
If there is a white precipitate it could be excess CuCl that don't dissolve. It can be because there is too little HCl in solution, CuCl is sparsely soluble in water but dissolves easily in HCl. The white solids you see could also be tin hydroxides and does not dissolve when HCl is added. So if it dissolves when adding HCL it was CuCl.

Many foils can cling to the board even when the copper is dissolved, shaking the boards or brushing them will knock the gold off.

By the way, if you see a mistake in an old post you can edit it yourself. I added the missing line and deleted your second post.
It's against the rules to do major editing to your posts as it disturbs the thread, but smaller edits like corrections and adding missing information is okay.

Göran
 
In the past couple of years I have found that a good air supply helps with agitation as well as adding oxygen. The agitation supplied by a larger air pump helps shake loose some foils that appear to still be attached. I still use aquarium pumps quite a bit, but in my larger copper II chloride tank, I am running a jet type nebulizer to help with the extra agitation.
 
DSC_0468.JPGAnother update.

Well had a bit of success with a toothbrush!!. Ran it across the surface of the chips and all those gold dots just came off easy as pie. So worked my way through all 180 of them and separated out. I washed off the gold dots into another bucket. Then filtered the AP solution and washed those filtrates into another bucket. An observation: The AP solution was definitely brown so was CuCl.

A couple of pics to show progress to date.

First is the pile of washed off chips - Question - is there any value left in that pile or are they exhausted and can be thrown away? You can see one of my used filtration papers, I've been keeping these as I would intend,once I've enough, to incinerate to recover Au residues not washed off the papers.

Second a small amount of the filtered solution. This was what I had already washed with HCL and water. The liquid you can see is just water - it has a very faint chlorine smell. You can clearly see gold and other debris. I intend to get the rest of the solution washed and into this state before next steps. You can also see the milky substance in their - I think that this is SnCl(2?) and have mentioned this before it is not dissolving in the water.

Third the two buckets - brown one was the AP, now CuCl. I filtered this and, based on other comments here put the solution back in a plastic bottle and labelled. Questions: I can use this again on my next batch yes? I'd heard of someone putting a piece of stainless steel in there which would draw the copper back out of the solution (so that it would be better to use on the next batch as it wouldn't be so saturated with copper?. Is that a good approach? If not how best to store? The second bucket contains the water washed off the chips while I de-golded them!!


Finally my next steps - will wait for comment prior to executing...


  • First will filter through some fine mesh to get rid of some of the bigger pieces of debris.

    Second use a magnet to remove any iron/ferric materials.

    Third move to AR and dissolve the gold?. My concern here is the amount of debris still mixed with the gold and the AR will also dissolve some of that. Any ideas on further processing before I move to AR.

Thanks for your inputs.

Russell

Just a little update - have been (with water) filtering/washing/filtering washing etc today. I have diminished all the liquid and its filtrate down to gold dots and a light brown muddy substance - will post a pic in due course (as always). Have now put a 36% of HCL on top and will steep for a day or two, to take out any residual metals that are not gold ( I hope).
 

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Hi,

Another update. Another puzzle.

So I had taken all of the gold off the chip bases with the AP method. Since then I've steeped the gold and debris in 400ml of conc (36%) HCL for a couple of days. Used a magnet to take out all magnetic pieces left in the HCL another day. Then filtered out from the HCL. Then sieved a couple of times to take out larger pieces of debris. Now I have washed/filtered/washed/filtered in water three times (even now a very faint smell of Chlorine lingers - but i would guess very very very small amount of HCL left given the amount of H2O washing I've done).

But.....

What I have left is a mix. Clearly from inspection, some very small pieces of glass/silica but also, a very very fine 'dark grey' muddy substance that the gold is mixed up with. See Picture to demonstrate.

I can't see a way to separate the gold physically so...

I think that this might be just very fine organic/fiber board/silica mix so I think I can move to AR directly. Unless I know what that mix is however, this could cause problems - I'd dread to think about the mess I'd have if the whole lot dissolved in the AR.

I'd really appreciate suggestions at this point before I commit to the AR.

Thanks a lot

Russell

ps Göran - thanks for the tip on the colour difference between the HCL/Cu chemical mix types - I'm quite clear on that now (or dark brown if you take the liquid colour into account lol!!!)
 

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Russel, don't over think it. You're still in the recovery phase. It's looking good, and you're ready to dissolve that which will dissolve, and precipitate your gold. You will almost always have some "junk" in what you dissolve in your first refine, especially when you're first starting out. Don't worry about it. Some of it will dissolve along with your gold. The precipitants we use (copperas, SMB, etc.) are somewhat "selective". They precipitate what we want to precipitate, and leave most of the other junk still in solution.

Once your gold is precipitated, wash it well, following one of the several methods documented here on the forum. If you want to clean it up more, dissolve it again, and drop it a second time.

Dave
 
FrugalRefiner said:
Russel, don't over think it. You're still in the recovery phase. It's looking good, and you're ready to dissolve that which will dissolve, and precipitate your gold. You will almost always have some "junk" in what you dissolve in your first refine, especially when you're first starting out. Don't worry about it. Some of it will dissolve along with your gold. The precipitants we use (copperas, SMB, etc.) are somewhat "selective". They precipitate what we want to precipitate, and leave most of the other junk still in solution.

Once your gold is precipitated, wash it well, following one of the several methods documented here on the forum. If you want to clean it up more, dissolve it again, and drop it a second time.

Dave


It just could not be explained better than that. The thing to remember is.
You're still in the recovery phase.
I look at this way, get my gold first (the recovery stage) then worry about improving on the purity, (the refining stage). Quite often I will save recovered powders from various recoveries then refine and melt. It makes for a bigger button, :)
 
Great result,

I mixed up 200ml of 36% HCL and 50ml of 70%HNO3 i.e. Aqua Regia, and slowly poured it over the results from the AP (see last picture). I was expecting some bubbling and heat but at first nothing happened (probably because the original precipitation was still quite wet with H2O from previous cleaning. I was thinking that I might have to heat it up, which would cause me a problem because I've got no heat source I could use outside at the moement. I then stirred a while and gradually the gold dissolved. I've left the solution a while and can see quite a bit of the debris has dissolved too.

Leaving for a couple of hours I returned and the mixture had cleared and is a beautiful golden yellow color with some settled debris at the bottom - looks just like the color I've seen in any of the numerous videos on this topic. Will post a pic tomorrow as always.

One point about this phase - that AR really really does fume. I've left the mix outside covered with a plastic bucket so its not concentrating anywhere but in the dark with a torch you can really see the fumes coming out of that mix. Advice to anyone - never mix this inside without suitable extraction - there is no way you could be safe with this in a contained room/garage/shed etc without such precautions - Hoke mentions a heating method with a cover sitting in a bath of water (so fumes bubble through the h2o)- but that is too complicated for my set up at the moment.

Am going to leave over night before filtering and then moving to precipitation but.... I really am delighted with the result of this phase.

Many thanks to Dave and Shark for recommending I go ahead with the AR as I was nervous about making a mess at this stage. Still got some work to do and that brings me to my next question.

So. I have some Sodium Metabisulphate. Based on a few posts mentioning this here this seems to be ok, but,,, Hoke uses Copperas as the precipitant chemical. She says that there are a few trace chemicals that will be brought down with the gold (also precipitated) that can be dealt with (and I can follow her method for this) but.... what about SMB.... does anyone have an analysis of whether the same trace chemicals get brought down with the gold when that is used?? Any other comments on Copperas vs SMB.

Thanks for everyone's inputs so far - you are a great bunch. I'm learning loads, very quickly.

Russell
 

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