# new button has a film on it?



## glorycloud (Sep 28, 2016)

WAAH!

I have a new Au button that's just a hair over an ounce. All from fingers and well washed
and cleaned with H2O / HCL / ammonia / H20. Nice looking Au powder went into the melt.
When it came out of the melt the bottom looks great but the top has a milky sheen to it
like I spread mayo on it. I did use steel needle nose pliers to pluck the button out of the
dish. I need to get a pair of stainless steel forceps for sure!!

Would using steel pliers cause this issue?


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## FrugalRefiner (Sep 28, 2016)

glorycloud said:


> and cleaned with H2O / HCL / ammonia / H20. Nice looking Au powder went into the melt.


I would suspect the first H2O wash. Read Lou's post in Gold has been refined and melted, now has orange hue.
Dave


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## glorycloud (Sep 28, 2016)

Actually, I use pretty fastidiously use Kurtak's wash procedure. It just 
seems like when I am removing the buttons from the dish with the steel
needle nose pliers, something flashes across the face of the button but 
it all happens so fast that I can't be sure.

I did have some interesting gold flakes / crystals in the powder that 
wanted to float around during the later washes. I should have taken
a picture of them.


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## GotTheBug (Sep 28, 2016)

Try giving it a boil in dilute sulphuric and see if that helps.


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## glorycloud (Sep 28, 2016)

Good idea. I will try that tomorrow. How dilute?
I have H2SO4 from the auto parts store.


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## Barren Realms 007 (Sep 28, 2016)

WEEEEEEELLLLLLLLLLL. What does your melting dish look like? 8) 

Your close to pure just no cigar yet.  


I'm sorry I just still miss the art work.  


You know I'm never going to let you live that down don't you? :lol:


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## mls26cwru (Sep 28, 2016)

probably just surface contamination... could be from impurities the borax caught... try the sulfuric and if you remelt, see if you see 'scuzz' floating around on the top when the gold is molten just before it cools (it will have a different color orange that the gold). I have seen this a couple times and adding a pinch of borax right on top of the gold usually 'catches' the scuzz by absorbing it.... my guess is that if it is more than surface impurities, it will show up again after the sulfuric and remelt.


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## glorycloud (Sep 29, 2016)

Dish is light purple like always. I'll do the dilute sulphuric and then a remelt. 

Thanks,!


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## anachronism (Sep 29, 2016)

If that's what it looks like it might be, and it's borax then you might not need to do any remelting after you've treated it in the sulphuric.


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## goldsilverpro (Sep 29, 2016)

Like Nick implied, you might be able to clean it in the melt. I would use borax and sodium or potassium nitrate (niter). Get the button melted and rolling a bit. If it's not mirror bright, and it has a film (usually whitish) floating around on it, add a prill or two of niter. You should see a reaction and see more stuff coming to the surface. Let it react and then add a small pinch of borax (preferably, anhydrous) - that should carry the garbage to the sides of the dish. If there is still a film, repeat. If it won't clean up after doing this 4 or 5 times, re-refine in AR.

If the purity is way off, this won't work.

To me, if you're going to sell your gold, it is very dishonest to the buyer to clean up any discoloration with acids. With any surface discoloration, you must assume that the contamination is also within the gold itself. With any discoloration, I first try re-meting and cleaning it. If that fails, I always re-refine it.

I don't believe the tweezers caused the discoloration. Probably, when you touched it with the cold tweezers, the gold immediately solidified. In fire assaying, at the moment the pure gold bead solidifies in the cupel, it emits a small flash of light, which is called a "blick." Maybe the same phenomenon occurred when your button solidified.


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## kurtak (Sep 30, 2016)

glorycloud said:


> Actually, I use pretty fastidiously use Kurtak's wash procedure.



Actually - the washing procedure I have posted in "the past" I learned form read Harold's posting about washing when I "first" joined the forum 

That said - I have been using Lou's method for washing ever since he first posted it - it is a much better method & eliminates the ammonia --- the ammonia is not needed unless there is a lot of AgCl --- & there shouldn't be a lot of AgCl if you dilute, cool, settle/filter the AuCl before dropping the gold 

Kurt


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## kurtak (Sep 30, 2016)

goldsilverpro said:


> Like Nick implied, you might be able to clean it in the melt. I would use borax and sodium or potassium nitrate (niter). Get the button melted and rolling a bit. If it's not mirror bright, and it has a film (usually whitish) floating around on it, add a prill or two of niter. You should see a reaction and see more stuff coming to the surface. Let it react and then add a small pinch of borax (preferably, anhydrous) - that should carry the garbage to the sides of the dish. If there is still a film, repeat. If it won't clean up after doing this 4 or 5 times, re-refine in AR.



I agree with Chris on this one & use this method often if the contaminant is slight - I use the potassium nitrate (stump remover carried in most hardware stores) & from what I can see in this case it looks like this method has a good chance of working - it would be my first try at cleaning it up - then if not go for the re-refining 



> To me, if you're going to sell your gold, it is very dishonest to the buyer to clean up any discoloration with acids. With any surface discoloration, you must assume that the contamination is also within the gold itself. With any discoloration, I first try re-meting and cleaning it. If that fails, I always re-refine it.



I absolutely agree :!: 

Kurt


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## kurtak (Sep 30, 2016)

Not all stump removers are potassium nitrate - this one is - the fact that it is potassium nitrate is not identified anywhere on the front or back label - unless - you peel the back label & read that part of it

Kurt


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## UncleBenBen (Sep 30, 2016)

Nice paperweight, Kurt!!  :lol:


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## Barren Realms 007 (Sep 30, 2016)

kurtak said:


> glorycloud said:
> 
> 
> > Actually, I use pretty fastidiously use Kurtak's wash procedure.
> ...



If you can find one of Lou's original post's on his HCl washing method he tells that it he does it this way to remove the small amounts of silver chloride so that he doesn't have to deal with the ammonia wash. If I remember correctly!!!!



Here is something that everyone needs to realize and keep in their mind. Each of the members here that produce high purity gold have their own way of doing it. We don't all follow the same procedure but we get pretty close the same results. You have to learn the develope your procedure around what you have available and are comfortable in working with and the time frame you have to process your material and the patience you have in achieving your goal of purity.


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## glorycloud (Sep 30, 2016)

goldsilverpro said:


> To me, if you're going to sell your gold, it is very dishonest to the buyer to clean up any discoloration with acids. With any surface discoloration, you must assume that the contamination is also within the gold itself. With any discoloration, I first try re-meting and cleaning it.



No dishonesty or deception from this fellow. Not going to sell what I have - they're just for
me and my bride of thirty years to look at and keep. Momma likes "shiny" not milky looking.
That's the reason for this thread, not how I can deceive a buyer.  

Having made that disclosure, thank you for the advice. I have some sodium nitrate. Let me attempt
a re-melt and see what happens.

These fingers were from really old fingers and I guess they could have some metals that I am not used 
to having present when I process and refine the gold from fingers. At the end of the melt when the
gold is all melted and iridescent looking, I did see a whiteish bubble / circle "fall off" from the top
to the side of the gold circle. I never knew what that was but I have seen it occasionally occur. An
impurity of some sort or another PM perhaps?


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## anachronism (Sep 30, 2016)

Barren Realms 007 said:


> kurtak said:
> 
> 
> > glorycloud said:
> ...



I agree Frank. You can get rid of AgCl using HCl. I don't use ammonia in this process at all. Also you're quite right in that everyone has their own "bent" on how to get their pure gold based on the right procedures. I still think that button looks like it has a cap of borax on it though however it's a picture not the real thing in my hand.


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## Topher_osAUrus (Sep 30, 2016)

If its hi yield sodium nitrate, that product only contains 26% NaNO3.
The stump killer kurt showed (available at lowes) is 99% nitrate.

Hope this helps


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## glorycloud (Sep 30, 2016)

Can anyone tell me how dilute the sulphuric should be when cleaning the borax from a refined button?


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## Topher_osAUrus (Sep 30, 2016)

I do 10-25%, and let it sit overnight.

But heating it can hasten things.

Edit to add


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## glorycloud (Sep 30, 2016)

OK, if I do one part sulphuric acid and four parts water should that be dilute enough?


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## Palladium (Sep 30, 2016)

1 part nitric and 3 parts water heated will work to.


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## glorycloud (Sep 30, 2016)

Thank you!

EDIT - I don't have nitric just sulfuric right now.


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## Topher_osAUrus (Sep 30, 2016)

Yes, I'd imagine so Glory.

Also, borax can be removed by plain water.
It takes alot of heat and patience, but boiling water can remove the borax layer.

4Metals gave that advice to someone a few months back.

I always have sulfuric, and my nitric is precious to me, so I always opt for dilute sulfuric. If put on the hot plate, it can make quick work of the borax layer.


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## FrugalRefiner (Sep 30, 2016)

Barren Realms 007 said:


> If you can find one of Lou's original post's on his HCl washing method he tells that it he does it this way to remove the small amounts of silver chloride so that he doesn't have to deal with the ammonia wash. If I remember correctly!!!!


I provided a link in the second post in this thread. In it, he warns that going directly to a water wash can cause problems.  

Dave


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## glorycloud (Sep 30, 2016)

WOW - that post by Lou made my brain hurt. I'm a hobbyist at best and not a chemist. 8) 

In layman's terms, is Lou suggesting that the first washes of the precipitated gold
should be in muratic acid (HCL) followed by washes in water?


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## anachronism (Sep 30, 2016)

There is also another quick way. Heat it up (don't melt it of course) and drop it into cold water.


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## Topher_osAUrus (Sep 30, 2016)

glorycloud said:


> WOW - that post by Lou made my brain hurt. I'm a hobbyist at best and not a chemist. 8)
> 
> In layman's terms, is Lou suggesting that the first washes of the precipitated gold
> should be in muratic acid (HCL) followed by washes in water?



Correct


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## Shark (Sep 30, 2016)

I started using HCl for a first wash as Lou suggested a few months ago and the change was pretty dramatic. I don't really know why that would make such a difference, but it does.


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## Topher_osAUrus (Sep 30, 2016)

I think its because water can change the pH drastically enough(in the minute amount of acid in the powders) to reduce metals to their hydroxides, leaving impurities mixed with your perfect powders.


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## glorycloud (Sep 30, 2016)

OK, HCL first from now on!!


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## anachronism (Sep 30, 2016)

Ahh but this if where Frank's comment has come to the fore. Everyone has their own little tweaks. I boil my gold in water first as a wash before using HCl. 

I get 4 x nines verified by XRF so it works. 

Caveat: I am talking about a refine not a recovery drop. I still water wash first though even on a recovery drop.


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## Topher_osAUrus (Sep 30, 2016)

You rebel you..
8)


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## g_axelsson (Oct 3, 2016)

I can see the merits of washing with HCl as the first wash.

After precipitating gold we still have a lot of chloride ions in solution, this keeps the silver chloride in solution too. I assume any solid silver chloride is filtered off before dropping the gold.

Going directly to water in the first step will dilute the chloride ions to the point where silver chloride will precipitate. This fine chloride is possible to dissolve by washing in HCL in the following steps, but it will take more effort.

When doing the first wash with HCl the silver chloride in solution will be diluted and washed away with less effort than if it had precipitated first. Then when washing with water there is no more silver chloride to precipitate so there is no solid silver chloride that needs to be dissolved.

The same purity of gold could be achieved, but I'm convinced that doing the first wash with HCl and not water can only make it easier to reach high purity gold. The same result can be achieved with washing with water at first but it will require longer time or more washing. It is always easier to just wash away than to have to dissolve the silver chloride again.

Some numbers...
At room temperature 0.0016 g silver chloride is soluble in 1 liter plain water.
A 23% solution of sodium chloride dissolves 0.3 g silver chloride per liter solution.
Solubility in HCl seems to be about half of the solubility compared to a concentrated chloride salt solution.

Göran


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## anachronism (Oct 3, 2016)

Good point. Bear in mind you can't assume that one HCl wash is going to take away all the silver chloride that's in the powder. Often you perform the first HCl wash and as soon as you move to a water wash more silver chloride precipitates out. Especially if you are performing a recovery drop from a dirty solution that hasn't been diluted. Then again dilution is another topic entirely with many experienced members having individual approaches.

It's not a one size fits all solution, no matter which way round you choose to do it but it's good to understand the chemistry behind it so an informed choice can be made.


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## g_axelsson (Oct 3, 2016)

Of course, the amount and type of contaminant will affect the washing procedure.

As a reference here is the two original gold washing posts discussed...
Harold : http://goldrefiningforum.com/phpBB3/viewtopic.php?f=49&t=325&p=2620#p2620
Lou : http://goldrefiningforum.com/phpBB3/viewtopic.php?f=49&t=22328#p233671

As a bonus Lou's post included a link to an article with numbers of the solubility of silver chloride in HCL. The link might result in a strange filename, but once renamed to end with pdf it can be read in acrobat without problem.

Both Harold and Lou starts with HCl washes.

Göran


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## anachronism (Oct 3, 2016)

I'm not trying to re-invent the wheel Goran so don't worry I'm not going against the establishment or correct anyone


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## 4metals (Oct 3, 2016)

But don't forget to ice down the aqua regia before you filter it. The low temperature is where the solubility of silver chloride in the solution really drops down. If you filter the pregnant aqua regia while it is room temperature, some dissolved silver chloride will pass right through the filter paper. If you chill it, that same silver chloride is now a solid and can be caught on the filter paper. 

So the best approach is to get as much of the silver out as possible before you drop the gold.

One piece of equipment I always tell my refining clients to be on the lookout for is a used ice machine. Adding 2 pails of ice to 20 gallons of aqua regia before filtering really gets it cold and gets that silver out of solution where it can be filtered. 

I think taking advantage of solubilities of silver chloride through different temperature ranges will pay you back better than debating water first or Hydrochloric first.


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## Grelko (Oct 3, 2016)

4metals said:


> But don't forget to ice down the aqua regia before you filter it.



Would this be the same if you're working with HCl/Cl?

I'm guessing you would need "distilled water" ice cubes. Wouldn't want to contaminate the solution with tap water.


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## 4metals (Oct 3, 2016)

The bad actor in tap water is chlorine. Since both Aqua regia and HCl solutions already have plenty of chlorine, tap water is fine.


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## Barren Realms 007 (Oct 4, 2016)

4metals said:


> But don't forget to ice down the aqua regia before you filter it. The low temperature is where the solubility of silver chloride in the solution really drops down. If you filter the pregnant aqua regia while it is room temperature, some dissolved silver chloride will pass right through the filter paper. If you chill it, that same silver chloride is now a solid and can be caught on the filter paper.
> 
> So the best approach is to get as much of the silver out as possible before you drop the gold.
> 
> ...



Hence the reason I always do my filtering of 2nd refined gold with a charmin plug in a funnel filled with crushed ice.

Attention is in the details.


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## Grelko (Oct 4, 2016)

4metals said:


> The bad actor in tap water is chlorine. Since both Aqua regia and HCl solutions already have plenty of chlorine, tap water is fine.



Thank you, this should work for me, but if someone else is using water from a well, they might need to buy ice from the store instead.


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## 4metals (Oct 4, 2016)

Well water is not chlorinated in NE Pennsylvania and my well water can be used for nitric dissolves instead of distilled. Try out your well water, if it isn't chlorinated, or too hard, it should work fine.


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## glorycloud (Oct 4, 2016)

Well, she cleaned up nicely after "bath time" in dilute Sulfuric. 8) 



And the whole family after "bath time".  



THANKS everyone for the help and encouragement!!
What a GREAT forum!!


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## anachronism (Oct 4, 2016)

Ha! Result.

Well done Glory


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## Grelko (Oct 4, 2016)

4metals said:


> Well water is not chlorinated in NE Pennsylvania and my well water can be used for nitric dissolves instead of distilled. Try out your well water, if it isn't chlorinated, or too hard, it should work fine.



Thanks for adding more to this 4metals, We have city "tap water" here (Western Pa). I was just getting a bit more information about it, for other members that may be using a well.




glorycloud said:


> Well, she cleaned up nicely after "bath time" in dilute Sulfuric. 8)
> Au button 31.04gr 10-4-16.jpg
> 
> And the whole family after "bath time".
> ...



Nice clean up on the button glorycloud, looks great  When I saw the first picture in this thread, I thought it looked like a marble counter top (I'm not trying to be rude, since I haven't gotten over .908 yet. I need more practice)


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## glorycloud (Oct 4, 2016)

That's why I was so disappointed with this last button at first because I knew how
hard I had worked on all the washes to attain a nice quality refined gold. 8)


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## 4metals (Oct 4, 2016)

> We have city "tap water" here (Western Pa). I was just getting a bit more information about it, for other members that may be using a well.



I know guys running large silver cells who do not buy distilled water but treat tap water with silver nitrate. The silver nitrate forms silver chloride and takes the chlorine out of the water. And since they are using it in silver cells, silver nitrate is not an issue. But you need to let the silver chloride settle out and take off the top dechlorinated water. Every once in a while you need to clean out the silver chloride and reduce it to recover the silver. 

This does not work with public water supplies chlorinated with chloramines. If you use a lot of distilled water it is worth a try on your public water supply for water used to cut nitric to digest inquarted gold. You can call the water authority and see if they use chlorine bleach or chloramines.


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## Barren Realms 007 (Oct 4, 2016)

glorycloud said:


> That's why I was so disappointed with this last button at first because I knew how
> hard I had worked on all the washes to attain a nice quality refined gold. 8)



I know I give you a hard time but it is all in fun and you know that after the years we have traded back and forth on stuff.

I am very proud of the results to have learned to obtain in your processing and the quality of the pipes are increasing as you learn.

Keep up the good work. and keep pooping out the grand kids. :mrgreen:


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## glorycloud (Oct 4, 2016)

Thanks Frank!


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## johnny309 (Oct 6, 2016)

glorycloud said:


> Actually, I use pretty fastidiously use Kurtak's wash procedure. It just
> seems like when I am removing the buttons from the dish with the steel
> needle nose pliers, something flashes across the face of the button but
> it all happens so fast that I can't be sure.
> ...




This was the sentence that maybe had the key....
The bottom seems to be fine...only the upper side...is contaminated.
Could it be from pliers....Ni or Cr plate ...on high temperature electrons migrate.


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