# Howdy, help please,purple powder created



## jonn (Jan 14, 2010)

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??


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## jimdoc (Jan 14, 2010)

Gold.
Was there solder on the pins?

Jim


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## butcher (Jan 14, 2010)

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


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## jonn (Jan 15, 2010)

May be Tin, How does one get rid of it


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## jimdoc (Jan 15, 2010)

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


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## Oz (Jan 15, 2010)

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.


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## butcher (Jan 15, 2010)

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


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## Harold_V (Jan 15, 2010)

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


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## jonn (Jan 15, 2010)

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)


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## shadybear (Jan 15, 2010)

jonn said:


> 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.


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## Harold_V (Jan 16, 2010)

shadybear said:


> jonn said:
> 
> 
> > 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)
> ...



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


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## jonn (Jan 16, 2010)

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.


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## Harold_V (Jan 17, 2010)

jonn said:


> 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


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## jonn (Jan 18, 2010)

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.


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## Harold_V (Jan 19, 2010)

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


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## jonn (Jan 19, 2010)

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!!


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## Palladium (Jan 19, 2010)

jonn said:


> 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 )


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## jonn (Jan 19, 2010)

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.


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## butcher (Jan 19, 2010)

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)


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## jonn (Jan 19, 2010)

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:


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## butcher (Jan 19, 2010)

Alkind of sounds like silver chloride cottage cheese, 
white powder can be several metals or a combination of metals,
Chlorides are usually Copper (I), Silver, Mercury, or lead, all insoluble as chloride salts in water or dilute acid solution,copper (I) would be soluble in slightly acidic solution, and of coarse if the more noble metals were present they can be mixed with these would be insoluble.
these chlorides can be seperated and tested.
a good test to see if you have a chloride solution would be to use silver nitrate solution, if chloride was present it would precipitate a white silver chloride, as either a creamy solution or as white cottage cheese,
say you have white powdered chlorides and you want to seperate them and test, adding a dilute say about 6M solution of HCl and water, if copper the solution will turn blue to green, in cold solution, and decantingand repeating till solution clears somewhat would leave mostly the silver, mercury or lead.
(I say mostly because I believe the crystal structure of these chlorides is hard to seperate, as I think as crystals grow they do not neccasarily grow of one metal but more valuble metals may be locked up in the crystal, and without completly dissolving and seperating them they may stay locked together, just washing the outside of the crystal or disolving the outside layer of the crystal may not ever seperate them completely, also I feel if I can see it in solution and it will precipitate it is a crystal salt made up of many atoms, and possibly different types of metal atoms unless this was the only pure metal in solution), not sure my explanation here is understandable.
now AgCl, Hg2Cl2,PbCl2, insoluble in cold dilute HCl/water solution,
but heating and the lead chloride becomes more soluble, so by boiling this solution giveng time for insolubles to settle while keeping hot but not aggitated the lead chloride will dissolve into solution, and can be seperated by decanting, now if allowed to cool they would grow crystal powders of lead chloride again, a test for lead cloride is pottasium chromate with lead will show bright yellow precipitant.
the Hg2Cl2, and AgCl white cloride powders are insoluble in this dilute solution,now if we added Ammonia (caution never let this solution dry it can form dangerous shock or temperature compound, Always remove silver by acidifying solution with HCl, to precipitate silver and making solution into ammonium chloride), ammonia will dissolve silver into solution as Ag(NH3)2, and by adding HCL will precipitate white silver chloride powder (white cottage cheese), the white Hg2Cl2 in ammonia changes to gray-black precipitant of HgNH2Cl if it was ever present to begin with.
I don't know if this will answer your question or not. but hope it helps.


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## jonn (Jan 19, 2010)

Thanks Butcher, that helps alot. That all makes alot of sense, which is why im confused?! I inquarted gold with sterling silver. Beaded in water. Boiled in 70% nitric. I had black mud left.Decanted into another beaker( a seperatory funnel), washed with water at a boil, decanted, washed with hcl, decanted, washed with water, decanted again. Now what i have left is the original beaker with washes and decants with a white powder i was telling you about. The sep. funnel has silver nitrate, i diluted slightly and stuck a rod of copper in it overnight. It dropped silver.That solution is in another container for the meantime with the silver on an evap dish. Ok now, the HCL wash solution is in yet Another container, it tests like mad for gold and palladium. Super dark purple black and a nice vibrant Yellow. Now back to the reaction flask. Washed and have white powder. I will read your post again and again, im sure im missing something.Is it possible that its AuCl?? Should i dry and try a melt in my dish?? oh boy,Thanks again.


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## butcher (Jan 20, 2010)

gold can make a white powder but it is extreemly rare, more likely silver, and possibly some gold mixed in (or any other insoluble metal), an ammonia can dissolve the silver, and not the gold, if in solution, (but if any PGM, they can also make a complex with ammonia), (but if these are chloride powders any Pt would precipitate from ammonium chloride formed),

also some of these chemicals can form NaCl table salt, depending on process used, what is nice about table salt is it will dissolve in water, and if no other metals will be fairly clear, I could also use the silver nitrate to test and see if it was salt, when added to silver nitrate my test solution will precipitate the familiar silver chloride white cottage cheese ( or at least make a milky solution if not enough salt to make precipitant).


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## jonn (Jan 20, 2010)

Thanks again butcher, i dont think its salt. every step was boiled and upon adding some to my silver nitrate it simply made a white layer on top. that was an accidental experiment. i used a baster to pull water out and spilled some in my silver nitrate. Why is white powder gold so rare? You says its possible but not likely. Do you think i should try and melt a sample? I have about 60 grams, only thing is, i dont want to poison the air if it is lead.I cant imagine where the lead would come from or why it wouldnt dissolve in nitric or hcl at a boil though.


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## jonn (Jan 20, 2010)

By the way, the solution after boiling and settling was yellow with a faint fluorescence of green. Stannous chloride on that liquid is purple, black,yellow orange and slightly pink.Darn.


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## butcher (Jan 20, 2010)

Jonn,
I am not exactly sure where you are with these powders, and I am somewhat confused as to exactly what you have done to get them, 
Have you incinerated them? If not you can have lead and tin from solder, these two metals will give trouble,
Lets start from the beginning with these powders. Here is a way and I'm just assuming a mix of metals. If doing this don’t skip steps. Or rearrange orders, until you know why
Lets boil them in hot water, note color of liquid formed. Filter all. of the decanted solutions, test any liquid for values.
Then lets let them settle well, maybe overnight, 
Carefully remove water solution; I use a suction bulb then eye dropper type tool,
Now lets cook these powders slowly bringing up temperature till dry, then raise heat, these salts may melt to syrup, and bubble, we will raise heat as needed till dry again at high heat, I use a brown glass Pyrex skillet (on a hot plate with cast iron heat plate), once these powders are dry and heat high and smoking of gasses stop I use propane torch and burn the powders, till they glow red hot, crushing lumps in air, until there is no smoke keeping them red hot in air so any metal that can will oxidize, let them cool,
Now that we have oxidized any base metals, and drove out any nitrates or chlorides from these powders,
We will assume they have lead and solder tin in them.
Lets make them into chlorides first, cover them with HCL, we wont need a whole jar just enough to cover powders, add a few squirts of water to wash down sides of container, this little bit of water will also keep chlorine gas somewhat in solution, I sit this in warm place stirring well any lumps. Let sit in this warm place soaking, after good warm soak lets Dilute with lots of warm water, let settle well again till solution whatever color is clear, this color now can tell you if you had copper, blue or greenish, the solution may also contain any tin you may have had, and maybe some of the lead, we will decant this solution and test it for values, the powder would contain lead, some tin, silver, gold and possible PGM, (of coarse I do not know what yours contains, just play along here),
Now we have chloride salts, let’s rinse them let settle decant.
Now lets boil these in water to get the lead chloride soluble, get the powders to rolling boil, then turn down heat, keeping solution just under a boil, but letting any powder that is insoluble settle, and the solution hot to keep lead chloride soluble, decant the hot solution to another container let lead chloride cool to salt, if much lead repeat this till lead removed as much as possible from your values, now that we have removed as much tin and lead from these as we could with these processes lets rinse and settle and decant again, and incinerate these powders as we did before, roasting them red hot to eliminate any chlorides from them, now that we got this far we will give them a wash in 70% nitric with equal volumes of water, now since these are powders and may be very reactive to nitric I would cover the powders in water, add my nitric solution a little at a time, waiting for reaction to finish before adding any more, one there is no more reaction with new additions, lets heat this solution, and powder, but not too hot, we don’t want to drive our nitric from solution, now lets let this sit again to settle, this nitric should dissolve any base metals, silver, if Palladium, (and possibly some platinum if it was alloyed with silver), we will decant this well settled solution from powders, powders may contain gold and possible platinum group metals. This solution we will use HCl to precipitate silver as white chloride cottage cheese, let settle overnight decant and then use copper bar to check for Pd etc,
The powders insoluble in nitric we will dissolve in Aqua regia, adding just minimum nitric, we don’t need a whole jar of acid for a small amount of powder, and by using minimum nitric we will have less trouble later, and using heat here also helps to dissolve these metals, and keeping our acid use low, now we have these dissolved we will heat them at a higher temperature evaporating off liquids till we get a thick syrup, adding HCl to wet again, evaporate to syrup again, wet with HCl again, evaporate to syrup one more time,(add a couple of drops of sulfuric to make any lead into sulfate), add at least 3 times or more volumes of water, let settle, any silver or lead chlorides will form as white powder, add a little HCL see if any more silver chloride forms, if so let settle, overnight is best, now decant and filter this solution of liquid gold and possible PGM, making sure it is clear colored solution free of sediments or muck, now we can add our chemical to precipitate gold (sodium metabisulfite or ferrous sulfate or whichever we use), (note the ending of these names ite and ate). If using sodium metabisulfite we will smell SO2 gas and our bright yellow solution will turn brown and precipitate gold, we will let settle well and decant, washing these powders to Harold’s instruction's, 
And if we had PGM's we would concentrate solution go after them with ammonium chloride for Pt, and sodium chlorate for Pd.


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## jonn (Jan 20, 2010)

Hi Butcher, Thanks again. I will do as per your instructions, it will take a couple days im sure but well worth it. Will post results once complete. Thanks and thanks Harold as well. Talk with you soon. Jonn


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## Anonymous (Feb 15, 2010)

jonn said:


> 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!!


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## Barren Realms 007 (Feb 15, 2010)

palladium pro said:


> jonn said:
> 
> 
> > 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!!
> ...



That's darn good for a first post. Welcome to the forum?


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## Irons (Feb 16, 2010)

Palladium said:


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



Just remember: It takes a Village to make an Idiot. :mrgreen:


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## Platdigger (Feb 16, 2010)

Hahaha..... leave it to you Irons.. :lol:


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## Irons (Feb 16, 2010)

Irons said:


> Palladium said:
> 
> 
> > jonn said:
> ...



I'm glad you're doing better.


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