Washing pure silver powder

[jeweler1]

Using Metalicmarios Video on Metalicmario’s channel on YouTube as a guide I dissolved a Palladium/ Silver alloy with 50%nitric acid and 50% distilled water. I than used a combination of Salt and HCL to obtain silver chloride, after filtering and washing several times with distilled water to get it white I added Sodium hydroxide and Karo syrup to get “elemental silver”. It’s Gray? How do I wash it to get it White? It’s pure white in the video with no explanation of how it got that way? I wash my gold powder with distilled water and HCL followed by more distilled water. But what is the “proper method for washing pure silver powder?

 

[Lino1406]

Wash the AgCl with hot water, check if
the rinse water colors SnCl2 solution

 

[butcher]

silver chloride is white, if washed and diluted it will try to convert to silver metal powders in light which will darken towards black or dark violet color powders.at least what portions of the fine crystals the light shines on will.(Same principle photography uses).

Normally after sodium hydroxide and Karo syrup to convert the silver chloride to elemental silver metal powders gets dark gray or blackish in color the liquid looks like tea or root-beer.

I have noticed if the silver chloride is dirty with other metals it does not convert back to elemental metal as easily as good clean silver chloride will.

GSP has posted several times how he washed his silver chloride,and how it is important to good conversion, and how he tested for copper using ammonia.

The suggestion to test for Pd using stannous chloride (or DMG to test for palladium), is a good idea.

 

[philddreamer]

If I use the Sodium hydroxide and Karo syrup,(or sugar), I rinse my silver with hot tap water until the water is clear, (and it doesn't smell like burnt sugar). Then I place it in a couple of coffee filters and let drain; then dry it. Then to the melting dish! :mrgreen:
Phil

 

[kadriver]

The silver chloride is usually pure white after washing over and over with hot water - boiling if possible.

After converting the silver chloride to silver oxide with lye (sodium hydroxide) the material should look almost pitch black.

After adding the Karo Syrup or sugar to convert the silver oxide to pure elemental silver metal, the silver should look grey in color - just like cement silver.

The pictures of the cement silver might make it appear white, but it is grey in color, as it should be.

I place the silver powder in a container, add boiling tap water, stir it for several minutes, then settle and pour off the liquid.

I have two 5 gallon buckets that I use to pour off the wash water. The wash water will have suspended silver particles that take forever to settle completely.

Unless you wait over night after each wash water addition (takes too long), you can pour the wash water into these buckets and allow them to settle completely and then recover the silver later on.

I do the same thing with gold washes - sometimes I need the gold sooner and I can't wait for it to settle overnight. I pour off the wash water into a large glass container and allow it to settle overnight and then get the gold after it settles completely the next day.

When you wash the final product make sure and check the pH of the wash water as you go - keep washing until the pH test is neutral, then wash it one more time.

It takes quite a few washes to completely remove all the sugar and residual sodium hydroxide, use HOT water if possible.
If the lye is not washed out completely it can etch your glass drying dish.

I ruined a nice corningware casserole (pyroceramic) dish due to incomplete washing. Some of the lye was still in there and it started to dissolve the glass when I attempted to dry the silver powder.

kadriver

 

[mikeinkaty]

Why would one choose the Silver Chloride method over using copper to drop silver? I don't recall ever seeing this discussed. I know how they work - just don't see a good reason for choosing one method over the other. Looks to me like the copper method would be cheaper.

Mike

 

[SilverNitrate]

whichever method of making silver powder use sequestration ...not that 'sequestration' for removing metal oxides e.g. ethylenediaminetetraacetic acid. Or you can simply titrate with a tiny amount of HNO3, boil and blend of course, to force the reaction away from silver. I don't know if Pd is reactive in HNO3 but if it is less reactive than silver, you will have to process that first.

 

[amesametrita]

whichever method of making silver powder use sequestration ...not that 'sequestration' for removing metal oxides e.g. ethylenediaminetetraacetic acid. Or you can simply titrate with a tiny amount of HNO3, boil and blend of course, to force the reaction away from silver. I don't know if Pd is reactive in HNO3 but if it is less reactive than silver, you will have to process that first.

Be ready to be blamed for mention EDTA here. :shock:
Only locally approved procedures should be discussed here :lol:

 

[skippy]

Anybody know if it Is feasible to get right to 999 or better silver right from silver chloride? That is silver chloride dropped from a solution with moderate base metal contamination I gather it's hard to get all of the original solution washed out, it takes many washes etc. I suppose if you took the silver chloride and dissolved it in sulfuric acid, then filtered any lead sulfate out and then reduced with an appropriate agent that would be one way of getting there, or at least quite close.

 

[kadriver]

I have made 999 fine silver via silver chloride conversion.

It is kind of fun to do the reactions and watch it change before your eyes.

But use caution if you have a large batch - I had 2 liters of AgCl once and I was adding cane sugar to convert to silver metal.

The batch made slight popping sounds then erupted like a volcano spewing my silver out of the container.

I had it inside a 2gallon plastic bucket and had that in a catch container and got all my silver back.

I have had this happen twice. And it does not happen the same way on each batch - some batches are docile while others are ferocious.

kadriver

 

[kadriver]

Why would one choose the Silver Chloride method over using copper to drop silver? I don't recall ever seeing this discussed. I know how they work - just don't see a good reason for choosing one method over the other. Looks to me like the copper method would be cheaper.

Mike

Mike, it took me two weeks to generate 74 Troy ounces of fine silver using the silver cell.

I could have made the same amount of silver via silver chloride conversion in just a couple of days.

Speed is the advantage, but there is much more opportunity for losses with the silver chloride conversion.

If you need lots of pure silver right quick, then silver chloride conversion is one way to get it.

kadriver

 

[mikeinkaty]

Why would one choose the Silver Chloride method over using copper to drop silver? I don't recall ever seeing this discussed. I know how they work - just don't see a good reason for choosing one method over the other. Looks to me like the copper method would be cheaper.

Mike

Mike, it took me two weeks to generate 74 Troy ounces of fine silver using the silver cell.

I could have made the same amount of silver via silver chloride conversion in just a couple of days.

Speed is the advantage, but there is much more opportunity for losses with the silver chloride conversion.

If you need lots of pure silver right quick, then silver chloride conversion is one way to get it.

kadriver

How pure is the silver that you get from the silver chloride method?

Mike

 

[amesametrita]

How pure is the silver that you get from the silver chloride method?

The drawback is loses.

 

[SilverNitrate]

Be ready to be blamed for mention EDTA here. :shock:

Is EDTA a bad word?. I think its one of those wonder chemicals.

The way to get silver chloride to metal the fastest is to melt it along with sodium hydroxide at about 2000F with plenty of flux (can be a bit dangerous tho)

 

[kadriver]

Mike,

The silver i made from silver chloride conversion was sold to a refiner and their assay said it was 999

kadriver

 

[amesametrita]

Is EDTA a bad word?. I think its one of those wonder chemicals.

It's a kind of religion here.
The Bible is Hoke's book "Refining metal waste"
EDTA is not mentioned in the Bible.
And forum members suffer with dropping gold from aqua regia by SMB and oxalic.
Knowledge here stuck 100 years ago.

And if you try to educate people, you got a religious blame:
http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=50&t=17138

 

[goldsilverpro]

amesametrita,

I developed a unique method of using a form of EDTA (HEDTA) to consistently drop 999.9 fine gold from AR solutions in the late 1960's, early 1970's. Using this method, several 100's of 1000's of oz of pure gold (used to manufacture PGC plating salts) were produced by the company I worked for. It replaced their Wohlwill cells. The EDTA derivative alone will precipitate the gold and, at the same time, chelate most of the metallic impurities and keep them in solution.

In your infinite wisdom, amesametrita, did you know that EDTA will drop gold? If so, the only place you could have gotten it is from me. I've never found it in the literature.

I do admit I found your discussion on silver cells enlightening. However, I have seen nothing else of real merit come from you. Are you just a one-trick pony? If not, show us your stuff. I would also suggest you lay off those constant sideways insults, like the thread title, Silver Cells for Dummies, or those comments on EDTA and Hoke.

Using EDTA to chelate the impurities in silver chloride conversion is an excellent idea.

The biggest problems with using EDTA are the cost and the difficulties of treating the waste solutions.

I had been refining, big time, for about 7 years before I knew the Hoke book existed and, therefore, it wasn't tremendously valuable to me. The reason it's promoted here for the newbies is that it gives, in a simple understandable manner, the very best background for the chemicals used and their reactions with the various metals. No other book I know of compares.

 

[amesametrita]

I developed a unique method of using a form of EDTA (HEDTA) to consistently drop 999.9 fine gold from AR solutions in the late 1960's, early 1970's. Using this method, several 100's of 1000's of oz of pure gold (used to manufacture PGC plating salts) were produced by the company I worked for. It replaced their Wohlwill cells. The EDTA derivative alone will precipitate the gold and, at the same time, chelate most of the metallic impurities and keep them in solution.

In your infinite wisdom, amesametrita, did you know that EDTA will drop gold? If so, the only place you could have gotten it is from me. I've never found it in the literature.

Dear goldsilverpro,

Unfortunately you haven't discovered the method.
It's almost industry standard for high purity wet method.
And I haven't heard it from you.
And I haven't seen you offer it when members ask about better gold reducing agents.
Moreover if you read my previous post here you can see that I meant EDTA exactly as substitution for their SMB and oxalic methods.
If you know the method, why don't you discuss it with the members?

I do admit I found your discussion on silver cells enlightening. However, I have seen nothing else of real merit come from you. Are you just a one-trick pony? If not, show us your stuff. I would also suggest you lay off those constant sideways insults, like the thread title, Silver Cells for Dummies, or those comments on EDTA and Hoke.

After a warm welcome from the forum celebrities after my post about silver cell I decided to offer my help only in private messages.
Some users already benefited from that.
You keep your secrets (like about EDTA), I share them in private messages, others sell books and DVDs.
What's wrong?

In public forum places I comment only absolutely nonsense ideas (Like Geo's offer to add some H2SO4 to AgNO3 to remove lead)

Regards.

 

[its-all-a-lie]

I developed a unique method of using a form of EDTA (HEDTA) to consistently drop 999.9 fine gold from AR solutions in the late 1960's, early 1970's. Using this method, several 100's of 1000's of oz of pure gold (used to manufacture PGC plating salts) were produced by the company I worked for. It replaced their Wohlwill cells. The EDTA derivative alone will precipitate the gold and, at the same time, chelate most of the metallic impurities and keep them in solution.

In your infinite wisdom, amesametrita, did you know that EDTA will drop gold? If so, the only place you could have gotten it is from me. I've never found it in the literature.

Dear goldsilverpro,

Unfortunately you haven't discovered the method.
It's almost industry standard for high purity wet method.
And I haven't heard it from you.
And I haven't seen you offer it when members ask about better gold reducing agents.
Moreover if you read my previous post here you can see that I meant EDTA exactly as substitution for their SMB and oxalic methods.
If you know the method, why don't you discuss it with the members?

I do admit I found your discussion on silver cells enlightening. However, I have seen nothing else of real merit come from you. Are you just a one-trick pony? If not, show us your stuff. I would also suggest you lay off those constant sideways insults, like the thread title, Silver Cells for Dummies, or those comments on EDTA and Hoke.

After a warm welcome from the forum celebrities after my post about silver cell I decided to offer my help only in private messages.
Some users already benefited from that.
You keep your secrets (like about EDTA), I share them in private messages, others sell books and DVDs.
What's wrong?

In public forum places I comment only absolutely nonsense ideas (Like Geo's offer to add some H2SO4 to AgNO3 to remove lead)

Regards.

Im sensing animosity in your posts since you were corrected when you thought it would be cute to put down the work of other members here. This forum is here to help the hobbyist refiner learn proper techniques in the refining methods he/she needs and each person here decides which method works best for him/her, without regard for what you or anyone else thinks it looks like. If the method/setup works and produces the desired results, who are you to belittle them and their equipment? I think i speak for most if not all here when i say the attitude you are showing is not appreciated nor is it welcomed here. True, the methods taught here are 100+ years old, BUT the methods taught here work and they work well. Your comments towards Kadriver's silver cell reminds me of a few guys at the local dirt track, they never win a race but their car is always spitshined when they start one. The guys who win most of the races do not drive the newer fancy cars, their cars are beat up and dirty, but they win, their cars get the job done. Noone is here to impress others, they are here to make themselves happy and most have been able to acheive that, but when someone comes around telling them their setup is completely wrong and it does not look good, some will get discouraged and stop trying to learn. It is clear you have alot to offer the members of this forum and im sure there are things you can learn here too, but take this as a heads up, the game you are playing will not last long and you will not win it.

 

[amesametrita]

This forum is here to help the hobbyist refiner learn proper techniques…

The key word is “proper” here. If the proposed method is wrong or outdated or not efficient I comment.