DMG and unknown Pd amount

[kjavanb123]

All,

I have a palladium nitrate solution that the amount of palladium per liter is unknown. Can DMG method be used to find out how much Pd I have in it?

Freechemist (R.I.P) mentioned 2.5g DMG will drop 1 gram of Pd. So if I take 500ml of Pd nitrate solution, and make DMG solution by dissolving 2.5g DMG dissolved in 100ml of water, and add it to 500ml Pd nitrate solution, filter the canary yellow, incinerate it then melt it to find out how much Pd was in 500ml solution to calculate gram per liter for Pd?

Best regards
Kj

 

[patnor1011]

You will find it is very hard to dissolve 2.5g of DMG in 100ml of water. That water would have to be boiling hot (as solubility in water is just 600 mg/L @ 20 deg C), even if boiling I dont know if you achieve dissolution of 2,5g in just 100ml.
I do not know, perhaps it can be used as powder to precipitate directly from Pd nitrate solution, but that is just a guess.

 

[kurtak]

Kevin

To prepare your DMG ad 4 grams NaOH per 100 ml HOT D-water then ad 5.81 grams DMG stir till DMG is dissolved (water needs to be HOT but not boiling) cool & filter

The DMG becomes quite soluble with the addition of the NaOH

When you "first" ad the DMG solution to your nitrate solution it will form a precipitate of other metals because of the NaOH - but the NaOH precipitate goes right back into solution as the acid overcomes the "small" amount of NaOH thereby leaving you with just the DMG/Pd precipitate

You would need to ad enough DMG to a sample be sure ALL the Pd is precipitated - then calcine (or convert with zinc/HCl - or convert with formic acid) then weigh the sponge from the sample

Calcining (using heat to convert) is not an easy task - to much heat you risk burning Pd off in vapors - or you may not get complete conversion

Personally I would suggest using ether metal exchange (zinc/HCL) or chem reduction (conversion of salt to metal) rather then calcining (incinerating)

Kurt

 

[kurtak]

All,

I have a palladium nitrate solution that the amount of palladium per liter is unknown. Can DMG method be used to find out how much Pd I have in it?

Freechemist (R.I.P) mentioned 2.5g DMG will drop 1 gram of Pd. So if I take 500ml of Pd nitrate solution, and make DMG solution by dissolving 2.5g DMG dissolved in 100ml of water, and add it to 500ml Pd nitrate solution, filter the canary yellow, incinerate it then melt it to find out how much Pd was in 500ml solution to calculate gram per liter for Pd?

Best regards
Kj

Kevin

simply adding 2.5 g DMG to 500ml solution will only tell you if there is 1g "or less" in the 500ml --- if there is more then 1g you still don't know how much more --- you have to ad enough DMG to your sample to be sure ALL the Pd has been precipitated --- then reduce (convert) the salt to metal & weigh

Cacining is risky - you may or may not get complete reduction - &/or burn Pd off in vapors

Kurt

 

[4metals]

Add the DMG to assure you have dropped all of the Pd. you can use a smaller sample as well. filter and collect the Palladium Dimethyl-glyoxime and multiply the weight by 0.3167 to get the Palladium metal content of the salt. Make sure you rinse well as any impurities are weighed with the salt. The greatest error in Pt and Pd analysis comes from weighing junk so errors in assay make results higher. Make sure you dry the salts completely and cool in a dessicator.

Pd salts dropped with DMG are bulky. This was a small 1/2 gram sample of high yield Pd.

 

[kurtak]

filter and collect the Palladium Dimethyl-glyoxime and multiply the weight by 0.3167 to get the Palladium metal content of the salt.

8) Thanks for posting this math 4metals - I was un-aware of the salt to metal ratio before this - very handy info :!:

notes are being made now :mrgreen:

Kurt

 

[kurtak]

Kevin

you may want to consider dropping your Pd from nitrate solution as a diamine salt rather then a DMG salt & then reduce the salt with formic acid

do some research (all the info is here on the forum) use diamine as a search word & formic acid as a search word (search them each on there own)

you are working with ammonia here & ammonia fumes are very toxic (even deadly) so you need ether a "very good" fume hood - or work outside - up wind (wind behind you) & a "good" cartridge respirator

Also other metals in a nitrate solution with ammonia can form explosive compounds if not acidified right away - so be sure you fully understand the process

Hydrazine is another option - I don't know enough about to say anything about it at this point as I have not yet played with it & have only read about it in my own research

Kurt

Edit; to change the wrong wording "down wind" to the right wording "up wind" (typing faster then I was thinking)

 

[4metals]

I was un-aware of the salt to metal ratio before this - very handy info :!:

notes are being made now :mrgreen:

Some other factors you may find useful.

Platinum dropped with ammonium chloride (NH4)2(PtCl6) factor 0.4395

Palladium dropped with sodium chlorate Cl4H8N2Pd factor 0.37431

 

[kurtak]

I was un-aware of the salt to metal ratio before this - very handy info :!:

notes are being made now :mrgreen:

Some other factors you may find useful.

Platinum dropped with ammonium chloride (NH4)2(PtCl6) factor 0.4395

Palladium dropped with sodium chlorate Cl4H8N2Pd factor 0.37431

Awesome & thanks for posting 4metals

do you by chance have the number to factor the Pd diamine salt :?:

Kurt

 

[kjavanb123]

All,

Thanks for your advise. I think DMG usage has the advantage of precipitating all Pd in solution, eventhough it is more expensive than sodium chlorate. I have collected more than 40 liters of nitrate solution that has mostly copper, silver and palladium.

I have used silver reduction by precipitating it as silver chloride, I do not have a filter press yet, so rinsing the silver chloride from Cu and Pd nitrate solution is difficult.

I decides to drop Pd first as DMG compound, then drop silver using copper bar, and finally recover copper using electrowinning.

So I prepare a DMG solution, using 58 grams of DMG, 40 grams of lye added to 1 liter hot distilled water. Take 1 liter of Pd nitrate solution, add the DMG solution, until the remaining solution tests negative for Pd, filter dry the Pd DMG salt, multiply that weight by the factor to find out how much Pd in 40 liters of solution, and prepare accordingly.

Regards
Kj

 

[kjavanb123]

All,

Our recent smelting batches, have produced a lot of liters of nitrate solution that contains both palladium and copper. Since I have posted this thread, never had a chance to actually test it till today. Hope this becomes useful to everyone.

Before I start, I should thank freechemist (R.I.P) for his detailed description on DMG usage, and Lou for his comments on PGMs.

I took 200ml from 10 liters of palladium copper nitrate solution, its been produced from smelting 40kg of laptop boards. Here is the photo,


Prepared a DMG solution by first dissolving 4g of lye in 100ml of water, add to that 5.81g of DMG. Added this solution to nitrate solution while stirring, a mixture of yellow canary and green powder formed, as can be seen in the photo,


Here is the filter paper as I opened it to rinse the materials to a beaker, wonder what are those green mud,


I checked the filtered solution with stannous chloride and tested negative for Palladium. Rinsed everything from filter to a beaker to use zinc and 10% muratic acid process to convert yellow salt into palladium sponge,


After some amount of zinc addition and stirring, yellow solution turned almost greenish in color as can be seen here,


More in next post

 

[kjavanb123]

Here is yellow salt solution after 20 mintues of zinc addition and stirring,


Finally the solution is rinsed, gray powder is washed with hot water few times, then added weak sulphuric acid to dissolve any remaining zinc powder, as can be seen here,


I will wait until all zinc is dissolved, wash the residue with hot water until pH shows 7. Dry and weigh the palladium sponge from 200ml solution, multiply that by 50 to estimate the amount of palladium in 10 liter nitrate solution.

Regards
Kj

 

[kjavanb123]

Hi,

The dried black powder from above process showed 0.8g of Pd black powder. Since this was percipitated from 200ml of 11.2 liters of palladium-copper nitrate solution, I plugged in the DMG powder weight I had available, to formula given by freechemist, took 5.5 liters of nitrate solution, and added 9.7 liter of DMG solution.

Here is the result,


The yellow canary salt being filtered,


Here is the stannous chloride test on filtered solution, the spot on top of picture, and the below it is the stannous chloride test result on original palladium copper nitrate solution before DMG solution added,


Filtered canary yellow salt to a beaker to convert to palladium sponge,


I usually dry the yellow salt on low heat, weigh it, then use formic acid method to convert the yellow salt to metal, this time I used 10% hcl plus zinc powder method, the yellow salt keep floating on top with each addition of zinc. I kept stirring and the yellow foam never seem to settle, so I filtered it again, and drying up the yellow foams as we speak.


One thing is the foaming, the other thing is usage of DMG for palladium unknown quantity test in a solution, based on my calculation from 200ml solution I figured there should be 44g of palladium in 11200ml of pd nitrate solution, but looking at the yellow salt half of the solution produced I am guessing it wont be more than few grams of Pd sponge. Please advise

Regards
Kj

 

[Lou]

Buy some superlig2.

 

[kjavanb123]

Lou,
Please kindly advise what is superlig2. I did a google search and it shows a lot of soccer related articles. Is this some sort of resin?

Regards
Kj

 

[kjavanb123]

Hi Lou,

Finall found some company in Utah, called IBC, they seem to have superlig products for selective extraction of metals from complex solutions,

http://www.ibcmrt.com/products/superlig/

Thanks
Kj

 

[Lou]

Yes. Tell them I said to call, they know me. It is a very expensive product but it works and works well. Each kilo will do 100 or more ounces of Pd, usually to 4N. Just be advised that you MUST remove the gold first from the solution.

 

[nickvc]

Lou you are a mine of information to be explored... :roll:

 

[Lou]

What's with the eye roll?

The product is silly easy to use and for anyone who can afford it and having certain necessary subsystems...highly efficient. Not the highest capacity of a resin for Pd at about an oz per kilo, nor the most concentrated eluate. However, the quantitative recovery, insane kinetics (you can literally pour a dark brown Pd solution down the column and watch the Lig strip it colorless)...it's pretty hard to mess up!

 

[nickvc]

Lou it's British humour, I know you know more than I ever will and your scope of knowledge is staggering, do I have to kiss butt all the time :shock: