NEC telecomm box components

[anachronism]

Hi Kevin

Thanks for the second pic. As you say that certainly looks a lot more Pd like than the first pics. 8) 8)

Jon

 

[kjavanb123]

Hi

I had some black powder cemented out using zinc from DMG salt from scrap that was positive for Pd,

And dissolved that powder in nitric acid, expecting to see a brown solution but it was green like the solution above.

So from solution to DMG salt seems ok, when cementing DMG yellow with zinc it produce a metal that is not soluable in hcl yet black / dark gray in apperance.

I suspect there is something wrong with zinc powder I use for cementing, maybe too much cab o sil?

Keep u all posted

 

[johnny309]

If you suspect that your zinc powder is not pure Zn....dissolve some powder in HCl.....if is pure...H2 and ZnCl2(colorless solution) should occur ....no sediments...

 

[kjavanb123]

Hi

Actually I bought a new zinc powder and it worked just fine.

 

[kjavanb123]

Hi everyone

Supplier of those samples clipped the contacts from the entire telecomm box and sent then to process for Pd, Ag, Au and Pt

Here is the first type of contacts which weighs 22.17 grams


Dissolved them in warm dilute nitric acid


Added couple of drops of hcl till no more white appeared, let it settle as silver chloride


Checked the green solution for Pd, stannous chloride testing solution turned dark brown, indicating a concentrated Palladium solution.


More in next post

 

[kjavanb123]

Silver chloride was filtered and washed throughly with hot water till the solution passed the filtee turn clear and stannous test showed no more Pd.

Silver metal from cementing with zinc powder and hcl.


That silver metal powder was washed till passing solution showed ph 7 on the pH meter.

The dried silver powder from 22.17 gram lot 1 weighs 1.39 grams.

 

[kjavanb123]

After nitric acid dissolved the contacts of lot 1, there was some white powder which it is believed to be tin,

And some heavy black fine powder as can be seen here


Washed them to a beaker added hcl and put it on steam bath, added few ml of hydrogen proxdie (35%) and after 10 minutes got this solution


Based on the color of solution I gussed it to be gold, but further testing with stannous chloride testing solution indicated Platinum


Since there was no Potassium Ammonia salt available to precipitate Pt, I used zinc powder


After washing and drying that powder it weighs 0.06 gram of Platinum powder.

Next post Palladium

 

[kjavanb123]

Ok the dark green solution that had shown concentrated Pd, after removing silver and adding the silver chloride washes to it

I checked the pH of that and it shown close to 3 so I added 200 ml of nitric acid to that solution and stirred.

Prepared a DMG solution, added 4 grams of lye to 100 ml of hot distilled water, to that added 5.81 grams of DMG.

Let it cool, and added it to 600 ml of dark green solution and this appeared


After filtering the yellow Pd DMG salt, checked the solution and still showed Pd presence.


Again prepared the same DMG solution but this time only added 43 ml of that to the filtered solution and got the following


Since each 43ml of DMg solution drops 1 gram of Pd, and I have used up 143 ml of DMG therefore I expect 3.39 grams of Pd

Here is the combined Pd DMG, after being rinsed throughly with hot water

 

[kjavanb123]

I transfered the Pd DMG salt to a much bigger plastic container as I had already experienced lots of foaming during zinc cementing.

Here is the Pd DMG salt in a larger plastic pan


Added 200 ml of hcl (31%), then sprinkled zinc powder and as expected DMG Pd salts started to bubble and foam up


I kept spraying with water then swirl the mixture, as it gradually changed color to dark green


More agitation and a little zinc addition


Near the completion

 

[kjavanb123]

Here final pics

And Pd powder drying

Melting is done tommorow using acetylic oxygen gas

 

[glorycloud]

I would like to buy you a pair of gloves to protect your skin
while you are working with these acids and salts. Would anyone
else like to pitch in and buy a pair or two to protect this nice
person from causing more harm to their body? :shock:

 

[kjavanb123]

Hi

Thanks, I do wear gloves, I took them off for taking the photos with my phone.

Thanks and regards
KJ

 

[glorycloud]

But the world doesn't see that in your photos. If you take your gloves
off to take photos, perhaps you can find a way to take the picture
not showing your unprotected fingers because it gives the hundreds
off viewers of your post the impression that gloves are a nuisance
or are not necessary when refining.

 

[kurtak]

glorycloud

the question/warning to members about waring gloves is generally asked/given to new members to inform them of the need for safety concerns

Kevin has been at this for a very long time & I am "sure" he is "fully" aware of the NEED to ware gloves during processing &/or handling chems

taking pics with gloves on is cumbersome & in fact when taking pics with my smart phone the touch screen wont even work with gloves on

looking at the pics Kevin has taken it is clearly evident he wares his gloves during processing - otherwise you would be seeing chem stains on his fingers - chem stains on the fingers "can not" be avoided during handling/processing if done without gloves - chem stains (on the fingers) is a dead give away

I don't see any stains considering Kevin works with this "every day" so IMO its really a non issue - certainly not one that needs to be "pushed" after a proper explanation is given by an experienced member

Its more a question/warning for new members to insure they stay safe (IMO)

Kurt

 

[kjavanb123]

Hi Kurt

Thanks a lot for your support there. I used my finger in the pic as a reference to the size of black powder.

Yes it is almost impossible to take photos with smart phones with gloves on.

My intension for this post was to show anyone interested in Pd recovery and refining steps I have learned from this forum.

One note regarding the dried weight of Pd powder is 3.34 grams which is very close to expected Pd by adding 143 ml of DMG solution.

I hope to get all the powders melted tommorow and show the final result.

I will be processing more lots of the same box

 

[glorycloud]

Understood. It is hard to take pictures with a smart phone with gloves.
BUT, the point remains. This is a public forum and it simply gives the
appearance that it's OK to do what we do without gloves on.

If you had never been on this forum before and you happened to stumble
upon this thread, what would your impression be?

That is the only concern that I have. Especially when dealing with something
as truly potentially hazardous as the salts formed what you are doing.

I will return to anonymity now.

 

[kjavanb123]

Hi

I finally got to melt the powder into metals here are the results

Pd black powder weight: 3.34 grams
Silver powder weight: 1.39 grams

Pd bead after melting: 2.23 grams
Ag bead after melting: 1.36 grams

Purity of both metals are high. I am just curios about loss of over a gram of palladium depite many washes of dmg salt.

Here are some pics






And silver bead




Nexf I will be processing all of the contacts at once.

Thanks and regards
KJ

 

[rickzeien]

Hi

I finally got to melt the powder into metals here are the results

Pd black powder weight: 3.34 grams
Silver powder weight: 1.39 grams

Pd bead after melting: 2.23 grams
Ag bead after melting: 1.36 grams

Purity of both metals are high. I am just curios about loss of over a gram of palladium depite many washes of dmg salt.

Here are some pics
View attachment 4

View attachment 3

View attachment 2

And silver bead
View attachment 1



Nexf I will be processing all of the contacts at once.

Thanks and regards
KJ

Thanks. Great info.

Sent from my SM-G950U using Tapatalk

 

[anachronism]

Glad you got the Pd Kevin 8) 8)

Jon

 

[johnny309]

It is not lost ....is in your melting dish....if you can provide a picture of your melting dish (I'm guessing covered in black...because you did not reach the temperature for melting Pd....and that I say only looking of the final product.... it is "frozen")