I was recovering and refining scrap Sterling 925 silver jewelry used nitric acid and distilled water to produce silver nitrate, then used hcl to form silver chloride, and lye & sugar to cement the silver out. I rinsed with boiling distilled water about 10 times with a hcl boil about midway through. This morning everything was settled out, had doctor appointments today. When I got home getting ready to finish up. This weird science stuff was going on, settlement had started to float. It didn't go all the way to the top of the solution it stayed about an inch from the top. Looked like it was suspended in time slow motion. I do my refining out on my front porch, it mid 90s today in South Florida. I did notice that going down as temp started cooling down. These chemical reactions are so amazing and mind blowing.
Weird thing happening
- Thread starter johnalden082
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I’ve often wondered how long it would take for global warming to raise its ugly head in the refining world!!!!
What are saying did I do something wrong? I'm just trying hone my refining skills is why I posted what I did. I you only have smart a$$ comments just keep them to yourself. But if have information that will help to hone my skills I'm all ears.
Thank you anyway
As far as I can tell the only thing you did wrong is refining on your front porch. But I didn’t want to mention that because you might have taken that as a smart a$$ comment.
A little ice may have made it settle better but a quick filtration will separate the Silver from the rinses easy enough.
Do yourself a favor and move away from your house with your refining work.
A little ice may have made it settle better but a quick filtration will separate the Silver from the rinses easy enough.
Do yourself a favor and move away from your house with your refining work.
I'm not completely stupid. I do my work in an fumehood where the fumes are piped a 100 feet from the house. The porch is a open air style with only a roof over it. You can't any more ventilation then that.
Good that you have a hood, can’t say I’ve ever seen a refining hood on a porch before, a swing or a rocking chair, perhaps, but refining equipment is usually tucked away out of sight. But to each his own.
Your description of what you did doesn’t coincide with the looks of the solution. I assume you did 10 washes after you filtered the Silver Chloride from the nitric dissolve. Then you added the caustic and sugar, before going to the doctor? So what we are looking it is the alkaline sugar solution with metallic Silver suspended in the liquor?
I always processed chlorides in a polypropylene epoxy cement mixer so I never could see if any Silver was suspended in the solution. Depending on how much water you added to the rinsed chlorides and how much caustic and sugar was added, you may have made a dense solution ( too little water and high solids ) and had a solution where the density of the solution was sufficient to allow the silver to float. That’s not a problem, just a possible explanation of what you saw.
Once you filter and rinse the Silver post a photo of the clean Silver. I’m sure it will be clean and completely reduced.
Your description of what you did doesn’t coincide with the looks of the solution. I assume you did 10 washes after you filtered the Silver Chloride from the nitric dissolve. Then you added the caustic and sugar, before going to the doctor? So what we are looking it is the alkaline sugar solution with metallic Silver suspended in the liquor?
I always processed chlorides in a polypropylene epoxy cement mixer so I never could see if any Silver was suspended in the solution. Depending on how much water you added to the rinsed chlorides and how much caustic and sugar was added, you may have made a dense solution ( too little water and high solids ) and had a solution where the density of the solution was sufficient to allow the silver to float. That’s not a problem, just a possible explanation of what you saw.
Once you filter and rinse the Silver post a photo of the clean Silver. I’m sure it will be clean and completely reduced.
Thank you for your explanation of the situation. This was the rinse the day before with some silver flow over. It had settled out over night, during the day some of the sediment started floating to within a inch of the surface. I noticed that as the temperature lowered so did the suspended matter, this morning was all settled to the bottom again.
I didn't filter the silver chloride, I rinse with boiling distilled water until clear and did a hcl test until no cloudiness. Then used sodium hydroxide to convert to silver oxide, the used straight regular table sugar let it sit for a few hours. Then started to rinse with water, hcl and no filtration.
I haven't seen anyone filter the chloride or the metallic silver. Now when I do a copper cementation I will filter that.
I always rinsed the Silver Chloride well. Filtered it once followed by decanting and additional rinses. The purity of your Silver from this process is largely controlled by how well it has been rinsed as the fluffy Silver Chloride tends to trap liquids which contain the impurities. So a decant followed by good mixing before decanting again gets the solid mushy Silver Chloride moving so the rinses are more effective.
You can rinse less if the purity you are looking for isn’t critical because you are going to follow up with a silver cell. So if that wasn’t your goal you can get to 98-99% by cementing with copper out of the nitric and skipping the chlorides entirely.
Once you go to Silver Chloride heavy rinsing will get you 999 Silver so the cell isn’t needed.
A lot of sterling has a little gold in it. So larger refiners will filter the solution before dropping the chlorides to get it out.
You can rinse less if the purity you are looking for isn’t critical because you are going to follow up with a silver cell. So if that wasn’t your goal you can get to 98-99% by cementing with copper out of the nitric and skipping the chlorides entirely.
Once you go to Silver Chloride heavy rinsing will get you 999 Silver so the cell isn’t needed.
A lot of sterling has a little gold in it. So larger refiners will filter the solution before dropping the chlorides to get it out.
Thank again for enlightening on a different way to process the silver. Like I said before I'm here to hone my refining knowledge and skills.
I've had a refiner in Miami didn't trust his XRF machine and had to melt the gold button I was selling him. It tested 99.999 he couldn't belive I took scrap jewelry and done that good of job on it. The few silver bars that I have done has been 99.999 also
goldenchild
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Silver chloride stacks up and becomes a huge amount of material to deal with very quickly. What I always did was keep a very clean and dedicated 5 gallon bucket (white) for dealing with chloride. After the initial decanting of the blue/green liquid i would set the chloride in the 5 gallon bucket and hit it with a garden hose. This lets the material get blasted thoroughly getting all the base metal liquor out of all the nooks and crannies. Decant and repeat.
In the end your chloride should be snow white. If doing it outside the sun will put a little purple/violet tint on the chloride but is not a big deal at all. Don't do the reaction in the 5 gallon bucket though. Put it in a glass beaker or some other bucket keeping the dedicated 5 gallon pristine. You could dedicate one for rinsing and one for the reaction. Keeping one bucket clean makes if very easy to see when the rinsing is 100% done. Using this method I consistently got 4 nines silver.
In the end your chloride should be snow white. If doing it outside the sun will put a little purple/violet tint on the chloride but is not a big deal at all. Don't do the reaction in the 5 gallon bucket though. Put it in a glass beaker or some other bucket keeping the dedicated 5 gallon pristine. You could dedicate one for rinsing and one for the reaction. Keeping one bucket clean makes if very easy to see when the rinsing is 100% done. Using this method I consistently got 4 nines silver.
Thank you for your insight and method of cleaning silver chloride. You definitely don't want to do the lye and sugar method in plastic unless you want it all on the floor. Lye and sugar is a very violent reaction and temperature close to 200 degrees Fahrenheit.
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What kind of vacuum furnace do you use for your silver bars? How do you justify the inert atmosphere equipment and just do a few bars of silver? What mass spec do you use to ascertain 5N purity?
