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kjavanb123

Well-known member
Joined
Apr 1, 2009
Messages
1,746
Location
USA
Hi everyone

Hope all is well. The same seller who brought had brought me vitnage sparks plug, gave a few components he had removed from a telecomm box he had purchased as scraps.

He had already done similar contacts using lead smelting but wanted to do them cheaper using chemicals.

The following are 4 different samples which he gave me and wanted me to process each sample separately and report its yields.

So please kindly post their correct techniccal names if you know them.

Sample 1
I divided it into two sub samples, one long stainless steel looking one and brass looking pieces.

There were total of 6 brass looking samples and and many more of stainless steel looking (as it turned out, it only looked like stainless steel, wheb it dissolved in nitric acid the color was copper based alloy, maybe bronze)

IMG_0496.JPG

Upon close inspection under a lope, there were two tiny contacts which supplier claimed to be Pd, at one side of the sample 1. Here is a closer look,
IMG_0497.JPG

Here is the bronze / brass color sample,
IMG_0498.JPG

Here is a closer look at the contacts on one side of the tips, according to the supplier, these two sub samples were connected together.
IMG_0499.JPG

More in the next post.
 
Here are photos of the other samples, which shared similar contact points as the the first sample.

Except the sample 4, which according to visual inspection, supplier claims and test showed gold, palladium and possibly one other PGMs.

Sample 2
IMG_0500.JPG

Sample 3
The line which contacts were attached to the end of it on this sample was a lot shorter than other ones
IMG_0501.JPG

Sample 4
IMG_0502.JPG

More next post
 
Supplier had asked me to test the sample 4 as he claimed it has gold in the contact.

So here is the sample 4 broken down into its parts.
IMG_0488.JPG

Here is a close up of the 8 pins at the bottom of the above picture, under a closer look you can see some of the contacts have a yellow tint.
IMG_0489.JPG

I used scissor to remove the part of pins thaf contacts were attached to.

Total cut parts weighed 1.60 grams. Dissolved them in dilute nitric acid, as you can see solution turned green and reaction with nitric was pretty fast, so the based must have been an alloy of copper.
IMG_0492.JPG

Here is what was undissolved in nitric acid, here is some pieces of gold foil and some gray color foils which can either be aluminum or Ir or Pt.
IMG_0491.JPG

Next post I processed the palladium nitrate solution from processing sample 4 contacts
 
Here is the green solution after adding 5.85 g of DMG dissolved in 4 grams of NaOH which had already mixed in 100 ml distilled hot water.
IMG_0493.JPG

Upon filtering and washing the color of participant didnt change, so I cemented it with zinc powder and HCL, here is the final undissolved palladium black from sample 4 contacts.
IMG_0495.JPG

It is being dried, as I had weighed the filter paper and it weighed 1.01 grams. Once it is dried weighed I will know how much Pd from that one sample 4.

Amount of gold and unknown foil is so small that I am not able to weigh.

More results in 10 hrs

Thanks and best regards
KJ
 
So ...I read wrong,or maybe not....from 0.16 grams of contacts ..you have 1.01 grams of powder?
That's magic.
That seems to me like an average relay contact point of relays used in 70' in telecom industry.
If you can provide an type of it ...serial....can be identified.
by the look of your picture and your solution is Pd/Ag ...30/70 alloy...speed in HNO3 diggestion and the green colour.....and Au flash...5um in thikness....but tear down by age....
If you drop with Zn.....Cu will drop too....this is why you have that much powder.

P.S.: why ...NaOH involved in this?.......Why do you have to raise the Ph ....nitric is allready spent dissolving metals and forming salts...
 
johnny309 said:
P.S.: why ...NaOH involved in this?.......Why do you have to raise the Ph ....nitric is allready spent dissolving metals and forming salts...
DMG is weakly soluble in water unless the pH is high, read Freechemists post about it at:
http://goldrefiningforum.com/phpBB3/viewtopic.php?f=48&t=9477
So the NaOH is used for dissolving the DMG and that solution is then used to drop the metal.

http://goldrefiningwiki.com/mediawiki/index.php/Dimethylglyoxime

Göran
 
johnny309 said:
So ...I read wrong,or maybe not....from 0.16 grams of contacts ..you have 1.01 grams of powder?
That's magic.
That seems to me like an average relay contact point of relays used in 70' in telecom industry.
If you can provide an type of it ...serial....can be identified.
by the look of your picture and your solution is Pd/Ag ...30/70 alloy...speed in HNO3 diggestion and the green colour.....and Au flash...5um in thikness....but tear down by age....
If you drop with Zn.....Cu will drop too....this is why you have that much powder.

P.S.: why ...NaOH involved in this?.......Why do you have to raise the Ph ....nitric is allready spent dissolving metals and forming salts...

Hi

I do not have that information about make and model of the telecomm main box.

Actually I made mistake it was 1.60 grams and changed that here. My scale can show 0,01 g and up.


I dropped Pd using DMG, and according to members with more experiene, that NaOH in the DMG mix, precipitates other metals but since more acid is there they get back to to solution and only Pd salt remains.

In sample 1 no silver was found.
 
Thank's
Göran

The idea was that he follow the exact numbers from Wikipedia...aka 100 ml of water,5.81 grams of DMG and 4 grams of NaOH....and his beaker has under 50 ml of solution.
This is an standard test solution....methods for dropping PGM from solutions are others...less expensive.
When he failed....he put Zn in the solution....create more mess....and get back to the square 1....meanwhile loosing time and consuming DMG....and finaly...not a clear result of the metal alloy from those contacts.
I agree that GRF is loaded with information and helped many people....
This why I have to point it out that he is doing it wrong.
 
Could you please point out what is wrong with my procedure?

I have used the same DMG formula before, freechemists also provided very similar if I correct his was using 2.5g of DMG per 100ml of 4g of lye.

Zinc cementing the DMG Pd salt is also a method of choice for converting Pd yellow to Pd metal, and it causes a lot less losses than calcining.

I am drying and weighing the final Pd powder from processing samples 1, and 2-3 and will post them here.

Best
KJ
 
Drop with Zn?
Not providing free Cl- ions to an metal to form an ZnCl2 mix...the Zn will drop like an black powder.
So.....is this black powder PGM?

Put the black powder in an beaker and add HCl...and cover it...if is Zn...will release H2....and in a fast way.
 
Finally after drying and weighing the powder, rrcovered from contacts of sample 1 stainless steel looking and brass looking pins,

Total of 0.460 grams of Pd powder was recovered.

Sample 2 and 3 are being dried.
 
Hi

Total Pd powder recovered from sample 2 and 3 contacts, which were cut manually, weighed 0.4 grams.

Total weight of sample 2 and 3 cut contact points were 1.17 grams.

There were 0.18 grams silver chloride, and 0.07 grams of meta stannic acid also produced from these two samples.

Best regards
KJ
 
Supplier had also gave me a piece of wire for testing, here is a photo of that.
IMG_0602.JPG

A cm of that was cut and first tried to dissolve it in hot dilute nitric acid, it didnt react.

Again tried to dissolve in HCL and no effect,

I made aqua regia then after 10 minutes of heating brown fumes appeared and solution turned to this color.
IMG_0600.JPG

There were some foils undissolved and can be seen at the bottom of beaker.

I tested the wire with magnet and it was pulling it not strongly though, but it was magnetic, so conclusion it seems like Ni-Cr wire.

Just to be sure filtered the solution, and added DMG and this red particlpiant settled which is indicative of Ni.
IMG_0601.JPG

Next phase will be melting all these Pd black in an electric oven.

Here is the Pd cemented from processing samle 1 stainless steel looking pins, under the phone light it is dark gray color but in regular lighy looks black.
IMG_0599.JPG

Hope these help someone if they find a similar scrap.
 
Hi

I sent all the filter papers with black Pd powder in them to this trusted jewlery shop which have melted a lot for me in the past.

He called to let me know there was absolutely no beads after melting 0.9 g of black powder.

His procedure was damping the filter papers then adding borax and slowly melting using oxygen-buthane torch.

Last time this happened to me it was due to faulty zinc powder that was used in cementing the yellow Pd powder.

I am going to collect the dish he melted the powder in tommorow to see if I can dissolve it in nitric.

Best regards
KJ
 
You say your supplier says there might be Pd- what has he based that upon? Has he seen Telecoms points and made the assumption that "there must be Palladium" or has he actually had tests done that he can show you?

Not all Telecoms points have any PGMs. Silver, and/or gold plated material was used for the majority.

Jon
 
He said that based on his previous experience dealing with the same materials.

I also have used DMG to drop the Pd from solution.
 
I read that you have a black powder that someone has tried to melt but cannot get a bead. I've also seen a pic of some precipitate from DMG which you say is green, but looks pink to me. Maybe it's the light?

Either way what's conclusive about Pd here because it looks (so far) more of a matter of hope rather than evidence? I'm more than happy to be wrong but everything so far appears to be supposition and hearsay wouldn't you agree?

I'm not sure there's a great deal wrong with your process Kevin, but I think the fault lies in being told there is Pd, and then assuming that there must be Pd there without conclusive results. In my limited experience of DMG, it's hyper sensitive to the presence of Pd and is extremely visible in its presence if tested properly in a dilute solution and given time to precipitate fully. You appear (at this moment in time) to have evidence of Nickel.

Thoughts?

Jon
 
Hi Jon

Thanks for your comments. Here are the DMG salt prcipitated after adding DMG solution to nitrate solution.

For sample 1 stainless steel looking pins
IMG_0629.JPG

For sample 1 brass looking pins
IMG_0630.JPG

Unless DMG can drop any other metals ezcept Ni and Pd, the color of DMG salt there was close to canary yellow.

I am going to test a small Pd black that is left and dissolve it in nitric and check with stannous to make sure these black powder indeed are Pd

Thanks and regards
Kj
 

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