Howdy, help please,purple powder created

[jonn]

Hi, i dissolved 2 lbs of gold plated pins in nitric 67% and am left with gold flakes in purple powder. Any clues on what the purple powder is??

 

[jimdoc]

Gold.
Was there solder on the pins?

Jim

 

[butcher]

probably tin from solder, tin and HCl make stannous (tin) chloride, will turn violet with gold we use it for testing gold.

 

[jonn]

May be Tin, How does one get rid of it

 

[jimdoc]

Don't get rid of it until you are sure it is not gold.
Somebody will give you better advise than I can
give you. I had a whole bucket load turn purple on
me years ago and I ended up with 8 grams of gold
out of the purple mess. I think I got some solder or
tin mixed in to create the mess, I think it was a
batch of processors. I haven't had it happen again
since I learned what I have from this forum.
But I learned for sure that gold can look purple.
Jim

 

[Oz]

Tin in HCl can give you purple colloidal gold. However he said he was using 67% nitric and that leaves me at a loss as to the purple color he is seeing. By the way, tin in nitric gives you a gelatinous goo if in any quantity.

 

[butcher]

maybe I should read all the words before opening my mouth, was the nitric homade?

 

[Harold_V]

Simple to process.

Incinerate to redness, making sure you eliminate any carbonaceous material that is present (like filter papers). Include everything in the incineration and screening process. Screen well, grinding any lumps (mortar & pestle) so they can pass through the screen.

Wash the resulting material with HCl, heated. Allowing it to boil (use a watch glass) is a good idea.

Rinse well, until the rinse water is clear of color. I suggest you decant, not filter. Leave the solids in the container (beaker).

When you have decanted the final time, dissolve the values, and filter the solids, adding at least one rinse cycle. More is better. They should end up a cream color, and should filter well, thanks to the HCl wash and rinse cycles.

I suggest you do not discard the residue, which will still contain traces of values. If you choose to discard them, add water and stir well, allowing the solids to settle. Do this until the solution shows little or no signs of values. The solution should be processed for contained values.

Harold

 

[jonn]

Thank you all for your help, nitric is Not home made, the powder is consistent with no lumps and ran through a sep. funnel so there is no filter paper. I will try the hcl as mentioned , boiling, watch glass, pretty sure its tin now. Also, would rinse with H2o raise Ph enough to drop other metals and if so, would the HCL rinse those away? Thanks 8)

 

[shadybear]

Thank you all for your help, nitric is Not home made, the powder is consistent with no lumps and ran through a sep. funnel so there is no filter paper. I will try the hcl as mentioned , boiling, watch glass, pretty sure its tin now. Also, would rinse with H2o raise Ph enough to drop other metals and if so, would the HCL rinse those away? Thanks 8)

Dont forget to incinerate like harold said to do. Do it first, doesnt have so much to do with the filter paper as it is to remove the nitric chems and probably does other stuff. But I have noticed color changes when i do it and the hcl wash after you incinerate will work much better.

 

[Harold_V]

Thank you all for your help, nitric is Not home made, the powder is consistent with no lumps and ran through a sep. funnel so there is no filter paper. I will try the hcl as mentioned , boiling, watch glass, pretty sure its tin now. Also, would rinse with H2o raise Ph enough to drop other metals and if so, would the HCL rinse those away? Thanks 8)

Dont forget to incinerate like harold said to do. Do it first, doesnt have so much to do with the filter paper as it is to remove the nitric chems and probably does other stuff. But I have noticed color changes when i do it and the hcl wash after you incinerate will work much better.

The entire process will lower unwanted residues, but most importantly, you'll recover values, and the solution will be amenable to filtering,which it, otherwise, likely won't be. DO NOT ELIMINATE THE INCINERATION PROCESS. It is important that you follow these instructions. Do not pick and choose that which appeals to you. If you had enough experience to do that, you wouldn't be here asking questions.

Harold

 

[jonn]

Thank you Harold and all others for your help. I tried what you told me on a split batch. Test #1 was not incinerated, it yielded 1.3g which had to be mechanically brushed to remove the layer of junk but it looks real pretty now. I will try test #2 and post results with incineration included.

 

[Harold_V]

Thank you Harold and all others for your help. I tried what you told me on a split batch. Test #1 was not incinerated, it yielded 1.3g which had to be mechanically brushed to remove the layer of junk but it looks real pretty now. I will try test #2 and post results with incineration included.

Blink! Blink!

Mechanically brushed? The gold button?

Something is woefully wrong.

When you process gold properly, including doing the incineration, washes, dissolving of gold, filtering, precipitating, and then using a good procedure to wash the resulting gold, it requires nothing aside from melting, and even that requires almost no flux. After melting, a boil in very dilute sulfuric is generally all that is required.

You may wish to rethink what you're doing, depending on your objective.

Harold

 

[jonn]

Hi,Harold and thanks for your reply. I'm not too sure about how all this stuff works in respect to refining , but i've been at it for quite some time with NO LUCK and lots of frustration. I'm trying to refine mostly pins and fingers from pcs. I usually start with a nitric bath, filter and wash with water.I've not had much luck with the Aqua Regia as of yet.I have used Urea in the past and SMB to precipitate. Nothing seems to drop?!? I would GREATLY appreciate any direction you might suggest.You could PM me if you'd like. Thanks again.

 

[Harold_V]

What you're doing is closely related to the teachings of Hoke. I strongly recommend you read her book and concentrate on the use of AR, plus how to evaporate. I hesitate to take this off the list for a couple reasons. One of them is that there are others in the same position, so by keeping it public, there's a chance that others will learn, too.

If you are failing to recover gold from AR, the chief cause is that you have free nitric present. Until you eliminate the nitric, you'll struggle. You can do that a couple ways, neither of which include urea. Frankly, I wouldn't use the stuff, and never did in all my years of refining.

By using controlled amounts of AR, you can dissolve your values and not have much, if any, nitric to expel. Assuming you do have an overage, one of the fastest and easiest tricks you can use is to consume it with more gold. I routinely added a button of gold to my individual lots for that very purpose. If you weigh the added metal both before and after, you can easily determine how much you've added to the lot. This can serve to teach you how much acid is needed, for future lots, plus it permits a fast elimination of the free nitric, for you need not evaporate to near dryness.

If you read Hoke and still have problems, ask again.

Harold

 

[jonn]

Thank you Harold. Im in the process of reading Hoke and have realized lots of things I have forgotten. I read her book last year and have been struggling with this for a long time.Maybe its my medication, i forget alot if its not written down. I tried Inquartation and parting today. Boiled with water, boiled with hcl,boiled with water, boiled with hcl again.I still need to boil with ammonia and water. Question; what i have now is a white powder, Is that gold?!? Wow, i must sound like an idiot, but i refuse to give up.I have about 300 ml of this powder, its heavy and falls fast after boiling. Seems very pasty and sticky. I've been spending lots of time on this site in the past few days and learned quite abit. Its amazing how much info there is, and its all good. Thanks to you and GSP, Palladium, Lasersteve, and all the folks who contribute.I recently became disabled and this field is about the only thing that has my interest peaked, so Thank you.By the way , you make some incredible machines. I saw the filter press and ball mill; Outstanding! I would love to make those for my shop.Thanks!!

 

[Palladium]

I recently became disabled and this field is about the only thing that has my interest peaked.

Welcome to the forum John. I know the feeling. There was a time in the not so distant past that i to found myself in your position. Matter of fact that is the whole story was to the how and why of aflac. I can only say that there were many of days, and i do mean many, that had i not had this new found interest in the field of refining, this forum, or the wonderful support of all it members. I probably would have just lost all drive and interest in life period !
Had it not been for a very unfortunate turn of events in my life i would have totally missed one of the best adventures of my life as it plays out here on the forum.

I mean why just today Lazersteve taught us all how to make tea. Who would have ever thunk it. lol ( just kidding Steve )

 

[jonn]

That's right palladium, it an awesome site. I totally understand now that life takes different directions, but it always seems to work out. I get to spend alot more time with the kids and that is priceless. By the way, I love tea. Its easier to make than gold though, that's for sure. Funny how we become domesticated, no matter how hard we resist.Pleasure meeting you.

 

[butcher]

keeping the mind alive and vibrant, can help to keep the body alive,and healing.
stress and depression will kill mind and body.
not only great people to communicate with and learn from, but this forum is proving to be good medicine. 8)

 

[jonn]

Thank you butcher, you're absolutely right. I cant help but think i need to buy an atomic absorbtion machine. I created some pretty cool stuff during these trials of refining. For instance, what in the world is white,powder,looks like marshmallow cream. Actually want to lick the stuff, not really but it does look interesting.Its very creamy and heavy.Very thick not like honeycomb but almost looks like solid metal but its powder?? :shock: