Howdy, help please,purple powder created

Gold Refining Forum

Help Support Gold Refining Forum:

This site may earn a commission from merchant affiliate links, including eBay, Amazon, and others.
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.
 
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.
 
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).
 
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.
 
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.
 
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.
 
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
 
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!! :p
 
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!! :p
Ok Im not a scientist or anything but the white powder might be silver chloride.Also if you haved used any urea this white slime paste stuff can accour best never to use urea in a solution that contains any gold best to use up any free nitric acid with more pure gold in very thin sheet form or boil to almost dry add distilled water only use distilled water by the way boil add boil almost dry a few times. Add more distilled water boil but leave a good amount of water in the gold bearing solution filter then percipatate ,let settle ,decant, rinse, sevel times, then boil in nitric acid, the percipate make sure to rinse every molicule or nitric acid out then boil in sulpheric acid rinse very well then boil in ammonia rinse well place in crusicble a little very little borax melt and done sorry about my bad spelling good luck hang in there practice makes perfect

That's darn good for a first post. Welcome to the forum?
 
Palladium said:
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 )

Just remember: It takes a Village to make an Idiot. :mrgreen:
 
Irons said:
Palladium said:
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 )

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

I'm glad you're doing better. :p
 

Latest posts

Back
Top