Simplified Refining Instructions

[Harold_V]

Hi Harold
Thanks for you help
This polishing dirt that I have with a mixture of sand paper and some other things from jewelers bench
I have been boiling this thing for about 4 or 5 times and the liquid is still green.
How many times does it normally take to have it so that the green is gone in the liquid
Thanks

When I processed such material, after incineration and proper screening, to remove large particles that may not dissolve without difficulty, I then literally boiled the material in HCl. I'd use a rough balance of water and HCl, covering the material with a generous amount extra. You couldn't generally tell if there was still anything being dissolved, but I'd boil the material for at least 15 minutes. When I removed the vessel from heat, I'd fill with tap water, stir well, then allow the solids to settle. That could take minutes, or hours. Once settled, I'd rinse with tap water, stirring well once again, then allowing the material to settle once again. My experience dictated that a couple rinses with tap water were generally enough to lower the contained base metals that were in solution.

I would then go to AR to dissolve the values. It was my experience that there was generally little to no base metal remaining, proven by the nice yellow solution that came from the values. Gold precipitated from this process tends towards being very clean, especially when compared to gold that comes from processing dirty filings directly, without inquartation.

I do not recall ever having to go back for further processing this kind of material---one hard boil and proper rinsing appeared to be sufficient.

Harold

 

[golddie]

Hi Harold
Thanks for your help
So far I am just using hcl and water and its my first time so I am doing it slowly until I get the hang of it.
I have watched steves video on siphoning and I tried that and I couldnt do it
I have to get used to siphoning

 

[gotthebug2]

goddie;
Place some mud in a beaker with water to practice on, much cheaper than PM's, another handy thing for me is to use a plastic clothes pin to hold the hose in place while starting with the syringe.

 

[lazersteve]

Siphoning can be as easy as filling a tube with water and lowering one end into the solution while covering the other end to keep the water from flowing out.

Once the opposite end is in the source container under the solution level, lower the end you have your finger over and release into the catch bucket to begin the siphoning action. The bottom of the source container should be elevated above the top level of the catch container.

Steve

 

[Oz]

Oh my goodness, I just had a terrible thought. I certainly hope that given the difficulties suggested in “siphoning”, that someone was not trying to siphon acids like some do gasoline by sucking on the end of a hose.

 

[golddie]

This batch of dirt that I have was boiled in HCL for about 5 times and today I poured it all in a funnel with a filter.
I have no experience in this but to me it looks like silver
If it is dry than tomorrow I will incenerate it again
and more HCL and water boil
Am I overdoing things
Should I test it with solution A or should I just do nitric and water half half
I was going to use AR but I am not sure about that

 

[Barren Realms 007]

If you truely boil it in HCL you have the chance of dissloving some if any of your gold.

 

[Harold_V]

If it is dry than tomorrow I will incenerate it again and more HCL and water boil
Am I overdoing things

Yes, you are, and it makes no sense. If your purpose is to apply more HCl, filtration and drying is a worthless process. The only exception would be if you feel you could eliminate something by incineration. If you did your work properly before the first digest, there should be nothing to eliminate, for you would have incinerated fully then. If your next move would be to go to nitric, incineration is required. If your next move would be to go to AR, it's a wasted step.

The only way you'll get a feel for what you're doing is by proceeding to the next step. If you find you left base metals behind, you'll know that you need to do more for future batches. If you overdo and think that's the necessary amount, you'll then overdue everything in the future. Make a mistake or two along the way, but understand what the mistake is, and how to correct for the future. That's how you learn.

By the way, you said you think there's silver present. If there is, and it's the main value, you should have avoided the HCl process, and gone directly to a nitric digest. It would be very helpful if you could describe the source of your material, and what it looks like now. Tonight I don't think you have any gold present, otherwise you wouldn't be talking about silver. Color in this material is very telling. What color is the material now?

Should I test it with solution A or should I just do nitric and water half half

You should test with solution A (stannous chloride) at all turns, especially when you're new to refining, and especially when you are working with unknown materials. That way if you happen to dissolve some values, they can be recovered. If you discard solutions without testing, you won't know if they should be discarded, or not.

I was going to use AR but I am not sure about that

Neither am I, now. You must be more forthcoming of information, or tough it out alone. The choice is yours. None of us can read your mind, nor can we see what you have in your vessels unless you post a picture. That is usually very helpful.

A little friendly advice. Using punctuation is very helpful in allowing readers to better understand what you're trying to say. Please do not run all your sentences together. If nothing else, please use a period where appropriate.

Harold

 

[golddie]

Hi Harold
How are you
I appreciate your help very much.
I did diamond setting and made some silver jewelery and this batch is from that and this was a while ago so I don't remember what I have in here but it looks like silver mud maybe I am wrong but gold mud would look yellow and here I don't see any yellow

I also boiled this thing for so long that maybe the gold went into the solution like Barren was saying
but it is a good thing I still have the waste liquid I will have to check with solution A

My sentences look like a mess I need to have a crash course on writing and grammar

In all the entire amount is not very much I am not able to tell how many grams I am thinking of spiting this batch in half and make one part hcl/water and the second part nitric/water

Or I might wait for a camera and get an opinion based on your judgment from what you see in the picture

Thanks again

 

[golddie]

I am experimenting with 3 different batches of similar dirt and I will number each batch and describe each a bit
Batch 1
This is a mixture of polishing dirt and sandpaper dirt(mixture of gold and silver)
This is the batch I have been asking about till now
I have not done any new work on this today it is just filtered and I might split it in 2 and do half with nitric and water
and the other with AR

Batch 5
This is silver bench filings
I started this today and I used nitric and water half half
I got a green solution with some residue in the bottom of the beaker what should I do with it
According to the notes I should decant and add more water and nitric to the residue in the bottom
Than collect all the nitric and process it with salt or sugar(I will get to that later in more detail)


Batch 3
This is silver polishing dirt
I started this today and like batch 5 there is a residue in the bottom of the coffee pot and the liquid is
reddish.
Should I decant and add more water and nitric to the residue in the bottom
Than collect all the nitric and process it with salt or sugar(I will get to that later in more detail)

For batch 3 and 5 I am only processing a small amount something like 4 tablespoons of dirt and fill
Thanks

 

[golddie]

Right now I have batch 3 and batch 5
I am wondering why the liquids have color in them one is red and the other is green
Did I do something wrong with the boiling part this time I only boiled about 15 minutes

 

[Harold_V]

Hi Harold
How are you
I appreciate your help very much.
I did diamond setting and made some silver jewelery and this batch is from that and this was a while ago so I don't remember what I have in here but it looks like silver mud maybe I am wrong but gold mud would look yellow and here I don't see any yellow

That's not necessarily true. If you're dealing with mud, material that comes from incinerating filters, polishing wastes, maybe even floor sweeps, there's little reason for you to expect the color to be yellow, and it rarely is. What you can expect, assuming there's been polishing included, is for the color to be purple. Finely divided gold isn't yellow, it displays purple.

I think it's time for you to determine what you're really working with. Are you working with filings, or are you working with the things I mentioned, above? You would handle filings in a different fashion. Lets clear the air on that issue before I comment any further.

also boiled this thing for so long that maybe the gold went into the solution like Barren was saying
but it is a good thing I still have the waste liquid I will have to check with solution A

That's correct. You should ALWAYS test solutions, for you never know when there is some chemical involved that can result in the dissolution of values. It's not likely, but it's not impossible. Wise people always test, even when they *think* they know a solution is barren.

My sentences look like a mess I need to have a crash course on writing and grammar

What you have done in this one helps, but a period at the end of a statement tells the reader that you have finished that thought. Otherwise one doesn't know if you're through talking, or the next line is part of your comment. Please start using periods if you do nothing else.

In all the entire amount is not very much I am not able to tell how many grams I am thinking of spiting this batch in half and make one part hcl/water and the second part nitric/water

That's one way to gain an understanding. If you're working with a small batch, it won't require much effort. Remember---if you go from HCl to nitric, you should incinerate until you've heated the material quite hot--hot enough to burn anything carbonaceous. By doing so, you'll insure that you have eliminated all of the HCl, lowering the risk of dissolving values prematurely.

Again, are you trying to process filings? If so, did you combine them with anything else?

Harold

 

[golddie]

Hi Harold
The batch where I am processing silver polishing dirt and what I did was boil in nitric and water half half.I got a reddish color in the nitric.I wanted to know how many minutes should I have boiled this thing I did about 15 minutes is that good or should it be for longer time like 1 hour. Also once I do I siphon the liquid or do I filter and than I guess I will have to start the cementation process
Thanks

 

[golddie]

silver polishing dirt and what I did was boil in nitric and water half half

I did this yesterday and I am now watching videos on making silver nitrate and here silver crystals grow in the solution after a while.
When I go to my shop I hope I that does not happen because I didn't separate the dirt from the liquid

 

[Harold_V]

Hi Harold
The batch where I am processing silver polishing dirt and what I did was boil in nitric and water half half.I got a reddish color in the nitric.I wanted to know how many minutes should I have boiled this thing I did about 15 minutes is that good or should it be for longer time like 1 hour. Also once I do I siphon the liquid or do I filter and than I guess I will have to start the cementation process
Thanks

There is no real way to determine if you have boiled long enough, although the addition of a little more nitric should make no difference. What that means is if you have already dissolved all the silver (which happens fast), when you add more nitric (an ounce for a liter of material is more than enough) and you don't get any more brown fumes, you can safely assume that you have.

When you are confident you have dissolved all of the silver, you should then add water to the vessel, and stir well. That will dilute the solution, which, in turn, will prevent the formation of the silver nitrate crystals you have described. If they persist, use more water. I always used tap water, not caring if I created a little silver chloride, because all of my waste was further processed. If you prefer to not create any silver chloride, use distilled or deionized water. Stir well, allow to settle, then siphon the solution. Repeat with more water, until you get no reaction when testing the solution with a drop of HCl (test a sample, do not drop HCl in the solution). I suggest you filter only the solids, after you have siphoned off the bulk of the rinse solution. If you use an S&S Sharkskin, it's tough and will retain the processed dirt, yet allow fast filtration. If you try to filter the first solution, chances are VERY good it won't filter worth a damn. Do use a hose and siphon unless you have a lot of time to waste.

The reddish color you speak of is likely the result of dissolving Tripoli, which is iron oxide. That is to be expected, and it's not much of a problem. Do test the solution with stannous chloride, however, in case some gold is present and has been dissolved. Stranger things have been known to happen.

Unless you are absolutely certain that this material does NOT contain gold, once you have rinsed out the silver, you would then go after any remaining values using AR. If you suspect that gold is present, I highly recommend you incinerate, then screen, then do an HCl wash before attempting to dissolve further values. That will insure that the solution will filter properly. Not following this process can result in a solution that refuses to filter.

In the end, in spite of your best efforts, the material will not be barren of values. I suggest you incinerate to expel traces of acids, then store them. If you accumulate enough of this type of waste, it can be submitted to a major refiner for further recovery, or it can be processed in a furnace. It's almost always worth the trouble, and can be the source of a nice sum of money.

Harold

 

[golddie]

Hi Harold
I have a few experiments going on so that we don't have a mix up I will concentrate on the 2 batches that are very similar.
Batch 5
This is silver bench filings

Batch 3
This is silver polishing dirt


http://goldrefiningforum.com/phpBB3/viewtopic.php?f=50&t=4767&hilit=Silver+Powder+in+Nitric+Acid&start=20


All the residue went to the bottom because I left it overnight, the red from the Tripoli went to the bottom
also both solutions looked similar I was able to siphon successfully and I was tempted to mix them together and good thing I didn't because looks can be deceiving.
For one thing yield form batch from the silver polishing dirt looked less than the other and also after a few hour
of copper in this solution the color was different than the other.
I have left some copper in the 2 bathes so it stay there over the weekend

On this page There is a green solution and the result from my 2 batches were very close to looking like that
before I placed in the copper pieces.Sorry for not being able to supply pictures this time around.

I appreciate your help.

 

[Oz]

Hi Harold
I have a few experiments going on so that we don't have a mix up I will concentrate on the 2 batches that are very similar.
Batch 5
This is silver fillings

Batch 3
This is silver polishing dirt

Golddie,

I am assuming this is once again a misspelling and you are not processing “fillings” but meant to say silver filings. Please check and correct your posts for this error, and be very careful about this in the future. I understand “you” know the difference, but we cannot afford to have an error like that on the forum. Someone new may read what you write and think it is ok to put dental fillings in nitric. It is not, and could result in mercury poisoning!

 

[golddie]

Hi Oz
You are right about that
I think if I write in capital letters it will be easier to see
I am talking about FILINGS from a jewelers bench
and FILLINGS are from dentists and most likely contain mercury
Thanks

 

[Harold_V]

I was able to siphon successfully and I was tempted to mix them together and good thing I didn't because looks can be deceiving.

So long as you are not trying to determine the yield from each batch, mixing them together is acceptable.

For one thing yield form batch from the silver polishing dirt looked less than the other and also after a few hour
of copper in this solution the color was different than the other.

My guess would be that the solution from the filings was blue, whereas the solution from the polishing waste was likely green. That's to be expected, due to the iron dissolved in the polishing waste. I could also be wrong, for if filings had iron included, it's possible they would be discolored darker yet. I had a policy of using a magnet after incineration and screening, to remove as much iron as I could. It always carries traces of values, so it was sent to my stock pot, where they are eventually recovered.

I have left some copper in the 2 bathes so it stay there over the weekend

You should take a look at the operation and insure that the silver isn't creating a hard coating. If it is, you'll have to strip the surface, otherwise it can cease to cement. That's not a common occurrence type of thing, and is less likely to happen when you are working with dilute solutions. Remember to stir the entire lot at some point in time. Cement silver that is first deposited can drag down silver nitrate that won't get cemented. By stirring vigorously, it is liberated and eventually cemented. I used to do that with a gloved hand.

Test the solution with stannous chloride as the silver concentration is depleted. If there's any platinum or palladium present, it will be slow to cement. It usually comes down after the silver.

When you think all of the silver is down, take a small sample of the remaining solution, and add a drop of HCl. If you get no cloudiness, the silver is down. If you do, allow the solution to remain on copper longer.

Harold

 

[golddie]

Hi Harold
When I placed a piece of copper in the batch of the liquid from the polishing dirt there was lot of fizzing I guess that is normal.
I think you said don't use copper wires but I said I will try it in the beginning phase of the operation since the fizzing was so fast that I would have to worry about silver getting in between the wires,I still have not looked at this thing closely I will do that Monday.I placed the copper piece in the jar of liquid with those plastic things for tightening electrical wires together
When I took a quick look on Friday I noticed that one part disappeared is that normal

http://www.google.com/imgres?imgurl=http://www.sitesplus.co.uk/user_docs/638/Image/Black%2520Cable%2520Ties%2520edited.jpg&imgrefurl=http://www.toolsandhardwaredirect.co.uk/catalogue.php%3Fcat%3D505%26subCat%3D1163%26item_id%3D6108&usg=__P1r-gH6o6M9PMrXGWY6MrfHswbc=&h=426&w=640&sz=21&hl=en&start=15&zoom=1&tbnid=Be29niu5LB2-1M:&tbnh=108&tbnw=163&ei=oKVOTb3jFcWqlAeelezrBA&prev=/images%3Fq%3Delectrical%2Btightening%2Bplastics%26hl%3Den%26biw%3D1024%26bih%3D578%26gbv%3D2%26tbs%3Disch:10%2C464&itbs=1&iact=rc&dur=266&oei=m6VOTZylN4SclgeQ4eT3Dw&esq=2&page=2&ndsp=15&ved=1t:429,r:13,s:15&tx=97&ty=48&biw=1024&bih=578
Before melting the silver I am planning to wash it with hcl.
Thanks very much for your help