Has any seen this type of percipitate from AR before?

[Emryst]

Ok so I ran a few batches of gold filled, burned and processed my filters I have built up and processed nitric waste i been pouring over some gold colored chalices mark international silver co. in a collection pot and processed the other stock pots for any waste. Did several nitric dissolutions on all that for a single AR. I didn't get any silver out from the nitric solution even after a day of leaving copper in to cement. So ok I took all the filtration from the batches and filters and incinerated then into AR. Filtered solution added ice and sodium metabisulfite to percipitate the gold. I knew some gold was in solution from a stannous test. After a few hours or so I looked at it and these crystal formation are dropping out. (See photo) does anyone know what is dropping out so I know what to do with it? I.e. run thru nitric again to seperate and then thru AR to get gold out. Or if this is something other then silver or gold. I wouldn't think it's silver cause silver would have come out at the nitric phase of dissolution. I've just never had this reaction with metabisulfite to percipitate gold before.

 

[Yggdrasil]

Ok so I ran a few batches of gold filled, burned and processed my filters I have built up and processed nitric waste i been pouring over some gold colored chalices mark international silver co. in a collection pot and processed the other stock pots for any waste. Did several nitric dissolutions on all that for a single AR. I didn't get any silver out from the nitric solution even after a day of leaving copper in to cement. So ok I took all the filtration from the batches and filters and incinerated then into AR. Filtered solution added ice and sodium metabisulfite to percipitate the gold. I knew some gold was in solution from a stannous test. After a few hours or so I looked at it and these crystal formation are dropping out. (See photo) does anyone know what is dropping out so I know what to do with it? I.e. run thru nitric again to seperate and then thru AR to get gold out. Or if this is something other then silver or gold. I wouldn't think it's silver cause silver would have come out at the nitric phase of dissolution. I've just never had this reaction with metabisulfite to percipitate gold before.

I'm on a phone so it is not too easy to reply properly.
But it seems you plan changes many times and often without sufficient reasoning.
A weak Stannous might not even be visible as it cements.
And you spend way to much Nitric.
Ice is added before filtering not along the SMB.

 

[Emryst]

I'm on a phone so it is not too easy to reply properly.
But it seems you plan changes many times and often without sufficient reasoning.
A weak Stannous might not even be visible as it cements.
And you spend way to much Nitric.
Ice is added before filtering not along the SMB.

I don't know what u mean my plan change many times. I had alot of stuff gold filled jewelry, stock pots, filters and the pouring off pot to refine. Rather then do one each time with small or no gold values in each I held and combined for a single AR solution. For me to be able to do all the different sources i.e gold filled filters stock pots collections. I would have needed a 5 gallon beaker or some thing.

I don't know if this clarified why i did what a did and how i did it and i dont think the ice being added before or after filtering would matter much on getting this result in the AR percipitatant but i will add before filtering in future refinings. Tho you didn't even answer what this percipitatant might be given your greater experience in refining.

I haven't gotten a close look at it as it had not been enough time for the percipition to finish i will see that in a few hours when I can get back to it.

 

[nickvc]

The problem you are encountering is due to the fact you combined different material sources hoping to save time and or chemicals, we always advise to process each type of material separately for this very reason .
My advice add copper to your solution and try to recover the values that way .

 

[Emryst]

Ok so I ran a few batches of gold filled, burned and processed my filters I have built up and processed nitric waste i been pouring over some gold colored chalices mark international silver co. in a collection pot and processed the other stock pots for any waste. Did several nitric dissolutions on all that for a single AR. I didn't get any silver out from the nitric solution even after a day of leaving copper in to cement. So ok I took all the filtration from the batches and filters and incinerated then into AR. Filtered solution added ice and sodium metabisulfite to percipitate the gold. I knew some gold was in solution from a stannous test. After a few hours or so I looked at it and these crystal formation are dropping out. (See photo) does anyone know what is dropping out so I know what to do with it? I.e. run thru nitric again to seperate and then thru AR to get gold out. Or if this is something other then silver or gold. I wouldn't think it's silver cause silver would have come out at the nitric phase of dissolution. I've just never had this reaction with metabisulfite to percipitate gold before.

If anyone is following this thread and has any ideas. I finally got back to pour off the solution to see what percipitated out and here it is some kind of ugly looking shag rug lol. I have never seen this before. But my experience is far from vast with home refining. And I have no chemistry back ground to speak of as well. So any ideas would be much appreciated on what this is and how to proceed. Cause my only thought is to do another hot nitric on it and then back in AR after. It's really my only 2 weapons in my arsenal. Lol the last photo I think shows the gold that percipitated out first.

 

[Emryst]

The problem you are encountering is due to the fact you combined different material sources hoping to save time and or chemicals, we always advise to process each type of material separately for this very reason .
My advice add copper to your solution and try to recover the values that way .

Ok so if you could look at my last post to this thread and advice a course of action. I.e. hot nitric then AR again. I believe i can see my values on the bottom. I just don't know what the grey silverfish stuff is and how to seperate them. To my understanding platinum is not dissolved in nitric but does in AR. I use smb to percipitate and I may be wrong but I thought smb didn't target platnium to percipitate only gold. So I can't figure out what dropped out with gold in this crystal formation.

 

[Mike Low]

You are near the end of your process,
Think things through
Let's see a picture of your test for gold after your SMB drop

 

[100tific]

Something like this has ever happened to me. I think due to excess metabisulfite.

 

[100tific]

I think it is a copper compound that is formed by excess metabisulfite. It has happened to me that when I have melted it, instead of pure refined gold appearing, copper also appears. but it can be melted without problem. I would wash it well with water and filter, and then melt. you will get gold with copper and other metals, so you will have to refine it again

 

[Martijn]

I think it is a copper compound that is formed by excess metabisulfite. It has happened to me that when I have melted it, instead of pure refined gold appearing, copper also appears. but it can be melted without problem. I would wash it well with water and filter, and then melt. you will get gold with copper and other metals, so you will have to refine it again

Melting gold to refine it again makes no sense, imo
You have very fine gold powder ready to be washed clean by acids, so why melt the impurities back in the gold, where it is much harder to reach?

 

[Martijn]

Ok so if you could look at my last post to this thread and advice a course of action. I.e. hot nitric then AR again. I believe i can see my values on the bottom. I just don't know what the grey silverfish stuff is and how to seperate them. To my understanding platinum is not dissolved in nitric but does in AR. I use smb to percipitate and I may be wrong but I thought smb didn't target platnium to percipitate only gold. So I can't figure out what dropped out with gold in this crystal formation.

looking at your pictures; My very first advice for you to do: go buy some plastic gloves! Dirt cheap and life altering! (you will live longer)

 

[Martijn]

How many hot water washes did you do on this powder?

 

[Proffshuggarn]

If anyone is following this thread and has any ideas. I finally got back to pour off the solution to see what percipitated out and here it is some kind of ugly looking shag rug lol. I have never seen this before. But my experience is far from vast with home refining. And I have no chemistry back ground to speak of as well. So any ideas would be much appreciated on what this is and how to proceed. Cause my only thought is to do another hot nitric on it and then back in AR after. It's really my only 2 weapons in my arsenal. Lol the last photo I think shows the gold that percipitated out first.

@Emryst
If I were you, I'd listen to the feedback you've already received from some of the most knowledgeable professionals on this forum...
Just a piece of advice in all fairness.
Or call the bomb squad...

 

[Emryst]

Good looking out. I am trying to get better at remembering to put gloves on. I'm 53 and I have always used my hand from wood working to car repair. And stopping to put gloves on was never a thing. But yes it is a behavior I need to be much more mindful of. Appreciate you cheif.

 

[Mike Low]

If anyone is following this thread and has any ideas. I finally got back to pour off the solution to see what percipitated out and here it is some kind of ugly looking shag rug lol. I have never seen this before. But my experience is far from vast with home refining. And I have no chemistry back ground to speak of as well. So any ideas would be much appreciated on what this is and how to proceed. Cause my only thought is to do another hot nitric on it and then back in AR after. It's really my only 2 weapons in my arsenal. Lol the last photo I think shows the gold that percipitated out first.

I seem to remember adding a small amount of sulphuric acid during digestion, looks like a dirty drop, and to much SMB,
Ash it and start again, keep testing, nearly there.

 

[Martijn]

Good looking out. I am trying to get better at remembering to put gloves on. I'm 53 and I have always used my hand from wood working to car repair. And stopping to put gloves on was never a thing. But yes it is a behavior I need to be much more mindful of. Appreciate you cheif.

there clearly are salts on the bottom, some salts are soluble, some are slightly soluble, some are not. They look like tiny christmas trees.

Again: did you try a hot water rinse to see if anything dissolves? You can test it on a bit first and see if the salt is soluble in water, and if it stays soluble when cooled down.

then we can discuss the next step.

How much gold are you expecting? / how stong was that stannous test? / Did everything dissolve during AR?

Filtered solution added ice and sodium metabisulfite to percipitate the gold.

It works better if you decant (or filter if needed) the pregnant solution first, then add ice or dilute with cold water, then filter the silver chloride out you've pushed out by cooling and diluting, repeat filtering using the same filter, until you can read a newspaper through the solution.

The thing is, with AR you can recement your dissolved pm's back on base metals (which you suspected are still present after the nitric bath) So what was left after AR?

 

[Emryst]

there clearly are salts on the bottom, some salts are soluble, some are slightly soluble, some are not. They look like tiny christmas trees.

Again: did you try a hot water rinse to see if anything dissolves? You can test it on a bit first and see if the salt is soluble in water, and if it stays soluble when cooled down.

then we can discuss the next step.

How much gold are you expecting? / how stong was that stannous test? / Did everything dissolve during AR?

It works better if you decant (or filter if needed) the pregnant solution first, then add ice or dilute with cold water, then filter the silver chloride out you've pushed out by cooling and diluting, repeat filtering using the same filter, until you can read a newspaper through the solution.

The thing is, with AR you can recement your dissolved pm's back on base metals (which you suspected are still present after the nitric bath) So what was left after AR?

Ok so a couple people had said this might be from adding to much smb. Maybe this wasn't the best idea but I washed and redid AR and smb on it. This is the results after a ton of hot washing. I can see it is contaminated. And supports a fellow members post on this as well that this is why we don't do multiple batches for a single AR. So from here I'm think melt test gold karat and inquart with silver and proceed as a normal karat gold process. Any thoughts to that course of action? I have some other smaller values i percipitated that I had intended to melt inquart and refine again anyway so I could do it all together.

 

[100tific]

did you filter it after the AR?
what is the difference between first picture and the second?

 

[MvK]

At this point i would not inquart, silver should be filtered out already when it was converted to silver chloride in your AR step.

When i have traces of silver in a dirty solution i go to AR, dillute a bit and filter warm. After that im using ice to get the AR cold and run it trough the same filter. It seems to close the pores in the filter to catch more chlorides.
Dont disturb the filter by rinsing in your clean AR, transfer to temporary stockpot and rinse there.

Leave the AR for a day and if no contaminations have settled on the bottom proceed to SMB and do a Harold style wash.

 

[Emryst]

At this point i would not inquart, silver should be filtered out already when it was converted to silver chloride in your AR step.

When i have traces of silver in a dirty solution i go to AR, dillute a bit and filter warm. After that im using ice to get the AR cold and run it trough the same filter. It seems to close the pores in the filter to catch more chlorides.
Dont disturb the filter by rinsing in your clean AR, transfer to temporary stockpot and rinse there.

Leave the AR for a day and if no contaminations have settled on the bottom proceed to SMB and do a Harold style wash.

My idea to inquart is because i think there are other contaminates in the gold. It's greenish silver color. Maybe some iron i didn't add sulfur i don't have any at the moment.