smd's

[2002valkyrie]

Samual,
Did you boil your mono-caps in hydrochloric acid till the nickle was gone before adding them to AP?

(look like the right color?).

Yes that's the right color.

they both seems to contain Pd... where to from here?

You should treat them like any other pd containing solution. Steve's video shows how.

 

[samuel-a]

2002valkyrie, on the first time i added them 'as is' to the AP.
id did the first AP in that order:
24 hours on crock pot
24 hours on stirring
24 hours on crock pot
24 hours on stirring
24 hours on crock pot

day six i have changed the AP, from then it's on stirring all the time

 

[2002valkyrie]

2002valkyrie, on the first time i added them 'as is' to the AP.
id did the first AP in that order:
24 hours on crock pot
24 hours on stirring
24 hours on crock pot
24 hours on stirring
24 hours on crock pot

day six i have changed the AP, from then it's on stirring all the time

That's a lot of work! I finnished 1lb in 36 hours.
12 hours boil in hydrochloric
H2O rinse
12 hours boil in hydrochloric
H2O rinse
12 hours boil in AuqaRegia
***Start 3 times evaporation ***

 

[samuel-a]

well... the machins do all of the work :mrgreen:

let me see if i i get it right. (we are talking about un-crushed items)
the first boil will remove Pd along side the base metals - correct?
secund and third remove only Pd ?
what do you do with the water rinses? combine with the HCL leachs?

have you completed this process all the way to a Palladium powder?
how much HCL per lb of monocap's?

thank you for the info
SAMEUL

 

[lazersteve]

Sam,

Valkyrie is right on the money. Use HCl to pre-treat the crushed monolithics. Once the HCl extracts stop showing nickel (deep purple at first, then light blue-green for later extracts), move to AP, HCl-Cl, or AR to digest the Pd. I have also used directly AP on the whole capacitors, but it's way slower.

I have dug up my videos of the process, but it will take me most of the week to get them posted as there are about 35 segments to edit down. The videos cover, harvesting, crushing, nickel extraction, nickel testing, Pd extraction, and Pd testing.

Your next step is to filter the orange red solution until it is 100% free of sediment and suspended particles. Follow that up by watching the Pd videos on my website.

Steve

 

[2002valkyrie]

Hey Steve,
I just got a few pieces of an old office phone system and busted them open. Are any of these worth messing with? I took one one of the blue caps. and skinned it, then boiled it in hydrochloric for 1 hour - nothing. Boiled it in nitric for 1 hour - nothing.
Here's the link to pictures of the items in question. Forgive the phone pics. http://s420.photobucket.com/albums/pp287/2002valkyrie/phone system components/?albumview=slideshow

 

[butcher]

sounds like an MOV to me, Im on dial up so couldn't see your picture.
http://en.wikipedia.org/wiki/Varistor

 

[lazersteve]

The photos are of either MOVs or high voltage disc capacitors, not monolithics.


Monolithics are typically surface mounted devices (no legs).

Steve

 

[Scott2357]

Valkyrie,

Not sure about those first three types, could be several things. Some part numbers would help alot. However, the yellow radial lead type on your boards that are shaped like the end of a Q-Tip are tantalum.

 

[samuel-a]

steve, please, one clearification about Pd dropping that i couldn't understand from your DVD (and hoke).

do i have to evaporate the Pd bearing solution down to 1/3 - 1/4 of it's original volume and then add water, or to start treat it with ammonium chloride as it is...?

does other metals like nikel and tin in the solution will interfere the Pd drop?

 

[lazersteve]

steve, please, one clearification about Pd dropping that i couldn't understand from your DVD (and hoke).

do i have to evaporate the Pd bearing solution down to 1/3 - 1/4 of it's original volume and then add water, or to start treat it with ammonium chloride as it is...?

does other metals like nikel and tin in the solution will interfere the Pd drop?

Sam,

Pd is a little touchy to deal with.

Here are the key points:

1. The solution must be free of sediment of any kind. This includes salts and debris. If you are getting salts from HCl-Cl the best route is to precipitate the Pd out with zinc, then redissolve the Pd in 35% nitric, de-noxx to the chloride with HCl, and continue to step 2 below.

2. The solution must be concentrated. The color of the solution should be blood red. You can see the proper color in my Pd video on my website.

3. The solution should be heated to just below boiling.

4. Ammonium chloride is added to the hot solution. Use 1.25 times the weight of expected Pd in NH4Cl. The excess ammonium chloride goes into the water of the solution making the resulting Pd salt less soluble.

5. If the addition of Ammonium chloride forms an orange or yellow precipitate, you may have Pt in the solution which will require the solution to be filtered (vacuum filter preferred) free of the Pt salt. If Pt is removed, the solution should be concentrated again due to the addition of the dilute (15% ) ammonium chloride wash solution used to wash the resulting salt.

6. Add a few crystals of sodium chlorate to the hot solution, stirring with a glass rod, until the fizzing stops. If the Pd does not begin to precipitate, add a few more crystals. Repeat this process until the brick red Pd salt forms. Once the salt begins to form, let the cool and solution settle and note the color. It should end up a light yellow color to pale lime green, depending on the contaminates. Once the salt settles test a small sample of the solution in a test tube with a little more NH4Cl and chlorate. If you still get red powder, add the test tube contents back into the main solution and add more reagents to precipitate the last of the Pd.

I do mine like Hoke suggests, Lou does his a little differently and has an excellent post with pictures on his process.

I hope this clears everything up.

Steve

 

[samuel-a]

thank you steve very very much.

so, i have reduced the volume of the first AP leach (the one that looks dark green in my photos) from 420 ml to around 100 ml, the leach did got some dark red-ish tint to it, once it got cool some salts began to precipitate, i belive i should filter them out, dissolve them in HCL and check for values....


the only ammonium chloride i managed to find is branded "SAL AMMONIAC BLOCK"
see here: http://gormez.net/Hebrew/uploads/Gallery/AMMONIUM CHLORIDE BLOCKS13.JPG
is this good for the job? it is stated that it is ammonium chloride.
the only other option i found is to buy a 55lb bag for 53$ for CP lab grade stuff (to much for me)

Edit: a small search in the forum gave me the answer

 

[samuel-a]

my first time ever Pd dropping (done exactly like on steve DVD) is a great success .

i have reduced the volume of the first AP leach of complete monocap's (look up in my photos, it's the green solution in an erlenmeyer beaker) to around a 1/4 .
filterd, gave a little rinse to the filter with 15% ammonium chloride to get all of the leach down.
heated to aroumd 60-70 Celsius.
added 4.5 grams of ammonium chloride , waited 5 min...
and then started to add a sodium hypochlorite (chlorox) 3% CP.
ended up adding 12 ml of hypochlorite and dropped most of the Pd out of the solution.




Many thanks to the great people in this forum and for you steve 8)

 

[samuel-a]

here it is, fully calcined:




the whole process went well, but with a very disappointing results... only 0.5g of Pd from the main bolk of the AP leach.
i was expecting around 1.5-2.... i didn't weight the red powder, but i belive it was weighing around 7-8 grams.

steve, what is the usual weight ratio between Palladium ammonium chloride and the reduced metal?

 

[Platdigger]

I am not Steve but, Ammen has palladium chloride (PdCL2) at 60 percent metal.

 

[lazersteve]

Steve, what is the usual weight ratio between Palladium ammonium chloride and the reduced metal?

The molecular weight of the Palladium Ammonium Chloride is 284.31 grams per mole. The weight of a mole of Pd is 106.42g. Therefore, if your had a 100% pure palladium salt, free of excess ammonium chloride and other contamination, you should get :

106.42 / 284.31 = 0.374 g of Pd per gram of salt.

Since you started with 7 grams of salt you could expect a theoretical maximum of :

7 x 0.374 = 2.618 grams of Pd.

Losses occur if you heat too much during the calcining as the salt will vaporize along with the ammonium chloride. Your salt looks too orange to me, which may be an indication of excessive ammonium chloride trapped in the salt's structure. To remedy this problem you can dissolve the salt completely in 28% ammonium hydroxide and precipitate the purer yellow powder with HCl. Hoke covers this in detail. Another possible source of losses is calcining in a carbon (ie graphite) dish or heating with a direct torch flame that carbonizes the salt. Carbides of Pd and Pt are volatile.

Steve

 

[2002valkyrie]

Hey all, I finally got a few breaks from my gold. It comes before Pd! Here is a few pictures of my solution before the drop and of the palladium salt in the filter.

 

[samuel-a]

thank you steve.

the picturs does no justice to the powder, as it was deep red and not orange as it appears in the photo :|
but good possibility that i used an exess of ammonia... couldn't hurt

anyway, i believe that the calcining i did was ok, i tested the smoke with cold beaker every now and then, and there was no deposits other then white.
all and all it took 5 hours to complete.


this is a very 'magical' process in my eyes, and i wish to evryone to experience it .

Edit: BTW, in my hook book copy, there is missing one page - 178 which is re-purification of red powders.... :?:

 

[Oz]

I am glad to hear the color of that is not representative. It looked like a Pt precipitation contaminated with Pd.

Congradulations

 

[samuel-a]

thank you Oz.

by now i have processed 250 grams of mixed monocap's from cards, CPU's, mother boards, just about everything that looks like a monolithic capacitor, from a relatively new scrap (no more then 15 years old).

and the yield is steady - 0.5% Pd from total mass.