# hello friend presenstation and first sharing



## Abdoulapapatte (Jan 27, 2022)

*Hello Friends*
I'm from France and I live in Belgium (BE). I have a passion for metal, and since a few years and pushed by the passion I started to recover a little bit of electronic scrap and silverware, all thing that people throw away.
I rushed and filtered my first times in coke bottles (plastic), very few materials. with time:
I improved a little bit the basics of the materials, the security, the procedures.
I started by melting then with time to refine, that stuck at once with the money then then the gold with all the problems which one can meet while starting in this passion *
(deception, scam ..., contamination, low purity result at the beginning).
and then like every time
"nothing is impossible for the one who believes and acts".
So I pulled my fingers out of my arrs and started to dream.
With each victory I began to tell myself that in the long run and if I continued to like it, I would invest myself more. 

*finally *
after many efforts, discouragement, period of pose, here is where I am now in this tuto I will detailed
1) my xrf results (mass spectrometer)
2) my way of doing, my tricks, what I observe also alone.
3) my physical results and visible by your eyes.
Here are some pictures that illustrate a little bit all that .

I hope to have many readers.
If not, let's talk about me in a few words:
I love science
study cycle:
science orientation :
+ science technology of laboratory
+biochemistry, biological engineering
+Medical school 2 years to understand that it will quickly take the head.
+nursing (3 years) to understand that the hospital mental was not made for me 
+professional salesman because in the end, no need for a diploma to sell.

I thank the people who post, everything and anything, pros, beginners, amateurs, visitors ......
because contributing helps everyone
special thanks to : sreetips, dusan 999 mr owltech, alchimia canal , nudrage, nil red, chemistry games , mlbcc...........
topic to be discussed soon
alloy (*pd / au / rh ?/ pt ? / ag ? / cu)
little spoiler picture
SEE YOU*


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## Abdoulapapatte (Feb 21, 2022)

We will start here with one of the first important poles, an alloy [au/pd/cu/+X] where X designates all the unknown metals which can be present in addition in this alloy, such as for example:

X: suspect metals------> Fe+Ni+Ga+Pb+Al+Zn+Ag.

CHAPTER I ALLOY/MELTING/ANALYSIS/PREPARATION
Only the precious metals have been brought back, the base metals have not been sent to me, and there is no time to go to the store to analyze all this a second time with the spectrometer, that will cause us one more difficulty and we are rather like the difficulty and the challenges so let's start ^^. All the trash you see with a red tag

Translated with www.DeepL.com/Translator (free version)



We simply melted the metal, then poured the metal into a bucket containing cold water, the water was agitated with a piece of wood to create a current of water in the bucket, this avoids that the metal touches directly in the bottom, and especially here that it pierces the plastic seal. see video.


View attachment video-1613615227.mp4

View attachment video-1636916701.mp4




The melting was done with a Devil forge 4 kg + gas bottle premixed butane / propane, allowing to exceed and by far the 1000°C.

In the end we have

1) melted all the blocks to make the multiple alloys homogeneous in one: 

2) transformed the metal mass into several small shots 3) isolated and dried the metal
., 






and a small table to explain it all


View attachment video-1636916698.mp4

.


percentage in white % // weight in red (gr).

TOTAL 617 gr of alloy with 61.22gr of gold, 65.13gr of palladium, possibly some platinum remains ? Ag ? 

only a sample of 28gr of metal found in the forge is really unknown in its composition in precious , let's hope it remains a good news for us !






attacked the metal, we will begin to dissolve
1) cutting all the metals that we want to recover, I am of course talking about cutting, ferrous and non-ferrous, basically anything that can interfere with the purity of my precious metal. let's not forget that here, during the melting, borax was added, to reduce the melting temperature and oxidize everything that may have been oxidized in the process, it cleans some impurity, which is already a good thing, the copper present in the alloy also facilitates melting.
2) To attack effectively and recover all of the precious, while eliminating the cut, it takes a little to remember,
which acid, attack which metal, here, we move first Palladium, and silver (Ag, if present) with 65% HNO3, the other platinoids, and the gold should remain in the bottom of the beaker.
3) the metal will infuse in different concentrations and temperatures:
A) the first: +- 150 ml demineralized h2o + 200ml Hno3 65%, I personally call it the cold attack, we do not know the possible reaction between the alloy and the acid in general, it is this first times when the reaction can be the strongest, especially if it contains metals that are easy to digest for the acid and especially those that you want to eliminate first, the palladium will take longer to dissolve as well as the silver, even if they too are attacked by the hno3. we could have gone before, not muratic acid (hcl 37.8%) to really remove a good part of the cut without touching the PD, but we had little quantity of hcl, it stinks, and I prefer hno3, and recover palladium thereafter is not a problem. also if the alloy is not properly rinsed after using hydrochloric acid, in the presence of silver,
finally the metal is put in the beaker or we will be able to start again in hno3, the silver chloride could come here to piss me off


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## Abdoulapapatte (Feb 21, 2022)

the h2o/hno3 mixture is left for a while. The action of the acid can be observed by relying on the bubbles during the attack of hno3. Thereafter we observe a change in color of the solution, we can clearly see that it becomes bluish, turquoise blue


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## Abdoulapapatte (Feb 22, 2022)

to complete the last photos here is a summary, we distributed the shot in two large capacity beakers of 3000 ml in borosilicate 3.3 (pyrex, I preferably work with resistant material)


,important here because I go through heating stages, I also specify that in this kitchen, I had to adapt, because there was no material that I usually use at home, I am visiting a friend , I have to help him purify a little precious everything is mixed, see table. with red chalk / white chalk. I took a maximum of materials, but we never have enough huh!

So I have distributed as shown in the photos:



in a third beaker, we put +- 22 grams of 18k, which we put in quartation to be able to attack it better with the acid, to make it more soluble and to facilitate its dissolution, to do so, we cut it with copper , here is my quartation calculation:



18k (750/1000)

mass

m = 22 grams - 2 grams of iron, plastic, small stones
m= 20x0.75=15 gr of pure 24k gold



QUARTATION:

q= (15X3) - 5 grams
q= 45-5= 40 gr of copper to add.
q= We therefore add 40 gr of cut (copper) to arrive at an alloy containing 25% gold easily soluble by 68% nitric acid (hno3). So in the end, we after quartering we end up with + - 60 gr of alloy (20 gr of 18k + 40 gr of copper)

















I started by making 20 gr quart buttons, then I opted to make shots, small drops of metal, cooled by water, in the same way as the previous shots.




in beacker + h2o



I therefore attacked the 3 alloys contained in its 3 beakers.
We treated the quartation apart from the others, depending on the type of alloy we had.
here are our 3 beakers finally filled, with demineralized water.




the addition of hno3 was then made, the first addition was made with a quantity of + - 200 ml of hno3 in each beaker, without heating, this is when the acid can react quickly, I put always add water before the acid to allow it to dilute, and to reduce the risk of splashing and vapor. avoid the risk of injury. the ripening is done outside to avoid poisoning. a glass cap or here in the photos, in coping mode with plates, is put on each beaker to stop the vapors and prevent evaporation.

It is at this moment that the green color is present, a probable sign of copper, nothing bad since I cut my recycled alloy with this one, in particular a stock of dental debris (white gold, yum).
And let's not forget the quartation with the 40 g of copper added to beaker N 3 .




here is the beaker of the quartation, at this stage the color is turquoise green in a little all the beakers




successively, many additions of hno3 will be added by 200/300 ml, during the second addition, I leave 10 minutes to act, then when the reaction calms down a little I start heating the solution, my cruising temperature is between 85 °C and 100°C depending on the amount of liquid with my heating plates, not very precise to maintain an ideal T°, but we do with it.



After many passages and addition of nitric, my solution containing 300gr of gold/platinoid alloy, is colored going from light green, to bluish green, then dark blue, and finally dark black, very black, very dancing a big mud is form at the bottom containing gold and rest of platinoids, not attacked by hno3 or in the process of digestion,




I collect this syrup, hyper concentrated and I filter it to separate, the solid and the liquid, at the same time, now that it is well digested, I can put everything in a single beaker and gain a little in place.

I store this syrup in a large Erlenmeyer flask during the filtration phase, then once filtered well I store it in large 5 Liter cans.



We put them aside for the moment we will be interested in another important test, to detect if the silver is present in this solution, if there is, then we have done well so far to use only nitric.

Simple and very effective test: solution + addition of salt water [NaCl] (table salt)




Shit shit shit, the solution becomes cloudy, ok I have silver, in contact with NaCl in aqueous media, table salt is transformed into a Na+ kation and a Cl- anion, the silver present in the solution under form of Ag+.



When Cl- and Ag+ meet, it produces silver chloride, really the N°1 of the ball busters, especially when you don't want it to be there =), it disturbs the solution here, so it is very present!! !



See you for next episode
abdoulapapatte
#vince


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## Abdoulapapatte (Feb 23, 2022)

hello to all I come back to you to advance my cooking coup, after having highlighted the presence of silver with the salt I already know that I will not add chlorine, not before having precipitated the platinoids now, here are the 2 beakers united in one, it is the Au/Pd/Ag alloy + starting metal base,



I rinse it with water, then I iron a shot of nitric, I then redo a test for the money, I have no stannous chloride on me, nor what to make so, I test what I can and I proceed cautiously.
mud remains present rinse one last time with water and I decide to put aside the rest.
for the third beaker, that of the quartation, here is the current result, a pretty 6k well attacked by the acid, a typical color,




it's going to be time to go to the aqua governed for the two rest of the beaker, so everything that has held up well in the hno3 65%, will now be digested by the mixture of two acids HCL and HNO3-.
just before I start to take an interest in all my filter solution so far, I decide to put a 3 liter sample in an Erlenmeyer flask,



then to extract the palladium, especially here to concentrate it, I start with the DMG approach
or dimethyglyosime / Diacetyldioxime /


with 500gr I have room for my tests, this is the second time that I go through the dmg to separate the palladium from the rest, Dmg will create a precipitate, only yellow precipitate appears, we have boiled it really well acid before so it is very unreactive, there is no formation of gas or smoke at this time, the added solution is simply demineralized water, saturated with DMG powder,

you can clearly see the precipitate dancing in the magnificent Erlenmeyer flask.
we leave it aside for a moment, to let it rest a crust will form at the top a kind of yellow foam is at the bottom a heavier yellow mud.

View attachment video-1636263198.mp4



I will harvest it as the filtration progresses




At the beginning, the most difficult thing is to find a quick way to filter, not easy without a vacuum system.

While it gently precipitates and gravity does the work, I run the aqua regia into the gold/copper quartation beaker, and into the other beaker with the pd/AU alloy







this time the solution contains gold, this solution is not yellow / red, as when only gold is present, here it is very dark, during manufacture, I did something useful and too often ignored by some, when you leave with this solution, the mass of which is often unknown and the mud is dirty, you must first rinse a little with water, check for the absence of silver, wash again if present.

I have Keep a bottom of water in the beaker, new H2O +- 200ml / added 150 hcl, I waited 10 minutes, put back 200 ml hcl.

I start to heat very slowly, then I prepare a 10 ml pipette and a 60 ml syringe.
I start by adding small doses of hno3 to gradually create my aqua regia throughout the cooking process.
So no need to work on a set amount, and I can observe the mass of solid metal remaining to be dissolved in the bottom.At the end before filtering the 2 solutions to then precipitate the gold I add in each 5 / 8 ml of sulfuric acid to precipitate the lead (if present, it should precipitate in the bottom)
After finishing I filter the 2 aqua regia, one is all black, the other is piss yellow.

I then precipitated the gold with Na2O5S2 /SMB /sodium Metabisulfite

the two solutions darken and I see the gold precipitate, in the 2 beakers, one solution becomes clear again the other remains black, I carefully empty the 2 solutions into a treatment container (stock pot), and I recover this , which I leave to sediment well between each treatment



small quantity in the beaker containing 15 gr theoretical of pure gold.



more consistent in the second, this one remember follows my table


much more interesting


it remains here simply to wash wait / wash wait (H2O).
-empty the water, put a background of hcl / H2o [50/50] to rinse the gold, any small parasite may still be present.
-again I empty the rinsing solution of hcl /h2o,
- I wash mtn with H2O, then I dry on low heat.

Once very dry and very clean I obtain for the first beaker of quartation!!

15.41 g Yes




for the second: YES YES YES


not bad at all right?? if we refer to the table we are on the right trackµ

see you later and comment
thank you


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## Abdoulapapatte (Feb 24, 2022)

*avant d'avencer sur la palladium finissons l'or , revenons sur 2 ,3 choisi important *

just after taking out the gold from the aqua governed precipitated by the SMB
View attachment video-or precipitation reduction.mp4


, i wash
View attachment video-or lavage.mp4


then I dried it, price in photos on white paper, we can see that it pulls a little on the brown, brown, yellow, more than on the yellow, orange, it is quite dark





I passed it a little in HCl to eliminate the rest of the potential parasite, then I washed HCL with water, lots of water like here above, in the same way.

I dried it again, observe the color well now, clear HCl has done its job. Here we see the result after passing the hcl on the 61.38gr of gold

View attachment video-or début chauffe.mp4


washing water goes away
View attachment video-or séchage.mp4

A beautiful orange-yellow appears

a small piece of wood allows you to detach it without losing a single grain, at this time the gold sticks to everything, impregnates everything, even the pores of the skin, even the gloves, beware of loss.
View attachment video or se decole.mp4



the first 15 gr of the quartation, are melted first, the crucible is already used, therefore dirty and surely parasitized, copper silver, carat gold and others, I put borax again to separate the new from the old grime, and re-prepare my crucible for a new font.

I'm starting the gold castings and I'm starting them before the palladium one, because my metal here is clean and I don't want it polluted with the palladium.








View attachment video or transformation fonte.mp4

here I'm near bottom before switching to bi-gas (with O2 allows to have a hotter flame)


here is an example here, in a one liter tablet, it is expensive and it empties quickly.
we will see it in action on palladium (the secret weapon):

bef here is the output of the 15 gr of gold after melting




with a little borax on the button, very, and very little loss.
I finally decide to put it in the form of an ingot




sulfuric acid + H2O helps pickle borax.
when at rest: 61.99 g


Finally, here is the total: 77.27+- gr 24k








QUALITATIVE RESULT ............SPECTROMETER AT 998.5/1000 //// AG PARASITE 0.17%

END OF GOLD PROCESSING ..............



Now let's talk about palladium, and platinoids, I decide to do 2 tests in the simple stride:

*1)* search for and highlight the platinum if present (ammonium chloride)
*no precipitate here on a small sample

2)* check that the palladium is well precipitated, at 100% whether yes or no, if still present, I would put a little H2O saturated in DMG. *yes everything is there

3)* Taking a sample plus spectrometer analyzer, to have clues
(useful but to be taken with little consideration, many factors played)

Indeed I do not base with NOT MY MATERIAL, *BUT WITH THE BREAKDOWN, DON NOT EASY TO FAILE A GOOD RESULT I Put The 50/100* Given The Unknowns of X (Base Metal).

*4) *after sampling, weighing and melting, analysis and search for purity.

1) for me and with the current equipment, I looked for the plate in the following way,

I took + - 20 ml of the aqua regia stock solution which dissolved the sludge, previously treated in the 2 beakers containing + - m metal alloy = 300gr each (x2= 617 gr from the red writing board) I put a brief summary of the past stage
1) 
2) 
3)


3.1)

3.1)
View attachment video-nitric survivor_Trim timer.mp4


3.1) treatment so far hno3 exclusively, small dose by small dose

3.2) filtration

3.3) the solid goes into aqua regia, for liquids:

3.4)------> palladium/silver output

3.5) -------> palladium output (yellow sponge) / nickel?? (red sponge) ----> [DMG/Pd/Ni]

3.6)--------> storage of money in 5L containers

3.7) -------> timely release money deal with [Cu][hcl/or table salt]------->[NaOh/sugar]

4.1) AQUA REGIA. h2o / hcl (ratio 1/4 (100ml h2o/ 300ml hcl )

4.2) adding nitric bit by bit

5)------> output of gold with SMB (would have been better with coppers, except here equivalent because no excess of HNO3 therefore no platinoids were to precipitate.

Short......

we are therefore at 3.4) I come back to this step:
Stock solution



after extracting small samples like this


I realize two chose:

1) recommended yellow so good for palladium.

2) rush light metal quantity will be seen

3) very long and extremely boring ........ it doesn't flow well

4) I adapt as best I can


when I wash the sponge cleanly with water but it seems to go back into solution, to stop this phenomenon, I decided to wash the precipitate with water saturated with DMG, I think it worked well. But I have a doubt.




after h2o/DMG and it seems much better to me, doesn't it.
I let it dry and harden nicely





I priced a dirty piece and a clean piece, we'll see after melting what Mr. Spectrometer says, the only one who rarely lies on earth ............



I have to review a little cm hoke, (I'm moving slowly because I have to translate the book into French (hassle)).

I see on the videos that to purify the sponge many have gone through ammonia, then hydrochloric acid to make it reappear, but I have the impression that they lose a lot in solution and everything does not always come back in reminded (sponge). Also the dosage is tricky it's all about acid/base ph??



*3)* I tell myself we'll see, in the meantime, here are my samples *3):*



I burned it, with a small blowtorch, to gain in place and make a transformation close, it looks like coals. (don't pay attention to the weight, I don't even know if I put my scale to zero, and if the plastic is not included in the weight it indicates.





I took my precautions for the eyes and the hands during the manipulations, with what I had on hand,

whether during melting or during chemical reactions one more thing, I always put the acid in the water and never the water in concentrated acid, nor concentrated acid / base together, let's not forget safety, as well as the hands, with latex gloves, resist hno3 65% and do not burn in contact with it, as is the case with the hno3 form >90% (smoking).



now move on to makeshift melting here as for the quartation I start by calcining the sponge with this type of burner, not very efficient but the bottle lasts a long time for preheating.



ready to melt




To be continued in the next episode
feel free to comment, bye


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## Martijn (Feb 25, 2022)

Very impressive. I enjoyed reading your post and the beautiful results! 

Where are you in belgium? I'm across the dutch border in zeeuwsch vlaanderen. (spare belgium)


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## Abdoulapapatte (Feb 25, 2022)

re bonsoir a tous aujourd'hui je serais bref , pas la tête a passer


Martijn said:


> Very impressive. I enjoyed reading your post and the beautiful results!
> 
> Where are you in belgium? I'm across the dutch border in zeeuwsch vlaanderen. (spare belgium)


hello to you my first comment =)

thank you for your encouragement, the next step will be the rhodium one of its 4, and to shed light on what interests me in there.



Now let's move on to the next day on palladium refining.

On my photos ready to melt we can therefore see this famous PGM sponge, so I suspect palladium and certainly Nickel, which would therefore have been slipped by the DMG (dimethylglyoxime).
indeed nickel is also emitted by the latter, and is expressed by a red warning.
here we can see that the palladium after a slight melting and drying, has become orange!




At first I calcined my sponge until I had one gram with butane which did nothing, then with a mixture of propane70% butane30%, finally I finished it with oxy bi-gas, O2+ [propane70% /butane30%.]

View attachment video-preparation palladium fonte difficile_Trim tuto.mp4

after 10 minutes of intensive heating in poor condition (graphite is not great for heating and keeping heat, especially at room temperature 6°C, and especially with such a low flame ..........


despite everything, I observe a change in the material


yes we can see here that the gray color is starting to emerge everywhere, little by little the black gives way to grey......





The flame is not powerful enough, ok we take out the Devil forge




GOOD BLACK COVERED WITH BORAX A LITTLE DIRTY, it will be laminated for a spectrometer analysis



IN THE FIRST TIME THE spectrometer speaks, it gives me its results! ha oops, I can see that there is nickel, hard hard, as I expected since the alloy is a mixture of several alloys.
so 66.99% palladium!! yes!!!!
but we can improve all that can't we

!!!! Sir Yes Sir !!!! -OK



1) cu19.61% ok he helped me melt (lack of Ag money)

2) 6.51% Ni and again beware the samples are very dirty, and not representative of the rest.

3) At 3.56 (yes a little loss in particle or tiny dilution with hno 3 , Ag (quartation?)


my question here, how to separate the nickel, attack before the HNO3 with the HCL?

the palladium sponge calcines well, but to melt it is another story......

even with a devil forge, butane is inefficient, it is less calorific than propane, and I only have this one, it sometimes helps me out with copper, silver and gold, but not for the rest.... ..
View attachment video-palladium fonte difficile 2.mp4

I take it out but it cools quickly, faster than gold and silver, barely out the melting point is no longer reached, with propane butane 70/30 no problem, but my current gas is zero.. .....

I go in force with the O2, which directly makes the difference here is an example which shows the ease that the flame has in putting the metal in fusion

(video for information only, shows the strength of the flame)
View attachment video-quartation.mp4



watch now with O2-BI gas the metal melts, in 10 / 15 minutes of melting after a first calcination, a melting of a large palladium button, the whole for the moment is melted from this method
View attachment video-fusion or.mp4


in the end, I now find myself with a few buttons, a small piece of palladium


very hard to melt correctly all the same, it cools very quickly


I still manage to make a block


I pass a second time to the spectrometer a good performance, the machine has just been calibrated it is a machine with more than 50k, we can trust him,

this is a clean sample of the sponge, the purity is announced at 75% a little better (equivalent to 18k for gold).

case total 16gr at 69.99% and 71gr at 75%



Just before melting my colleague was too impatient, but if I had had more time, I think I would have tried to purify above 95%, it would have been nice, I'll see if I can find another way and refine even better. but hey sir is in a hurry to sell........the palladium is high right now!!!

ASSUMPTION AND IMPROVING PURITY

I'll think about it tonight




in the end afterwards with another alloy I get better purity and I no longer have nickel but indium and galium??



I must say that my sources are so varied

finally this image my block refine a first time on the right and the approximate state in which I received it.



still not easy to refine without XRF !!!!

to finish I will recover the x% of gold in the stock solution that remains.

Then we'll get to the money.

see you


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## Martijn (Feb 26, 2022)

I got a chance to read and look a little better beyond the gold boullion. Looking at the pictures, i have to say: be very carefull with the highly toxic pgm salts! 

You're doing this in the livingroom? 

Please get a dedicated space for this where nobody can get poisoned. 
Traces of these salts can have big consequences for your health and whoever is living there with you. 
Or the one that comes after you if it's a rental home for work. 
Look up the msds of the salts you're working with.


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## Abdoulapapatte (Feb 26, 2022)

Martijn said:


> J'ai eu la chance de lire et de regarder un peu mieux au-delà du boullion d'or. En regardant les photos, je dois dire : soyez très prudent avec les sels de pgm hautement toxiques !
> 
> Tu fais ça dans le salon ?
> 
> ...


Hello Martjin, the salts have been stored for an hour, I would say the time for the weather to calm down, and also the time to take some photos, we work outside most of the time, and in a ventilated space for melting with air extraction inside if the weather does not allow working outside

All the salt contaminants were then burned and calcined outside, the interior objects such as the glass table were drastically washed afterwards, unfortunately as you know yourself our region is not lacking in water and precipitation, the rains are proven .

at home I work outside or inside with an air extraction / filtration system I am currently redoing my installation

. To tell the truth, I may be going into a waste recycling project, I'm waiting to see what I'm offered as a job.....



I am located in Belgium in the Walloon region, originally from France Marseille, I will explore the borders and take a little interest in other countries for gold, there must be good exchange and business to be done


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## kurtak (Feb 27, 2022)

First of all - very interesting presentation !!!

You asked for comments - so here is my first comment based on the following picture & what you posted with that pic

You posted -----

I'm starting the gold castings and I'm starting them before the palladium one, because *my metal here is clean and I don't want it polluted* with the palladium.

Per the bold (red letters) in the above quote --- why in the world are you using what is very clearly a *VERY* dirty melting dish to melt your gold after you have gone to all the trouble to drop your gold - which should be relatively pure - if not pure (in other words when you drop your gold in the first place - it should be very close to pure with only VERY SMALL traces of impurity) --- & then go through the trouble to put that gold through the washes (HCl/water washing) *to get rid of any* *trace* contamination --- but then you take the gold you have taken the trouble to *insure* your gold is in fact pure - & then go & put it in what is clearly a *very dirty* melting dish which in turn ends up *contaminating* you pure gold with whatever *garbage* is in that very dirty melting dish 

In other words - there is a reason why your melted gold is coming out at only 998 instead of 999 (or 9999) 

it's because you are *contaminating it* when you melt it in that *very dirty melting dish * 

*Never* melt pure gold in a dirty melting dish --- always use a melting dish *that has never had anything* but pure gold melted in it

If you are melt pure gold - you *do not* need any flux of any kind - other then the borax used *to glaze* your melting dish before you use the melting dish for melting the pure gold

If you have to add flux when you go to melt your gold - then your gold is not pure in the first place - so - if you have to use flux to melt your gold - then there will be contamination in slag from that melt - once you have contaminated flux/slag in your melting dish - that contaminated flux/slag will also contaminate any gold melted in that dish after that

Kurt


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## kurtak (Feb 27, 2022)

Per the bold print (below) --- this is absolutely NOT the way to calcinate your DMG/Pd salt !!!

doing it this way (with a torch) is &/or will cause a good portion of you Pd to go up in smoke !!!

calcination of PGM salts (including DMG/Pd) needs to be done with the salts spread in a very thin layer in a fused silica or fused zirconium dish (Lou may comment & correct me on the dish) & it needs to be done at very controlled temps (380 C - or 717 F) or you will lose PGMs up in smoke --- using a torch like you are using is causing a fair amount of you Pd to go up in smoke - not to mention that smoke is VERY TOXIC 

now move on to makeshift melting here as for the quartation *I start by calcining the sponge with this type of burner*, not very efficient but the bottle lasts a long time for preheating.


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## kurtak (Feb 27, 2022)

This is NOT EVEN CLOSE to ready for melting --- if you try to melt that - a fair amount of your Pd is going to go up in smoke & that smoke is VERY TOXIC

ready to melt


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## kurtak (Feb 27, 2022)

You asked for comments so here goes 

Concerning the Pd --- if I understand right - the Pd you have in solution is what is left in solution after you have dropped you gold

you are then using DMG to drop your Pd

DMG - although yes it is true that it will drop your Pd - it is certainly not the best way to do so - for more reasons then I have time to post about right now

But just off the top & for starters - unless the solution is relatively clean to start with you are going to get drag down of other metals - especially Ni if Ni is in solution (which is why you are only getting 75% (plus/minus) Pd

Then there is the problem of "reducing" the DMG/Pd salts before going to melt - if reducing those salts is not done right you will suffer loosing some of your Pd up in smoke

IMO (In My Opinion) --- if you are looking to recover Pd (&/or other PGMs) from an AR solution after you have dropped the gold - you are much better off cementing that Pd (&/or other PGMs) from that solution with copper

Cementing PGMs from solution with copper is "a bit" more complicated then cementing silver or gold from a solution --- you can read about that in this tread here ------------









Fuzz Button Interconnects, need some advice


okay, back a while ago, I found a bunch of fuzz button interconnects... like the ones from this thread: http://goldrefiningforum.com/phpBB3/viewtopic.php?f=34&t=16018&hilit=fuzz+button&start=20 after doing some research on them, I was figuring on Be/Cu/Au wire was most likely what I was dealing...




goldrefiningforum.com





If you do the copper cementing right (follow the instructions in the above thread) there is no reason why you can't get your Pd back (plus minus) 98% & it can go direct to melt after washing & drying

If there are other PGMs in the solution those PGMs will also come down with the Pd --- as well as any trace of gold that may not have come down when you precipitated the gold

Kurt


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## Abdoulapapatte (Mar 1, 2022)

hello kurt thank you for your many answers, I think you must have a lot of knowledge that I don't have yet unfortunately , but you know what they say, knowledge comes by learning,



On the other hand, I can clarify certain points

1) for the crucible I know very well that it is dirty, here I melted my gold, I knew that there was something impurity left and I just didn't want to melt the palladium before the gold so as not to found with palladium in my gold it was the most important for me for the rest I knew that the palladium would not be pure at 100/100 because on being contaminated.

2) for the palladium sponge I think you are right, the sponge calcines, then crackles with yellow gas escaping from it, so there is a loss of palladium during the melting

Simple SOLUTION: I found that I could put a thick layer of borax, on top, so when I melt it, the borax melts first and will drip onto the powder, then it mixes with it, producing gasses. stop and the yellow smoke no longer comes out, I have the impression that it works quite well, if not to cook them at 380°C as you say I have to buy a light melting oven such as those with resistors inside. or else I will put it directly at melting temperature with borax?, can borax reduce this loss

3) for cemented palladium you are talking to me about copper powder, like zinc powder it will allow the cementation of Ag, Pd, Rh Pt, Au. For Cu it does not settle on it and remains in solution. In my opinion it will be very long, (even with heating + agitation + air bubble) , can you give me a time scale ? thank you

*kurtack an other question for you :*

Have you ever tried cementing on pure silver, since it is above copper in the red/ox scale I think it would be perfect, but a little longer, to remove Ag from solution then we could use HCL?

then go to aqua regia afterwards? (guess like you tell me.)

*I specify that I am French, I am in this very moment to make a translation of the book CM HOKES in my language, but that takes me enormously of time, and I am not yet on the chapter of platinoids.
so everything I do here, I learned it on my own, by looking at some post and by informing myself, so yes there are mistakes for sure, don't forget either that I put here, only part of my work and that I worked in a space which is not mine, and also that I did not have all my material =)!! important!!

Next time I plan to do this:*

with the same alloy I used for this experiment, or quite similar

0) I will no longer use copper, surely silver to make the base metal quartation, no more copper
1) hno3 65% alloy attack
2) filtration, I end up with a filtered solution and solids
3) addition of HCL in the filtrate and removal of silver filtration of silver chloride
4) once the silver has come out, this solution could contain the metal base, as well as the palladium dissolved by hno3 and surely other traces of platinoid.
5) I Denox the solution by adding sulfamic acid H3NSO3, it makes it possible to transform the excess of nitric into sulfuric acid, thus removing the excess of nitric and also of precipitate any lead still present in solution.
6) filtration of the lead with filter paper and recovery of the filtrate. lead output (Pb)
7) the DENOXE nitric acid solution and freed of all traces of lead and then placed in a beaker, the beaker is placed in a bucket containing water and ice (to cool the beaker and keep it at low T° ), you can add a magnetic stirrer,
8) we then add ammonia (20% 12% depending on what I have on hand) to add the ammonia, the reaction must be done with manual stirring, or with an electromagnetic stirrer to avoid the formation of "vokolen's salt" (precipitate purple if not enough ammonia added, or poorly stirred.
9) filtration if an unwanted precipitate forms
10) we then add 37% HCL, very very slowly add a little HCL stirred and wait then recommended.
11) by re-acidifying the solution which has become basic during the addition of ammonia, two important choices will be observed, a variation in color (due to the change in ph?) as well as the appearance of a yellow precipitate.
12) the yellow is called palladium Diammines Dichloride.
13) filtration ------------> yellow precipitate, placed in 1 beaker with water to cover it / heat

13) filtration ------------> filtrate + dmg + stannous test (search for traces of pd)
14) the yellow precipitate is therefore heated with a little water covering it. We then add formic acid, the salt turns black, we heat and add more formic acid until the black bubble is no longer formed when formic is added.
this black precipitate will therefore be pure palladium at 999.9 can someone confirm the purity obtained 999/1000

Do you agree with me that the result will not be affected by the copper and nickel present.
I put you a very useful link I find here the process comes from the youtubeur owltech (very good worker, as well as mr sreetips because technical + educational)
owltech palladium method 999/1000

*Question I ask myself:*
formic acid precipitate palladium only or will it also precipitate Pt, Rh, Ir........
do you see any problem in this process???





owl tech palladium refining technique




A very good day friends do not hesitate to criticize my work it is very important for me thank you.

if you have a person from the forum to recommend me, I'm interested, really a chemistry teacher would be the best thank you. for the rest I will soon recover my solutions from the process, I will see what remains as metal, I will do a little explanation on the recovery of silver
See you later friends



Ps: if you ever read this post, that you are a beginner, I would really be happy to help you and I promise, I will never make fun of your shortcomings, nor will I respond coldly. if I can help it will be with pleasure =) let's help each other.
Finally, you who are starting chemistry, do not hesitate to read, look for yourself before starting, the art of refining is long, tiring, sometimes thankless, extremely time-consuming, but with a lot of time, reading, and advice, believe me we are moving forward...............
goodbye


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## kurtak (Mar 2, 2022)

Abdoulapapatte said:


> *Question I ask myself:*
> formic acid precipitate palladium only or will it also precipitate Pt, Rh, Ir........
> do you see any problem in this process???



Formic is not a "selective" reducer so yes it will reduce other metals (PGMs &/or silver) if they are present with the Pd

Example; - here is a thread about reducing AgCl to silver with formic reduction









Silver chloride to Silver


Hello, I would like to change silver chloride to silver metal. I know that we can add it in caustic soda and then with dextrose obtain the silver powder. However, i would like to know if there is a way to disolve it in ammonia for example and then make the silver powder precipitate. My main...




goldrefiningforum.com







Abdoulapapatte said:


> 8) we then add ammonia



Be *VERY CAREFULL *using ammonia with metal salts whether those salts are metals dissolved in solution or metals that have been precipitated as salts

Ammonia plus (certain) metals (salts) can/will produce *HIGHLY explosive compounds !!!

Know & understand COMPLETELY* what you are doing when using ammonia in any refining process

This is all I have time for today

Kurt


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