# Rincing the crystals



## mikeinkaty (Jan 28, 2013)

I've been rincing mine 3 times with distilled water. I tested the rince water with ammonia and it did turn blue. I spot checked the rinced crystals by boiling 3 samples in a test tube and that water did not test blue. So, how good of a test is ammonia for the presence of copper in a solution?

Mike


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## butcher (Jan 28, 2013)

Ammonia is a very good indicator for copper in solution.
Try putting some of your final rinse in a test tube add some ammonia, with a white piece of paper behind the test tube, to help see a slight blue against white back ground, if it still looks clear you have removed about all of the copper the water washes can dissolve.

Copper metal as you know is not soluble in water, as you know.
But most of the copper salts are water soluble.


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## mikeinkaty (Jan 28, 2013)

butcher said:


> Ammonia is a very good indicator for copper in solution.
> Try putting some of your final rinse in a test tube add some ammonia, with a white piece of paper behind the test tube, to help see a slight blue against white back ground, if it still looks clear you have removed about all of the copper the water washes can dissolve.
> 
> Copper metal as you know is not soluble in water, as you know.
> But most of the copper salts are water soluble.



How likely is copper metal to be in the silver crystals? Does anyone have a fire assay of their silver from electrolysis? I'm curious if other metals were present, what they were, and how they got there.

On my next batch of crystals I'll do the ammonia test on all 3 rinces. Is there any need to wash the crystals with boiling water? I've just been rincing with distilled water at room temp.

Mike


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## mikeinkaty (Jan 28, 2013)

My normal batches of 4 or 8 ounces have been coming clean with the 3rd rince with room temp water. My last batch was 16 ozs and it took 4 washes with the first two being with almost boiling water. The ammonia test for copper did not show clear until after the 4th wash.

Mike


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## butcher (Jan 29, 2013)

I was not sure where these silver crystals you were washing came from, being a cell you probably would not have much copper salts to wash, and no metal copper in your silver crystals if the cell was run properly.

But if these silver crystals came from cementing with copper and you used thin copper pipe or wire then you could have copper in with the silver crystals, this is the reason for me mentioning the copper in my reply above.


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## Palladium (Jan 29, 2013)

What are you washing them in?


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## mikeinkaty (Jan 29, 2013)

Palladium said:


> What are you washing them in?


A stainless steel bowl and distiller water. With 4 to 8 ozs of crystals it generally takes me 3 rinces to git rid of the coppr nitrate.

The bars that are going into my cell were made by disolving sterling with Nitric Acid and by dropping the silver with copper. Some of these same bars were also used to make the electrolyte. I wouldn't expect more than 1% or 2% copper in these bars. But, there is copper in the electrolyte and it is increasing every time is do another batch. I am washing the crystals to get rid of this of copper nitrate. Is there another way to get rid of it?

Mike


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## Palladium (Jan 29, 2013)

A buchner funnel is best. I get my water boiling and pour it on top of the crystals with out vacuum. I let it set for a minute and then turn the vacuum on. I repeat two more water washes with the vacuum on. By washing it in a bowl, beaker, or what have you you are not so much removing contaminates as much as you are diluting them each rinse.


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## mikeinkaty (Jan 29, 2013)

Palladium said:


> A buchner funnel is best. I get my water boiling and pour it on top of the crystals with out vacuum. I let it set for a minute and then turn the vacuum on. I repeat two more water washes with the vacuum on. By washing it in a bowl, beaker, or what have you you are not so much removing contaminates as much as you are diluting them each rinse.



Well, I have a Buchner funnel but lately its been pressed into sevice filtering dropped mud! But I will try that.

Mike


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## Palladium (Jan 29, 2013)

Why filter dropped mud? Gold is not suppose to leave the beaker once it is dried. Procedures are the backbone of refining.


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## mikeinkaty (Jan 29, 2013)

Palladium said:


> Why filter dropped mud? Gold is not suppose to leave the beaker once it is dried. Procedures are the backbone of refining.


We're talking silver here! I call it mud, I guess most call it cement.



Mike


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## Palladium (Jan 29, 2013)

My bad! I see.


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## mikeinkaty (Jan 30, 2013)

I've cut back the current on my two cells from 6 amps to 3 amps. Even though it doubles the time I prefer working with the larger crystals. Heavy and rince well and melt well. Plus I'm supposed to be retired - why get in a hurry. I'm at the point now where I melt and pour as soon as the crystals are dried. Some day I'm going to figure out the art of pouring! No science to it, it's all art. I keep getting like crystalline patterns on top of the bars. They are smooth but its crystalline looking on top of the bar. Bottom is nice and shiny like silver should be. To much oxygen I guess getting to the top. I don't know how to describe it.??? Sooting the inside of the mold definitely makes the bottom of the bars look better. I tested several bars and the silver test solution behaved exactly as it did on an Englehard 999 bar.

I've run over 80 ounces, combined, through the electrolyte in the two cells now (each 4 liter) and they are still producing nice clean pretty crystals. Even better at low amps. I got another batch of electrolyte waiting. Hope I didn't disolve 8 ozs for nothing. 
Mike


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## butcher (Jan 30, 2013)

Mike, 
I cannot wait until I can retire and not to have to be in a hurry.

The crystaline structure on top of your bars may just be showing its purity.


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## mikeinkaty (Jan 30, 2013)

The Buchner funnel is much better and easier way to clean the crystals! After the 3rd rince with boiling water the water shows clear on the ammonia test.
I collected and poured 1.1 oz of silver from my last collection from my waste buckets. These were five, 1 gallon jugs that had accumulated over the last week. I had left the copper in them for 2 or 3 days. 

Thanks everyone!

Mike


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## mikeinkaty (Feb 2, 2013)

butcher said:


> Mike,
> I cannot wait until I can retire and not to have to be in a hurry.
> 
> The crystaline structure on top of your bars may just be showing its purity.



Could be. I notice these are softer than the 98%-99% bars. Every one of these bars has that crystalline pattern on top. I am begining to get the knack of pouring these. I now keep a Mapp gas torch on the mold all the time while pouring several bars and I soot the mold between bars. Slowly swirling the crucible and the torch at the same time and varying the distance between the torch tip and the molten pool makes a clean pool of molten silver with no floaters on top. I always add a TINY amount of 20 mule team borax once the pool quits sticking on the sides. When the pool is no longer sticking anywhere inside the crucible and the top is clean then I pour. That seems to be working. Makes a nice smooth bar with just a small indentation on the top and a flat bottom.

Mike


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