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Specialty Chemistry Forums => Citizen Chemist => Topic started by: Elroachito on June 15, 2016, 07:48:07 AM

Title: Silver refining process(nitric acid) and equipment advices
Post by: Elroachito on June 15, 2016, 07:48:07 AM
Hello, my name is Daniel, I’m 25 years old and I’m kinda doing the mad scientist stuff. After a little experiment in refining silver at home with improvised equipment, following  this http://www.abovetopsecret.com/forum/thread810904/pg1 (http://www.abovetopsecret.com/forum/thread810904/pg1), I’ve decided that I want to do it again with the proper equipment to minimize the loss of silver. In this topic I’m going to present the equipment that I want to use and why i want to use them, so after i can ask some questien and advices.
I want  to mention that I have almost 0(a few hours of research on google) knowledge in chemistry and I’m expecting answers that I can understand.

So, let’s start….

Equipment for Dissolving process:
For dissolving the silver scraps I’m thinking to use a Round bottom flask with two necks, with angled side neck - 1000ml like this:

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/1x%20-%20Round%20bottom%20flask%20two%20necks%20with%20angled%20side%20neck%20-%201000ml_zpsrjdq0bwm.png)

In the primal neck i want to attach an adaptor with right-angled (90) hose connection like this:

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/1x%20-%20Adaptor%20with%20right%20angled%2090%20hose%20connection%20-%2029-32_zpsm3gp41p5.png)

And to this I want to attach a hose so I can control NO2 gas.

In the side neck I want to use a cap which I can open whenever I want to add more Nitric Acid.

For the filtering process I want to use the Buchner filter-Vacuum process with these:

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/1x%20-%20Filtering%20flask%20with%20plastic%20side%20hose%20connection%20-%201000ml_zpswcg9xjmk.png)

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/1x%20-%20Water%20trump_zpsqxlvto8d.png)

 
And one of these Filter types.

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/1X%20Palnie%20Buchner_zpsj7apqrpe.png)

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/1x%20Palnie%20Buchner%20Disc%20Poros_zpsvb1murjz.png)

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/1x%20Filter%20Funnel%20-%20125ml_zpsjeheyo9b.png)

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/Guko_zpsxe9bzwlg.png)
 

 Additional equipment that I'm thinking it will be useful in my lab:

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/1x%20Erlenmeyer%20flask%20with%20narrow%20neck%20and%20graduated%20-%20500ml_zpsvthc3vsu.png)

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/1x%20Erlenmeyer%20flask%20with%20wide%20neck%20and%20gratuated%20-%20500ml_zpsikuuvtrw.png)

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/1x%20Beaker%20tall%20shape%20and%20graduated%20-%20600ml_zpsgmt65yzj.png)

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/1x%20Beaker%20low%20shape%20graduated%20-%20600ml_zpsclux5yhc.png)

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/1x%20Graduated%20cylinder%20high%20shape%20class%20A%20-%20100mm_zps7rq4loe3.png)

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/1x%20Graduated%20cylinder%20high%20shape%20class%20B%20-%2050_zpsjvj0atro.png)

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/3x%20-%20Stirring%20rod%20with%20melted%20ends%20-%20%20300mm_zpss8bgtwsi.png)

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/Glass%20boiling%20rod%20with%20paddle%20-%20250mm_zpsgx9yhain.png)

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/1x%20Alcohol%20lamp%20-%20100mm_zpsgssk6clm.png)


Pictures from previous experiment.

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/13453799_1462255503800719_719171744_n_zpsriosmxdd.jpg)

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/13472369_1462255513800718_880552504_n_zpstskiv7eo.jpg)

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/13472369_1462255513800718_880552504_n_zpstskiv7eo.jpg)

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/13473824_1462259483800321_1073634407_n_zpszuu7f4in.jpg)

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/13472378_1462255560467380_1144048817_n_zps7lqe3uzy.jpg)

The black marks it`s borax. Someone told me that it`s more then 950 but i really hope it`s more. Is it possible to found out somehow ?


Questions:

1.   Which kind of filter is the best to filter out the colloidal silver from the liquid and what`s the difference between them?

2.   After the vacuum filtering process the colloidal silver is completely dry or do I need to dry it? What kind of equipment I need to dry it?

3.   In my previous experiment I used copper to extract out the silver from liquid. What else I could use?

4.   Which is the formula to calculate exactly the amount of nitric acid that I need to dissolve a specific weight of silver.

5.   Which is the best process to melt the colloidal silver into metal without any loss? Untill now i used oxi-butan autogen stuff like this but i feel like it's too messy.

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/13457807_1462255557134047_756706791_n_zpsgm65qr6s.jpg)

6.   How pure is the refined silver since I’m refining industrial silver like this:

(http://i1378.photobucket.com/albums/ah110/Daniel_Lincu/13472180_1462259487133654_2133825430_n_zpswd2ogq8j.jpg)


7.   I’m thinking that by releasing the NO2 gas into the atmosphere I’m polluting and  I don’t like it, what option do I have with the gas? Is there any other chemical process by attaching something to the hose so I can get something useful from the gas or maybe to neutralize it.



i'm looking for all kind of advices.. especially for minimize the loss and to speed up the procces by adding components if it’s possible to the current setup. Also, If there is another setup on the internet I would really like to see it.

Thanks!
Title: Re: Silver refining process(nitric acid) and equipment advices
Post by: Intanjir on June 17, 2016, 09:48:20 AM
Interesting stuff!

Is it possible to simply reuse the nitric?
The major barrier to reusing it that I see is that the process given has a dilution stage. This means you would have to distill to get the concentration back to the original level. See this  recent thread (http://www.chemicalforums.com/index.php?topic=84726.0).
If there was no dilution stage than it might be possible to regenerate by electroplating out some of copper using carbon electrodes.

I would think that the metal that precipitates should be rather pure silver. You are using copper so nothing higher than it in the reactivity series should precipitate. So your only contaminates are likely to be noble metals and any copper that somehow didn't dissolve.

Rather than use copper you might use a source of chloride ions. Virtually all chloride salts are rather soluble with silver, lead, and mercury the major exceptions. So if you add some HCl to a solution containing dissolved silver then silver chloride should come right out. The remaining solvent now begins to resemble aqua regia, so if you had any gold you wanted to dissolve this might be a useful process. But since you are just working with silver then you are probably better off with a process where you can reuse your nitric.

Another possibility is to electroplate out the silver, ie electrowinning.
Title: Re: Silver refining process(nitric acid) and equipment advices
Post by: Elroachito on June 17, 2016, 10:17:09 AM
Interesting stuff!

Is it possible to simply reuse the nitric?
The major barrier to reusing it that I see is that the process given has a dilution stage. This means you would have to distill to get the concentration back to the original level. See this  recent thread (http://www.chemicalforums.com/index.php?topic=84726.0).
If there was no dilution stage than it might be possible to regenerate by electroplating out some of copper using carbon electrodes.

Could you tell me if you can find a distillation machine in this catalog that could fit to my hose and recycle the nitric.
http://www.adriansistem.ro/AdrianSistem_Catalog_Sticlarie_de_Laborator.pdf



Rather than use copper you might use a source of chloride ions. Virtually all chloride salts are rather soluble with silver, lead, and mercury the major exceptions. So if you add some HCl to a solution containing dissolved silver then silver chloride should come right out. The remaining solvent now begins to resemble aqua regia, so if you had any gold you wanted to dissolve this might be a useful process. But since you are just working with silver then you are probably better off with a process where you can reuse your nitric.

Another possibility is to electroplate out the silver, ie electrowinning.

This could be very usefull for me  i think. I'm practicing with silver, getting familiar with the equipment, preparing for refining gold... in the future i want to make alloys with colored metals and gold used in jewlery. I'm learning all of this so when i start making jewlery i will be abble to recycle all of my gold alloy scraps.

Maybe you know what else i could recover from the blue stuff and what equipment i need?

Thank you, i really appreciate.


Title: Re: Silver refining process(nitric acid) and equipment advices
Post by: Intanjir on June 17, 2016, 11:30:44 PM
Sorry, I've never done it so I don't know a thing about actually performing a distillation =/
I mostly get by with plain beakers for what I do.