# Questions and verification guys.



## Aeon13 (May 19, 2016)

Good day to all!

In pursuit of learning more, I would like to ask some questions and may I let you verify things which I read here in the forum.

All that was stated here are my understanding from my reading here in the forum. Please correct any statement if its wrong.

I have silver nitrate from boiling my inquarted gold with 50/50 nitric/water. I used copper method to recover the silver.

My question is: _How would you guys dilute the silver 

nitrate?_ I read topics that states the need for dilution of silver nitrate but I was not able to see the percentage of water to add.I have read somewhere here that too

much dilution makes very fine silver powder and is not easy to filter.

Please verify: This silver nitrate from 50/50 nitric/water, after I submerged the copper. Brown fumes came out which from my reading is the reaction of free nitric 

acid with copper. From my reading also free nitric acid is needed for the cementation of silver but not too much. Too much free nitric will just dissolve cement silver 

back to silver nitrate. This means lots of copper would be used. I have a limited stock of copper and I would like to ask: _How do you reduce free nitric acid from the 

silver nitrate to maximize the use of copper? Is it in the dilution? _

If by chance I have no copper left. I have no option but to use salt and do the silver chloride method. Then add diluted sulfuric acid and iron to make it elemental silver. 

From reading, Copper will cement any gold that is mixed in the silver nitrate solution. _But what if I used salt and made silver chloride? Does this mean the gold mixed in 

the silver nitrate will not be recovered?_

The liquid from the recovery of silver using copper is copper nitrate. I have stated my problem with supply of copper and I would like to recover the copper metal from 

copper nitrate to use it again for recovery of silver. I read that this can be done by using iron to cement copper. Another method I read was using sodium hydroxide to 

copper nitrate which creates copper hydroxide. Then heat it to form copper oxide. This is the post of TomVader _"I heated my copper hydroxide solution on medium heat 

on a hot plate. The light blue gel changed into a fine black powder"_ from his thread: http://goldrefiningforum.com/phpBB3/viewtopic.php?f=37&t=18267. 

Electrowinning cell for copper recovery is not an option for me now. _What do you guys use in copper recovery? What would you prefer?_


I have many questions and I hope to learn more. Please correct me if I had wrong understanding on the topics I have read here.

Much thanks and more power to the forum.


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## Topher_osAUrus (May 19, 2016)

Aeon13 said:


> Good day to all!
> 
> In pursuit of learning more, I would like to ask some questions and may I let you verify things which I read here in the forum.
> 
> ...



Dilute at least double the volume.

Use free nitric up by either more silver dissolution, or copper.

Geo has used sulfamic acid to remove some nitric from silver nitrate solution with too much nitric to cement.

Iron is your best bet to recover the copper.

Electricity can get the copper and regenerate some.nitric i believe (just read it, never did it)

I wouldn't mess with making copper hydroxide, more steps, more work.

More knowledgeable people will surely assist you further.

Topher


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## autumnwillow (May 19, 2016)

1) No need to dilute the silver nitrate. Diluting it would just generate more wastes.
2) Free nitric isn't really required for cementation. If the copper doesn't react with the silver nitrate, try to wait a few minutes or mix the solution, if it still doesn't start cementing add a drop of nitric, mix and wait. 
3) Gold does not dissolve in nitric, so there is no gold to begin with in your silver nitrate solution. If there is any present they should be at the bottom of your beaker. You can recover PGMs dissolved by cementation with copper after you have filtered the silver chloride.
4) Recovering copper is not economical on a small scale, search dealing with wastes. You can recover copper powder with iron. You can use this powder to cement silver but your silver will be most likely contaminated with copper. And you don't really want this copper to be used for inquartation as you will need more nitric to digest it.

Are you doing this in a fume hood? Proceed with AR and I will buy your gold!


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## Aeon13 (May 19, 2016)

Topher_osAUrus said:


> Aeon13 said:
> 
> 
> > Good day to all!
> ...




Thanks for the reply Topher. 

Then double the volume it is.



> 1) No need to dilute the silver nitrate. Diluting it would just generate more wastes.
> 2) Free nitric isn't really required for cementation. If the copper doesn't react with the silver nitrate, try to wait a few minutes or mix the solution, if it still doesn't start cementing add a drop of nitric, mix and wait.
> 3) Gold does not dissolve in nitric, so there is no gold to begin with in your silver nitrate solution. If there is any present they should be at the bottom of your beaker. You can recover PGMs dissolved by cementation with copper after you have filtered the silver chloride.
> 4) Recovering copper is not economical on a small scale, search dealing with wastes. You can recover copper powder with iron. You can use this powder to cement silver but your silver will be most likely contaminated with copper. And you don't really want this copper to be used for inquartation as you will need more nitric to digest it.
> ...



Thanks for the reply Autumn. I'm a bit confused right now.
1. I read somewhere here that diluting silver nitrate is better.

2. Again I thought free nitric acid is needed for cementation. In my situation, the copper reacts with the silver nitrate vigorously.

3. If I had small amounts of gold mixed in the silver nitrate and proceed to make silver chloride, where would the gold go?



> You can recover PGMs dissolved by cementation with copper after you have filtered the silver chloride.


 Then the PGMs would be mixed with the silver chloride?


Nope I have no fume hood for now. I am doing my refining outdoors. Mountain side to be specific. No people or animals around.

Aqua Regia method is not quite doable with my set up now Marvel. That's why inquartation is as far as I can go. Can you throw me a deal with the refined gold that I am 

making?

Thanks again


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## 4metals (May 19, 2016)

> How would you guys dilute the silver



You don't have to dilute the silver at all to cement it with copper.



> How do you reduce free nitric acid from the silver nitrate



The easiest way is to keep adding silver until there is undissolved silver in the 50/50 nitric water mix. When the silver stops dissolving the free nitric has been consumed. Free nitric is not required for cementation. 



> what if I used salt and made silver chloride? Does this mean the gold mixed in the silver nitrate will not be recovered?



The gold will not be mixed with the silver nitrate, it will be insoluble and be on the bottom. Any nitric soluble precious metals (palladium) will remain in solution with salt dropping of silver chloride. 



> I would like to recover the copper metal from copper nitrate to use it again for recovery of silver. I read that this can be done by using iron to cement copper.



Iron is the metal of choice because of its availability, iron drops the copper and all of the metals in between. It will produce a high in copper alloy which is useful for future copper cementation. I have heard of someone using lead in lieu of iron, this should produce a more pure copper as it is closer to copper in the electromotive series chart. (Which I have attached for your viewing pleasure!)

View attachment electromotive series.docx


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## Aeon13 (May 19, 2016)

4metals said:


> > How would you guys dilute the silver
> 
> 
> 
> ...



Thanks sir 4metals


Then I would add silver first to the silver nitrate for the free nitric acid to be used up. Anyway I will be able to recover it again. I feel stupid right now for not thinking on

doing that. :shock: 

I would use Iron then for the recovery of copper. I will download and read the document that you uploaded.

Thanks again!

Edit: just to add. Upon viewing of the document I really need to read first about the basics of electromotive series. :mrgreen:


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## autumnwillow (May 19, 2016)

Sir Mohammed,

I have found that running my small refinery is not economical at all when processing small lots. The difference from processing 60grams to 300grams is barely 2-4 hours addition.
Wait for my assay to be at least 1 percent accurate. I am still doing a bunch of tests, sacrificing my 4N bar for this.
This way I could buy your gold based on assay (0.5g - 1.0g sample) and you do not have to wait the whole day. And you can back out if you think my assay is not accurate as you are basing your gold content on specific gravity.
Then I will just consolidate your gold with the lots the I usually process. I have processed 300g already and I believe I could go higher.

Back to your refining questions.
1) No it does not have to be diluted. Again you will just generate more wastes, more room for storage and wasting water.
2) In order to save copper, put it in the silver nitrate solution, as soon as it cements silver, pull it out. Let it dissolve the silver. Then put it back again. Repeat. Or you could simply follow 4metals advice, put some silver in it wait for it to dissolve.
3) Gold will not be in solution in a 50/50 nitric digest, it will not dissolve when you do inquartation. Filter it with the finest filter paper you have to get the gold out before you proceed with silver chloride recovery. Remember to use non-iodized salt.
4) Before you think that recovering copper thru iron cementation and re-using this powder for silver recovery then using this silver for inquartation, as I have stated above the silver recovered here will most like be contaminated with copper. In my experience this is not economical at all. Compute the nitric required to digest that copper contaminant, time and fuel. Copper is cheap, go find a junk shop nearby you can buy them for $5/kilo.


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## Topher_osAUrus (May 19, 2016)

Sorry to mislead you OP

I too, could have *swore* i read that dilution for cementation helps it, as well as a bit of free nitric. But, i may have been reading the wrong persons stuff, taking it as bible truth.

I will look through my bookmarks and see where i initially saw it


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## nickvc (May 19, 2016)

I always found small trace amounts of gold in my silver from inquarting whether from careless pouring or silver chlorides from AR digests or something else I was never sure but if you run all your silver through a cell any traces will report in the slimes, my experience matches what we found when I worked for another refinery traces of gold would show in the silver if not put through a cell, if your only doing small quantities of inquarting then it probably isn't worth worrying about, we were using a lot of silver in both instances so it paid to recover the gold.


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## Aeon13 (May 19, 2016)

autumnwillow said:


> Sir Mohammed,
> 
> I have found that running my small refinery is not economical at all when processing small lots. The difference from processing 60grams to 300grams is barely 2-4 hours addition.
> Wait for my assay to be at least 1 percent accurate. I am still doing a bunch of tests, sacrificing my 4N bar for this.
> ...



I am more than willing to wait for your set up to be completed sir Autumn. Minimizing the waiting time is also a big help for me because I have to go back to the business 

that I'm running. I can manage to bring you higher amounts of gold as long as I am sure that I have a reasonable profit also. Last time was a break even for me as I have 

told you. I believe that you can do it and manage to do bigger batches sir Autumn. I know this because I met you already and know that you are an intelligent and kind 

individual. Can I ask what is a 4N bar?

For my thread:

1. You and 4metals already wrote that dilution is not necessary. This fact is then verified and thanks to you guys.

2. I will try both your methods and see whats easier for me.

3. Sometimes I think I am adding some fine powders in my pour that is why I am asking.

4. I will shop around for the cheapest copper.

Thanks again!


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## Aeon13 (May 19, 2016)

Topher_osAUrus said:


> Sorry to mislead you OP
> 
> I too, could have *swore* i read that dilution for cementation helps it, as well as a bit of free nitric. But, i may have been reading the wrong persons stuff, taking it as bible truth.
> 
> I will look through my bookmarks and see where i initially saw it



Yeah Topher. I have read somewhere also, I just can't find the thread. Anyway it's ok Topher. No need for apologies. This forum is for us to share and learn. You shared and we learned.

Thanks again.


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## Aeon13 (May 19, 2016)

nickvc said:


> I always found small trace amounts of gold in my silver from inquarting whether from careless pouring or silver chlorides from AR digests or something else I was never sure but if you run all your silver through a cell any traces will report in the slimes, my experience matches what we found when I worked for another refinery traces of gold would show in the silver if not put through a cell, if your only doing small quantities of inquarting then it probably isn't worth worrying about, we were using a lot of silver in both instances so it paid to recover the gold.




Hi nickvc! yeah, I think I am also pouring small amounts of gold from my inquarting. I have no silver cell as of the moment and yes you are right that I am doing my inquarting in fairly small quantities for now, but of course I am thinking big and hoping to do bigger volume in the future. Silver cell would be the option then.

New lessons learned again. One post and I've learned a lot already.

Much thanks nickvc!


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## autumnwillow (May 19, 2016)

4N is four 9's pure. 99.99 percent gold.


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## Aeon13 (May 19, 2016)

autumnwillow said:


> 4N is four 9's pure. 99.99 percent gold.



oh. Now I know. How I wish to make myself a 4N gold also. :mrgreen:


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## autumnwillow (May 19, 2016)

You can get up to 4N pure with nitric alone depending on your contaminants.

From your gallery pictures. I think you are doing something wrong along the process.

Are you using distilled water?
Did you follow the washing process properly?
Did you fully dissolve in nitric until there were very little to no red fumes?
Do you stir? Crumble the large chunks until they turn into fine powder? 
Do you mix the melted inquarted gold with the graphite rod?

When dissolving in nitric. put a cover on top of your reaction vessel. This will save up nitric as the gasses produced are heavy they will then to fall back on to the solution again.
Also use 2 H20 :1 HNO3 ratio for your first digest, adding a little 3 percent H202 will help save nitric.

Edit just to add: When I say cover just cover, do not seal the reaction vessel. There should be room for the gasses to go out.


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## kurtak (May 19, 2016)

Although it is true that you don't "need" to dilute your silver nitrate before cementing I have found that the benefit in doing so is well worth the increase in waste as described here (in point number 3) :arrow: http://goldrefiningforum.com/phpBB3/viewtopic.php?f=37&t=23441&p=246984&hilit=dilute#p246984 

I have had the silver from an un-diluted silver nitrate solution adhere so tight & so thick on the copper that it not only stopped the cementing process but it was also a real chore trying to scrape & pry it loose from the copper which in turn made it a real pain to wash the copper nitrate out after cementing was done because the silver cement was hard compacted large lumps of silver cement --- after a couple times of that I started diluting it by "at least" the same volume as the starting solution "every time" before cementing & I am a much happier camper as a result

Kurt


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## 4metals (May 19, 2016)

I guess it all comes down to what you started with in solution. I am used to cementing out spent silver cell electrolyte. That runs about 60 g/l copper and 40 g/l silver by the time it is changed. For that solution no dilution is required. Generally big silver cells are dumped in 100 plus gallon quantities so most are resistant to doubling the volume. 

If I were cementing waste from nitric dissolves on gold fill where it is loaded up with base metals I would cut it for sure.


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## Aeon13 (May 20, 2016)

autumnwillow said:


> You can get up to 4N pure with nitric alone depending on your contaminants.
> 
> From your gallery pictures. I think you are doing something wrong along the process.
> 
> ...



1. Yes I am using distilled water.

2. Yes I did this until the last nitric boil is clear and has no red fumes.

3. I did not crumble large chunks because I read here in the forum that this is not necessary because if it is inquarted properly the nitric will dissolve base metals retaining the shape of the inquarted gold. I guess I will try to crumble the gold on my next refining. 

4. Yes I mixed the molted inquarted gold using the graphite rod that you gave me. :mrgreen: 

I will have to look for hydrogen peroxide here in our place.

And yes I just cover the beaker where I boil the inquarted gold with glass and has enough space for gasses to exit.

Thanks again Sir Autumn!


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## nickvc (May 20, 2016)

If you keep using the same silver for inquarting the gold should report back into the next lot you process, you may carry some of the gold over again but it shouldn't increase the amount of gold held in your silver by much or if at all if your careful, as I stated it was trace amounts of gold not very much per kilo around 0.1 - 0.5 grams if I remember correctly.


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## Aeon13 (May 20, 2016)

kurtak said:


> Although it is true that you don't "need" to dilute your silver nitrate before cementing I have found that the benefit in doing so is well worth the increase in waste as described here (in point number 3) :arrow: http://goldrefiningforum.com/phpBB3/viewtopic.php?f=37&t=23441&p=246984&hilit=dilute#p246984
> 
> I have had the silver from an un-diluted silver nitrate solution adhere so tight & so thick on the copper that it not only stopped the cementing process but it was also a real chore trying to scrape & pry it loose from the copper which in turn made it a real pain to wash the copper nitrate out after cementing was done because the silver cement was hard compacted large lumps of silver cement --- after a couple times of that I started diluting it by "at least" the same volume as the starting solution "every time" before cementing & I am a much happier camper as a result
> 
> Kurt



Yes that was the post Kurt! Thanks for the link. I think I experienced this. Silver from my solution formed a ball covering the hanged copper. It seems that without mixing, the reaction will stop because of the thick silver cemented on the copper. You were saying that if the solution was diluted, then cement silver will drop by itself on the bottom.

All points taken and I will have to try different methods and find out what best works with my set up.

Much thanks again sir Kurt!


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## Aeon13 (May 20, 2016)

nickvc said:


> If you keep using the same silver for inquarting the gold should report back into the next lot you process, you may carry some of the gold over again but it shouldn't increase the amount of gold held in your silver by much or if at all if your careful, as I stated it was trace amounts of gold not very much per kilo around 0.1 - 0.5 grams if I remember correctly.




I really need to be careful then in pouring. Experience will teach me I'm sure but reading here is of big help as well.

Thanks for sharing nickvc!


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## autumnwillow (May 20, 2016)

H202 can be bought in drug stores as agua oxigenada though a bit expensive compared to buying in bulk as the chemical H202 itself.

Give it a try, see how the fumes go and how much nitric it will save. Compute then see if its worth the purchase. Its sole purpose is to scrub the fumes and convert them back to nitric.


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## Aeon13 (May 20, 2016)

autumnwillow said:


> H202 can be bought in drug stores as agua oxigenada though a bit expensive compared to buying in bulk as the chemical H202 itself.
> 
> Give it a try, see how the fumes go and how much nitric it will save. Compute then see if its worth the purchase. Its sole purpose is to scrub the fumes and convert them back to nitric.



I will try it in my next batch sir Autumn. I am refining now and will try to crumble the gold as you have said.

I will update later for the result.

Thanks!


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## autumnwillow (May 20, 2016)

Aeon13 said:


> autumnwillow said:
> 
> 
> > H202 can be bought in drug stores as agua oxigenada though a bit expensive compared to buying in bulk as the chemical H202 itself.
> ...



Crumbling the gold allows it to have a higher surface area for the nitric to attack. Your end product should be a nice tan colored powder. Before proceeding with the washings wash well with distilled water before you proceed with HCL wash or you will dissolve some gold. If you do dissolve gold, use the SMB i gave you to precipitate it.


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## kurtak (May 21, 2016)

autumnwillow said:


> Crumbling the gold allows it to have a higher surface area for the nitric to attack. Your end product should be a nice tan colored powder. Before proceeding with the washings wash well with distilled water before you proceed with HCL wash or you will dissolve some gold. If you do dissolve gold, use the SMB i gave you to precipitate it.



I assume you are talking about pouring it into a (deep) pan of water (the silver inquarted gold) we call that corn flake 

Kurt


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## autumnwillow (May 21, 2016)

kurtak said:


> I assume you are talking about pouring it into a (deep) pan of water (the silver inquarted gold) we call that corn flake
> 
> Kurt



Uhm no. We are talking about the corn flakes being digested in the nitric acid. Some people here prefer the corn flakes to maintain their shape so you can wash it easily. I find that fine if you are going to go for AR digest in the next step but Aeon is only doing nitric digestion and wants to achieve higher purity gold. So I advise him to break this corn flakes after a few nitric digestions and digest again in nitric so that the surface area that the acid can attack will be higher. What he should have as an end product should be very similar to precipitated gold from AR.


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## kurtak (May 21, 2016)

autumnwillow said:


> kurtak said:
> 
> 
> > I assume you are talking about pouring it into a (deep) pan of water (the silver inquarted gold) we call that corn flake
> ...



Ah - ok - somehow it went over my head what was actually being discussed  

probable the fact that now that the weather is nice I & bunch of friends get together around the camp fire on Friday night for a good time of drinking beer & telling stories of our old exploits in life (ok - so we tell a lot of lies) :lol: 

At least last night it seemed we where having a good time - today it felt more like a good time had me (especially early this morning) :mrgreen: 

Anyway - on another note - I like the way your lab & refining are coming along since you joined the forum autumnwillow 8) 

I don't comment &/or reply to very much of your stuff because (1) you are doing a fine job & (2) some of our other great members usually say what I would anyway 

In other words - glad you are here :!: 

Kurt


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## autumnwillow (May 22, 2016)

kurtak said:


> Ah - ok - somehow it went over my head what was actually being discussed
> 
> probable the fact that now that the weather is nice I & bunch of friends get together around the camp fire on Friday night for a good time of drinking beer & telling stories of our old exploits in life (ok - so we tell a lot of lies) :lol:
> 
> ...



Thank you Kurt, if it was not for you I could have built a failed fume hood. Although there are adjustments that needs to be made to my current fume hood, I would rather let it be for now and just replace it with a new one next time.


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## Aeon13 (May 22, 2016)

autumnwillow said:


> Aeon13 said:
> 
> 
> > autumnwillow said:
> ...



I did the crumbling and yes the purity is better. Thanks Autumn!..But with the wash is where I'm wondering. I am not washing it with hydrochloric acid. I missed this step. 

Whats the purpose of HCl wash? I did the inquartation by just having three cycles of diluted Nitric then wash with distilled then a last diluted acid boil before the final

distilled water wash.


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## autumnwillow (May 22, 2016)

Aeon13 said:


> I did the crumbling and yes the purity is better. Thanks Autumn!..But with the wash is where I'm wondering. I am not washing it with hydrochloric acid. I missed this step.
> 
> Whats the purpose of HCl wash? I did the inquartation by just having three cycles of diluted Nitric then wash with distilled then a last diluted acid boil before the final
> 
> distilled water wash.



About that, I'm not a chemist but I think that there are some metals that HCL can dissolve that nitric cannot. I would also do a sulfuric wash if I were only using nitric to refine. Distilled water -> sulfuric -> distilled water -> HCL -> distilled water -> ammonia -> distilled water.


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## Barren Realms 007 (May 22, 2016)

autumnwillow said:


> Aeon13 said:
> 
> 
> > I did the crumbling and yes the purity is better. Thanks Autumn!..But with the wash is where I'm wondering. I am not washing it with hydrochloric acid. I missed this step.
> ...



You are making things more difficult than they need to be. Just follow the suggestions give to you by the experienced members on how to process your material.


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