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WallaceFish

Member
Joined
Apr 23, 2012
Messages
22
Location
Felton, DE
Using AR method, 100g of alloy + 300ml HCl + 50ml Nitric added until no more recation. Let it settle overnight (very dark green solution). Lots of grey matter accumilation at the bottom. Filtered that off with some chunks of alloy left over. Next, had only good clean filtered, dark green solution. Dissolved 5g SMB in distilled water, added to filtered solution AND... precipitated more grey matter. Last time, I used the EXACT same method but got Au with SMB addition. Now it seems I am getting AgCl but that doesn't make any sense to me. All that should have dropped out while cooling overnight PLUS the material was low in Ag. If gold content in feedstock is very little, will this be difficult to recover?
 
AgCl will precipitate from AR solution when it cools AND when its diluted. use salt to remove the silver first and it shouldnt effect your gold drop.dilution using ice helps the silver chloride settle but even at that, there will still be silver in your gold. dont forget the washes and rinses to remove the silver from your gold powder.
 
at least double the volume, even triple the volume wouldnt be too much as you can always evaporate water.
 
would my addition of SMB have had any adverse affects on the process? meaning i added smb... got nothing. dilluted and filtering again. recommend next step please?
 
Before filtering, I've diluted by adding 3 parts tap water to 1 part AR for 40 years with excellent results. You have to understand that AgCl is slightly soluble in strong AR. If you don't dilute it (or, use ice to chill it) before filtering, it will precipitate mainly when you dilute it by rinsing the inside of the container into the filter. Even a very small addition of water will precipitate some AgCl from strong AR, which could end up with the gold. To me, it's easier to get the silver out early than it is to get it out later.

What sort of "alloy" are we talking about? Karat gold? What karat? Approx. what percentage of the metal didn't dissolve?
 
majority of the shot I made was GP junk. I am not even sure it was gold at this point. Along with it was some 14k stuff. As for the inner base metals of the GP material it was soft and gray like Pb but not as heavy. All together it made about 600g of shot. I only ran 100g as a "test run". I cant imagine there was that much Ag in this stuff. Im probably wrong though. After AR was spent, there was a lot of gray mud (AgCl I am guessing) and about 15-20 percent of the material left over but NOT untouched. It got beat up pretty good. It basically crumbles in your fingers. Stannous test is yellow but I am sceptical of my stannous solution. My chems are as follows:

HCl ACS reagent 37%
Nitric ACS reagent 70

Edit: Okay, I found the culprit. I threw in some watchband links and they are loaded with silver and steel. Looked at some samples under the scope. So, now that I have determined that I am overloaded with silver. Now what?
 
Ok Pub, thanks a bunch. I got blindsided there. Just out of curiosity and for future reference, what does adding salt do exactly? I also wanted to mention but forgot earlier, I added dissolved SMB. When that did not work, I added dry SMB and it instantly fizzed and turned brown then dissapeared. Whats that all about?
 
WallaceFish said:
Ok Pub, thanks a bunch. I got blindsided there. Just out of curiosity and for future reference, what does adding salt do exactly? I also wanted to mention but forgot earlier, I added dissolved SMB. When that did not work, I added dry SMB and it instantly fizzed and turned brown then dissapeared. Whats that all about?
Click to expand...

table salt is Sodium Chloride. the chloride in the salt reacts with the silver nitrate to create silver chloride.hydrochloric acid is another source of chloride, same principle.

if you put dry SMB in the solution and it fizzed, it means you have free nitric in the solution. thats the reason the SMB failed to drop the gold. you have to remove this free nitric so the SMB can do its job.
 
50 mls of nitric for your AR solution, but only 5 g SMB?

Those ratios are way off. If you needed 50 mls of HNO3, then you would have had over 100g gold (off memory. I'm traveling and don't have my spreadsheets with me). And 100g gold requires about 100g SMB to drop it.

Either you've not added enough SMB, or you used (and still have) way too much nitric.
 
Well having read this thread I can see major problems ahead. By melting all this material together you have created a headache to deal with, there could be a real mix of base metals including tin and this will be a nightmare if it's in your AR. There are thousands of posts and threads on how to deal with various types of scrap, recovering the gold or values and removing base metals, this for most scrap is mandatory. Now you have a mix I'd suggest cementing your values on copper sheet and test the solution to make sure all values have been recovered, stannous here is your eyes, put the recovered values aside, seal and keep somewhere safe the solution and start reading.
Start with C.M.Hoke it's available as a free download off many members signature lines, read the safety section here on the forum and the forum handbooks again free,visit our very own Lasersteves site and watch and better buy his videos, this might not what you want to hear but I highly recommend you do what I suggest or else your refining experience will be a very frustrating and troublesome one.
 
Nick, I pretty much covered all of the literature you mentioned. I am using the lab I work in, so I am extremely familiar with lab safety protocols. I wont accidentally be making any fulminates. As for Hoke's "bible" I have that covered. Maybe parts I misunderstand, but none the less I do have a biology degree that required some chemistry to obtain. In other words I would consider myself slightly more advanced than those that just "throw it in acid and see what happens". The things I am NOT familiar with: Identifying metals that look similar i.e. gold/brass, silver/platinum, tin/lead and so on. So I may have melted in all these metals not knowing there was tin involved in the process. Like I said, I cant take a piece of jewelry, look at it, and tell you what is there. I can see on the outside there is gold... A watchband has stainless steel and so on, but break it and look in the center... I don't know. Nickle? LOL And what is stannous powder supposed to look like? I have a small 10g jar but it is difficult to dissolve in HCl hence I am sceptical of its "authenticity". My next move will be to send pictures of what I am using as feedstock so you guys can see exactly what I'm dealing with. I think may get y'all closer to target.
 
Wallace,

I tend to agree with Nick, but you need to have some stannous to see where you are. Right now you're running blind.

I have pure tin metal I can send you. With it you can make some good stannous chloride test solution. Send me a pm.

The mistake you made was dissolving a bunch of metals in ar without even knowing what you had. You also, apparently did not dissolve base metals prior to the AR step with nitric acid. Skipping this step is a critical error.
 
Eric, did you read the whole thread? That is not what I did. I performed the same tasks as I previously performed with positive results. So based on prior success, I duplicated that process. So if we think scientific method here, and use the fact that I got Au from what I did last time as a controll, it tells me that the problem lies not so much in the methodology, but in what I used (meaning the feedstock). So no. I did not blindly take a bunch of metal and immerse in acid just to see what would happen. I had an idea of what I would expect to see based on past experience. As I am sure you know, there is a learning curve to this discipline, of which I am currently at the low trajectory of. It is my desire through a number of channels, including trial and error and this forum's members, to gain a realatively high level of understanding of this "refining discipline". I have joined other forums on other unrelated subjects which harbor those that leap into a given venture with no knowledge of the matter and just seek "free answers". I am sure "those" show up here. I take science very seriously as I am a scientist by trade. I would very much appreciate to NOT be lumped in with one of "those". Things aren't always what they "seem".

Lobby, I greatly appreciate your offer. Before we decide to take that approach, I have some things here that I suspect are fasioned from tin. Is there any way that I can confirm this? In the future, I will adjust my methods to comply with standards of success. My understanding of the processes is evolving all the time which is basically what I am trying to convey to Eric above. To clarify, I was under the impression that all base metals along with PM's are dissolved and when SMB is added, it reacts with and ONLY with Au at atomic level, forcing it out of suspension and back into solid state. I now stand corrected. I am sure it states this in the book and on this site, but I am the type that learns more by way of both text and experimentation in laboratory setting. So dealing with these problems are more like an excersise to me rather than a total XXXX-up. Thank you to all who have contributed. I truly am grateful of this resource and I look foward to learning from you all. If ever any of you are interested in fisheries management practices, fish ecology, stock assessment biology or policy thereof, I would be more than happy to return the favor. Maybe we can divulge a way to refine the mercury out of a fish or something like that. LOL
 
test solutions whether its gold or PGM's (platinum group metals), is covered in ms. Hoke's book. how to make and store and use them. stannous chloride test solution is the simplest of the lot. it is tin dissolved in hcl. it doesnt have to be pure tin, but it cant be contaminated with precious metals either. lead free solder is a good source of tin to make test solution.place a few grams in a glass bottle and add 100 ml's of hcl and let it sit overnight.be sure to keep a piece of undissolved metal in the solution to keep it active.
 

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