AMD Opteron 2212 for Noob

[g_axelsson]

You should use sulfite, not sulfate!

Göran

 

[Anonymous]

I don't understand why you used so much Nitric acid bearing in mind the amount of data on this forum that tells you otherwise?

You've used FAR too much.

 

[rjamjb]

Hi spaceships I used a 4:1 ratio which is what hoke, recommends. Other posts on here talk about a 3:1 ratio which is more than I am using. Can you help me with anything I'm missing.

Thanks Russell

 

[Anonymous]

Hi Russell

Thanks for the reply. Yes there are numerous posts and references on the forum to the amount of Nitric required to dissolve a gramme of gold and the recommendation not to use standard mixes for many types of refining/recovery. The best kind of searches to find this information are ones relating to denoxing AR solutions, excess Nitric, and related topics because this is where a lot of the information has been shared.

Effectively what's being said is that as an improvement to Hoke's ratio procedure, using as little Nitric as possible will make the denox process simpler, quicker, and use much less material.

In a nutshell if you use 50ml of 70% Nitric to dissolve 5g of gold you could be looking at having to neutralise up to 45ml of that Nitric in order to drop your gold. Warm HCl with the Nitric dripped in in smaller batches as required until the gold has been dissolved can provide far more efficient results.

I hope that helps in your journey.

Jon

 

[rjamjb]

Thanks both:

Göran, I made an error in my typing - it is Sodium Metabisulphite that I have.

Jon, Definitely a lesson learned. So, for next time, I'd cover in HCL and drop Nitric into it a few mils at a time until no more gold dissolves then add small amounts of additional nitric (and possibly hcl) until everything dissolved. This will definitely save on Nitric which is quite hard to come by at the moment.

Russell

 

[g_axelsson]

Thanks both:

Göran, I made an error in my typing - it is Sodium Metabisulphite that I have.

Jon, Definitely a lesson learned. So, for next time, I'd cover in HCL and drop Nitric into it a few mils at a time until no more gold dissolves then add small amounts of additional nitric (and possibly hcl) until everything dissolved. This will definitely save on Nitric which is quite hard to come by at the moment.

Russell

That is the good stuff! 8)

Now you might understand why we are so hard on spelling on this forum. Preview is also a good tip for everyone as there are a lot of stupid errors that is caught in preview, for example cutting off the code when citing another post, seen that today already in another thread.

As for dissolving gold, when I did my largest refining of 53 grams of gold I started by measuring up 1 ml nitric acid per gram of gold I had, then adding only half of it as a start. It dissolved most of my gold and I only needed to add a few ml to get the last part. In the end I used 28 ml nitric for dissolving 53g gold. The rest I could save for another time.

But don't feel too bad, it's one of the most common newbie mistakes. We have all overdosed the nitric acid and had to deal with it.

Never premix aqua regia, it will break down by itself and emit gases. If stored in a closed container it will build up pressure and the container might burst.

Göran

 

[Shark]

Since you know you have to much nitric you will need to deal with that first. You can (1) heat your solution until it is used up, (2) use sulfamic acid to neutralize the nitric or (3) add more gold until the nitric is used up. There may be other ways, but those are the one's I know and use. If you heat it, don't boil it, I try to get mine about hot as a good cup of coffee and keep it there until the nitric is depleted. ( I actually use the bottom half of a coffee pot for this)

For precipitation, Sodium Metabisulfite or copperas will work, I prefer coppera's, for dirty solutions, but they need to be prepared 24 hours ahead of time in my opinion, before being used. Which ever one you use try not to over use it, this will lead to even more contaminants dropping than if you only use enough to get the job done.

 

[upcyclist]

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.

Hehe, another language moment. I felt an instinctive "What?!? Open flame in a room obviously full of fumes?!?" until I remembered: oh yeah, he's a Brit. That's 'flashlight' in American English

Nice work, btw!

 

[MarcoP]

For precipitation, Sodium Metabisulfite or copperas will work, I prefer coppera's, for dirty solutions, but they need to be prepared 24 hours ahead of time in my opinion, before being used.

This is the first time I read that SMB or copperas needs to be made a day before, could you please explain why you are of this opinion?
I know copperas will need to be filtered, so you are probably letting the solution settle and then filter from decanting, but what about SMB (which I prefer to use it dry anyway, at least after my acquaintance tests).

Thanks
Marco

 

[Shark]

Coppera's need time, I use SMB dry as well. A bit of grammatical error in the original post.

 

[rjamjb]

Hi all – very frustrating, I’d posted this and for some reason didn’t lodge in the system when I hit submit. Probably will miss something out on this second attempt (which bye the way I’m writing in word and then cut/pasting into the forum).

So main reason for posting is to give an update, and a couple of pics, on my previous phases and then to enquire into my next phase of refining. (Recovery/Refining = very different which I now know).


Three main pics – first showing one beaker is the first filtration of the AR. This is what I’d been so delighted about – glorious orange/red colour.



Second is the picture of a paler yellow filtration which is what I’d got from washing out the filter and original beaker with some H2O. I added this to the first beaker’s filtration in the end and now have a glorious orange (hopefully) Chloroauric acid – albeit with excess Nitric acid as has been pointed out.

Third is a picture of the filter from the very final filtration. As you can see this is slightly yellow coloured and I suspect has traces of the Chloroauric acid in it. So am drying this out at the moment and will look to adding to a recycling mix at some point in the future.

So Göran I did only mix what I thought I needed (albeit with a bit more nitric than necessary, lesson learned as I mentioned before. I will save some Nitric following this, which is hard to come bye at the moment.


Shark, also I’ve never come across the Sulfamic acid method before, I’ll do a bit more research on this. My main problem at the moment is that I have no ability to easily heat solutions to reduce. I have an old unused coffee machine that I could probably adapt so will look into that (might be good in that the temperature will not be too high). But I have three possibilities SMB, Copperas, and your Sulfamic acid method. Will investigate all three.

Before I move to the next phase I’ll post my recipie/solution here for comment.

Another slightly unrelated point = I’ve various residue liquids from this whole process which I’ve kept. I think that I can resuse some/all (eg CuCl liquid) so will post a pic and update of those before I finish to get some further feedback. As a result I’ll be able to fairly accurately be able to publish overall cost/usage statistics to compare with the final gold refinement.

I am going to wait until I have some stannous crystals (ordered today) so I can test the various solutions, hopefully mid-week until I commit to my next steps.

Upcyclist – try to use colour as color on here as a Brit – I get corrected every time but, no way would I have got flashlight vs torch as a correction lol. Rest assured, as soon as I saw the fumes, everything was moved outside. (My trusty upturned plastic bucket has proved most valuable)

A couple more follow ups to come

Hopefully I've not missed anything

Russell

 

[Shark]

I still haven't found the post I wanted, but here is one that explains it almost the same.

http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=48&t=14026&start=20#p192509

I prepare mine by adding the water, and stir thoroughly.
Filter well, twice.
Add hydrochloric, mix well.
Allow to settle 24 hours.
Decant the clear fluid without disturbing the settled contaminants.

Hoke puts it this way. Extended for the OP's sake.

(6) RECOVERING THE DISSOLVED GOLD WITH COPPERAS
If possible, have the solution in a transparent vessel a glass jar,
beaker, or pitcher. If it is transparent you can see what goes on and
understand the process better. Later, when you handle large quan
tities, you will carry out this process in a chemical stoneware crock,
but while learning the processes, use transparent vessels whenever
possible.
In another vessel, dissolve in warm water about a pound of green
copperas for each 50 pennyweight of fine gold that you expect to
recover. Use fresh green copperas, with about a quart of water to a
pound. Add a little hydrochloric acid, enough to make the copperas
solution a clear green.
Pour the copperas solution slowly into the gold solution, and stir.
Metallic gold will appear as a dark cloud. Let this settle some hours,
or overnight, and you should find your gold in the bottom of the
dish, as a heavy brown powder.
Sometimes an impatient worker will cut short the evaporation described
in Section 5, and will fail to remove all the excess nitric acid. When this
has happened, bubbles will arise on the addition of the copperas to the
gold solution, sometimes so freely as to make the mixture boil over. So
add the copperas slowly at first. These bubbles are the same brown
fumes that you notice when nitric acid interacts with anything. In this
case the nitric acid is reacting with the copperas. Gold will not come
down until all the nitric acid has been disposed of. The solution will turn
dark, but no gold will precipitate. When this happens you must do
one of two things to get rid of this nitric acid.
One way is to add an extra quantity of copperas and hot water, stirring
constantly. Keep on adding copperas until the mixture stops fuming and
the gold comes down. Before trying this method, however, take out
about on ounce of the solution and get a rough idea of how much copperas
is needed. The other way to get rid of nitric acid is to evaporate
the whole solution down to a syrup again, and again add hydrochloric
acid, as in Section 5.

Edit for spelling

 

[Anonymous]

Stannous Chloride- - - HCl with some tinned solder thrown in it and left in a dropper bottle. Countless threads on here about that Russ.

Pop to B and Q or similar and buy the lead free tin based solver- - often on a blue reel.

Also check your PMs- I sent you a message earlier today. 8)

Jon

 

[Anonymous]

Shark

Mixing Ferrous II Sulphate for dropping takes but a few mins mate. It doesn't need leaving overnight or filtering out twice if you are using good grade green crystals.

 

[Shark]

OK, then I retract my previous post and leave it to the experts.

 

[FrugalRefiner]

Hi all – very frustrating, I’d posted this and for some reason didn’t lodge in the system when I hit submit. Probably will miss something out on this second attempt (which bye the way I’m writing in word and then cut/pasting into the forum).

I used to have problems like that quite often when I was using the CA Gen2 board style, which is the default style. Since switching to subsilver2, it rarely happens, but it's still a good idea to work in a word processor when you're working on a long post. See Board Style, User Control Panel for more information.

Three main pics – first showing one beaker is the first filtration of the AR. This is what I’d been so delighted about – glorious orange/red colour.

Second is the picture of a paler yellow filtration which is what I’d got from washing out the filter and original beaker with some H2O. I added this to the first beaker’s filtration in the end and now have a glorious orange (hopefully) Chloroauric acid – albeit with excess Nitric acid as has been pointed out.

Third is a picture of the filter from the very final filtration. As you can see this is slightly yellow coloured and I suspect has traces of the Chloroauric acid in it. So am drying this out at the moment and will look to adding to a recycling mix at some point in the future.

I see the same picture three times.

But I have three possibilities SMB, Copperas, and your Sulfamic acid method. Will investigate all three.

Just to clarify, SMB and copperas are used to precipitate your gold. Sulfamic acid is used to destroy excess nitric acid prior to precipitating.

Common ways to destroy excess nitric (referred to as deNO_xing) include the classic evaporation method described by Hoke, using urea (which has fallen out of favor for a number of reasons, and is not recommended), adding a button of refined gold (described by Harold_V), and using sulfamic acid. The best method is to add the nitric in increments, adding only as much as is needed, as you've now learned.

If there is only a tiny amount of excess nitric, SMB and copperas will actually eliminate it. As you add a bit of either, they begin to reduce the dissolved gold to metallic gold. But as quickly as it happens, the nitric acts to reoxidize it and put it back in solution. Eventually, the nitric gets used up and the gold will precipitate, but with a large excess, by the time that happens you've added so much precipitant that you've contaminated the solution and may have other problems with the drop.

Hope some of that helps.

Dave

 

[rjamjb]

Thanks Dave, hopefully the pic duplication has now been resolved.

Definitely the best approach would be to use a button of gold, Harold's comments on this are great. Unfortunately I've not got a spare button as this is the first time I've gone through the whole process so won't have any 'spare' gold (eg in the form of a ring or similar that I can say would be good enough to do that task - as probably not that pure). (Obviously I won't have this problem next time as I 'Have Learned' the error of my ways). So....

Sulphamate - which I am going to read up on or - Evaporation - are my solutions from this point on. - and thanks for pointing out this is a method to reduce Nitric and not to precipitate, as I had missed that point - probably would have realized when I read up though.

Thanks for the tip on this.

Russell

ps realised should have an s and not a z !!!! (englo/americ translation lol)

 

[Anonymous]

Definitely the best approach would be to use a button of gold, Harold's comments on this are great. Unfortunately I've not got a spare button as this is the first time I've gone through the whole process so won't have any 'spare' gold (eg in the form of a ring or similar that I can say would be good enough to do that task - as probably not that pure). (Obviously I won't have this problem next time as I 'Have Learned' the error of my ways). So....


Russell

ps realised should have an s and not a z !!!! (englo/americ translation lol)

There is a lot of discussion about this. As Harold has openly said, the use of Sulphamic acid is an equally viable option. It simply wasn't available to him during his extensive refining career.

It's cheap, and readily available and easy to use. Using the example of your case here. Using a gold button with 45 cm3 of excess Nitric would be impractical, take forever, and use at least 45g of gold which you don't have. 8) 8)

 

[g_axelsson]

Nice color! Looks like quite pure gold chloride. Good work so far. 8)

In this case I recommend evaporation over sulfamic acid as there is so much nitric in excess here. Evaporation doesn't add any extra chemicals and allows you to work with more concentrated solutions. Using sulfamic acid turns the nitric acid into sulfuric acid and that will add to the volume of the solution.
Evaporation doesn't add to the volume, you are switching out nitric for hydrochloric acid.

A small amount of sulfuric acid is just good to have to precipitate any dissolved lead as lead sulfate but you have quite an amount of excess nitric here.

I got some links about sulfamic acid on the bottom of this page:
http://goldrefiningwiki.com/mediawiki/index.php/Sulfamic_acid

When you are doing your final filtration before precipitating the gold you should have the solution a bit diluted and chilled to keep silver chloride from dissolving. A concentrated gold chloride solution is actually able to dissolve some silver chloride. Dilution and chilling makes sure that the silver is caught in the final filtration.

Then the only danger you face is that it's quite addictive to drop the gold from solution.
You will know what I'm talking about after the first time!

Göran

 

[JHS]

Ever since I saw this on youtube chanel Cody's lab I was looking for a good place to post it.I do not have a link,but he was gold plating his bumper.
Cody used a water bottle,he fit the top with a tube and drilled a second hole to put hcl in the bottle.
He first put a amount of SMB in the bottle and then added a amount of HCL. He then put the tube in his beaker and bubbled the so2 gas that he was creating in the bottle.He did not say how much SMB or HCL he used,but I'm itching to try it.
john
P.S.I got the link and it's about half way through the video
https://www.youtube.com/watch?v=_PmJGOcBZQI