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Are you sure that tin reacts with chlorine forming tin (II) chloride? I'm afraid you'll get a tin (IV) species (probably some basic oxochloride stuff) or relatively pure SnCl4' date=' which with the slightest contact with water is changed to SnO2 and HCl. The problem with tin is that the +2 oxidation state is quite unstable and very easily goes to the +4 oxidation state.

 

In fact, I have some SnCl2, but over the months it already is severely oxidized to some tin (IV) compound :-( , containing chloride and oxide (or hydroxide).[/quote']

 

Well, that and tin chloride isn't really soluble in organic solvents. It was tin iodide that I had read as soluble.

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Update:

 

the HCl and H2O2 that was electrolised with the solder ingots until the anode dissolved, and left over night, was still a white gell like gloop this morning, I`de added sulphuric acid and it eventualy started to "Split", leaving a clear liquid at the top and the gell stuff to sink slowly, I`m now filtering this (it`s taking forever! 1 drip every 15 secs now) but filtered liquid is nice a clear though.

if I get time today, I`ll electrolise this with carbon electrodes and see what (if anything) comes out of sollution.

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I may have found a solution for separating tin and lead. I did not try it personally, but it looks reasonably.

 

I take a quote from another forum:

 

A few weeks ago I was working with that same type of solder (60Sn/40Pb). I managed to create spongy lead and tin(II) chloride, both of reasonable(I think) purity. First this solder was melted and cast into electrodes. I then electrolysed a saturated solution of sodium chloride using these electrodes. The electrolysis was continued till the electrodes had both decomposed completly(I switched the polarity once one electrode had dissolved). The tin was in solution as tin(II) chloride, tin hydroxide had also precipitated, and any lead present was instantly plated out due to it being a more powerfull oxidizing agent, thus a higher reduction potential. It was necessary to scrape the lead that was plated out off the electrode many times. The mix was a dirty grey. I added some HCl(till litmus indicated the mix was slightly acidic) and the mix cleared up.

From here the mix was filtered, the filter kept the spongy lead. I am unsure of the purity of this lead however. To the filtrate was then added baking soda to precipitate tin(II) carbonate. The tin(II) carbonate was washed, dried and dissolved in a slight excess of HCl.

The solution was allowed to evaporate and a nice crystalline solid was obtained, tin(II) chloride.

 

What this person achieved was making tin (II) chloride. I did not try this personally, I just wanted to mention it at this place. No special chems required and no special equipment required. You might give it a try.

 

BTW: the source of this information is science madness, search for 'tin chloride' in the forum's search page and the link will pop up.

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Splendid info and Thnx, be sure that If this current experiment fails, I`ll be doing that one next :)

 

atm, it`s stil drip drip drip, so it`ll more than likely be tomorrow that I`ll get chance to find out (I`m quite busy at weekends, so we`ll wait and see) eitherway I`ll post my results :)

 

thnx again Woelen :)

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well it`s now tomorow and the electolysis is happening, on the cahote is a Clear buildup of a light grey coating, the anode is slowly falling appart too, the liquid is now a blackish color (probably down to the carbon rods) I`m getting gas of Both electrodes now (probably too much sulphuric acid) and there`s not a whole of metal being produced at all :(

I expect alot of the Tin salts were in the filter paper "Gloop" I threw away.

I`m ceratainly far from the 200mg of Tin metal that I need, the voltage is a little higher too, I`m running at 3.25 volts, it`s the only way I seem to get this grey cathode coating effectively.

it is building up in thickness slowly, but nothing appreciable, it`s been running for over an hour and 20 mins thus far.

 

Could this coating be a little bit of Tin metal?

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So youre kind of doing what I was thinking of b4?

lol.

Making tin chloride then ele-y it out?

:)

I take it the lead is plated first?

Then you will get tin after?

 

aha at least I was thinking along the right path, :P

I may try this may self now.

 

O you couldnt just add you metal to bleach to make it could you?

:(

My brain hurts, :D

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Could this coating be a little bit of Tin metal?

Yes, I think that this will be mainly tin. As I understand, you added dilute H2SO4 to the liquid with HCl and H2O2. This means that you precipitated almost all lead with the sulfate ions from the H2SO4. However, before adding the H2SO4, you almost precipitated most of the tin also with the H2O2, by oxidizing it to SnO2.

 

So, I can explain quite well why you hardly get any metal at the cathode and why you get gas at both electrodes. This is, because there hardly is any metal left in the clear liquid. If you have added sufficient H2SO4, then you removed virtually all lead (PbSO4 is highly insoluble) and apparently a small amount of tin remained in the liquid, so you get a very thin layer of tin, but mainly hydrogen gas at the cathode.

 

The yield of this method, of course is terrible.

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agreed, it was very very little.

 

I`m current electrolising the solder ingots in the NaOH soln, it seems to change its dynamics frequently and then "settle" into a "routine".

at 1`st both anode and cathode went dark and the Catode was bubbling away nicely giving off hydrogen, this stopped a few times though and I had to clear a dark grey spongey material off the base of it, then it would start up again, I`ve done this 3 times and now it`s running as normal.

the anode is really strange, that`s coated in a white powder and the whole bottom of the electrolysis vessel has been covered by a 6mm layer of it too.

the anode has reduced in diameter by a couple of mm so far (that`s encouraging).

and the distinct lack of Chlorines stink also makes a pleasant change from typical electrolysis of house salt :)

 

only problem is, I`ve realised that I`m completely out of Baking soda (I used it all the last kitchen fire we had).

 

now the cathode is still fizzing, but there`s no deposits being built up any more?

it can`t have gone to completion Yet, it`s only been on 35 mins?

 

edit: I assumed it was finished and carried on to the next part, I stired the white mix and Underneath was the grey stuff! invisible due to the white layer on the top, so it`s Possinle that the conductive layer of metal under it was stopping the electrodes working properly, the HCl has cleared it all un too! :)

all I have is metalic sponge and metalic particles in a clear liquid, that`s just this sec finished filtering, the results are great so far, now All I need to do is wait until I can go out and get some bicarb.

 

this method gets a full thumbs up so far! :)

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I`m current electrolising the solder ingots in the NaOH soln,

The original method I gave was with NaCl-solution.

With the NaOH I indeed can imagine that you get a lot of white stuff (being insoluble Pb(OH)2 and SnO2) from the anode. I however, cannot explain how you ever can end up with grey metallic particles plated at the cathode if you use NaOH.

With NaCl of course, this can be explained quite well, because Pb goes in solution as Pb(2+) ions, but in NaOH solution things are totally different.

 

Can you give a little more details about your setup with the NaOH-solution? Maybe it forms plumbate ions? But these are anionic, so how would these be reduced at the cathode?

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LOL, sorry, I meant NaCl, it was a typo on my part, I was probably thinking of the next step not having any Bicarb and wondering what else could be used. Appologies.

 

turns out that we`re going to go out in a min and get some :)

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well the Bicarb worked like a charm, plenty white precipitate like some sort of frothy milkshake on steroids!

it`s a very very fine precipitate though, some of it passes through the filter in the 1`st few seconds, I probably need a finer mesh next time.

I`ve run out of HCl again, so I`ll go make some in a bit, the little I did have left when added to this white precipitate fizzes just the same as the bicarb, so all seems to be on track thus far :)

 

edit: acids been made and used, the precipitate is dissolved and now being electrolised with carbon rods at just over 5 volts, and WOW!, from the catode you can actualy see the shiney metal "Fingers" form and spread towards the anode, they look like snowflakes do up close, but Very Flat, they form fast enough to cover exactly 2 inches across the tin 2 chloride soln in a little under 3minutes, it takes longer the more I keep removing.

 

now I know the whole procedure works 100%, I`ll scale it up next time and try to get at least a Gram or 2 of tin metal, thus far I have about a quarter gram on this small scale, hopefully when complete I`ll have enough to make up my 10% needed for my 2 thirds complete Gallinstan alloy :)

 

Thanks again Woelen :)

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Something REALLY strange is going on now? Woelen you`ve just Got To try this!

 

follow the procedure as outlined, then replace the carbon rods in the tin 2 chloride soln with the Solder ingots again, then add super saturated NaCl soln to make up 2x the liquid volume.

 

the whole reaction goes Backwards!

 

this time the Cathode is being "eaten" away and Tin Metal is coming out of Soln! and at the Anode there`s is a deep black deposit, there is No white precipitate or grey material?

the soln is still quite acidic.

 

the catode metal when heated reacts with the air, and tiny balls of pure shiney metal form leaving a yellow grey powder behind, the same thing that happened when I made the normal tin and heated it in a test tube, it orange glowed that spread and left tiny metal balls, I`ve tooth tested these sphere`s and they creak and squeek the same as Tin metal does, and they`re quite hard, much more than lead.

 

any idea WHAT is going on here????

 

edit: the damn thing`s taken another Shift again, the Anode has now shrunk with a thick layer of this jet black deposit coming off, the cathos is Still "growing" metal crystals, and has Now decided to stay the same size, eaten away, but holding at that point.

my only guess is that my original tin chloride soln wasn`t entirely exhausted yet, but there`s STILL no white precipitate to be seen, and unless this jet black almost oily sludge is the lead, I`ve no idea where the lead`s going !

LOL, one of you guys has Seriously got to try this yourselves, it`s crazy :)

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I'm going to try it, but I'm following what you do first, :P

Well as I havent any hydro acid.

 

Yt is it giving off Cl gas?

 

How do you make Hydro acid?

I'll start a new thread about that, :)

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there`s no Cl gas produced making the Tin(II)Chloride.

there is only a trace amount when plating it out with the carbon electrodes afterwards' date=' but you`ll hardly notice it.[/quote']

Yeah thats what I was thinking, the CL isnt made when 'burning' the tin/lead rods as thats binding with the tin etc.

 

Tin is easy to eley out but I'm not sure what would happen to the lead.

I was thinking if only the tin was changed to chlorids but the lead wasnt then that would just mix with the water, then filter out that stuff and you should have a mix of tin chloride and lead gel.

but wouldnt this lead react with the sodium hydroxide?

or are you making bot tin/lead chlride?

 

Then you make the Na(OH) ph7.

 

I'm just trying to figure why you doing it the way you are, :) best way of learning. :D

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Something REALLY strange is going on now? Woelen you`ve just Got To try this!

....

 

Could you summarize in short, step by step, what you did? Start with the NaCl solution and the molten electrodes of tin/lead solder. From that point I would like a step by step description. I have quite some idea what you did, but in order to repeat what you've observed, I think we must be very precise in describing what happened (e.g. voltages, concentration of solutions, precise order of actions, precise description of precipitates and also at which steps you obtained them, etc. etc.). I'm in for trying this also.

So, if you make a step by step description, then I'll try to repeat it next weekend, then I have some hours for such a lengthy experiment.

 

My experience is that even with simple "garage-chemistry" people can discover VERY interesting phenomena. I already have puzzled professional chemists a few times with simple plain reactions, just have a look at the riddles section of my website:

 

http://woelen.scheikunde.net/science/chem/riddles

 

I asked these questions at Usenet/sci.chem, at a Dutch forum of acedemic chemists and in personal communications with two university employees. Only the sulfite/iodide riddle is resolved so far, the others still are open more or less. So, with your tin experiments, there may also be something interesting, which cannot be explained with basic highschool chemistry or even beyond highschool chemistry.

The appealing thing of these riddles is that they can be repeated with such simple equipment and simple reagents.

 

Maybe your experiment can be added to this? Even better would be an explanation.

 

I'm looking forward for your as precise as possible reproduction of all steps taken by you.

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Certainly :)

 

1`stly I did everything as outlined in your post #53, with the exception of crystalising out the Tin(II)Chloride, I left that as the soln and then plated out the tin metal 4 times with carbon electrodes (there was still plenty tin chloride left in soln when I stoped).

 

then I decided to put the solder ingots back in place of the Carbon rods to see what would happen. I had roughly 80ml of soln at this time, and realised I didn`t have any NaCl soln in there, so I boiled a kettle, while that was boiling I added several tables spoons of salt to the bottom of a flask, poured on the boiling water to 100ml, and strired like crazy until no more would dissolve, I then added this to my 80ml tin chloride, I managed to pur in about 80ml of this salt soln before it became too full.

 

I was plating at roughly 3 volts.

 

I reaslise this is only in rough for now, I plan on doing the same thing all over again, from the start, I`de like to see what`s going on too, was it a contaminant? a Fluke? or something perfectly explainable?

I have an Idea, I think Both the lead And the Tin is being plated out, but not as a eutectic mixture anymore, I think it May have something to do with the Voltage, as the cathode was only just fizzing, and the material that came off it would go like stiff bubblegum when moved and almost solidify, as if it were a liquid metal cooling.

 

basicly I need to do a whole range of experiments and keep notes, I want to try acidulated NaCl soln and the 2 ingots at the same voltage see it that`s got something to do with it, I also need to test this metal that formed when I heated the product, I had a yellow grey ash and a silver metal, that makes a creaking sound when bend or bitten (typical of Tin) I`ve also done a scratch test, it`s harder than lead alone, and harder than the solder I used to make the ingots, but the same hardness as my Cast ingot (electrodes).

 

like yourself, when I get another quiet day, I`ll start all over again, read my posts and follow my rough steps, but keep measures etc...

then hopefull we`ll be able to replicate this and Someone will have an answer as to what`s happening :)

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I was just thinking.

When you use lead/tin rodes when doing electrolysis on the salt water.

You would get:

lead chloride

tin chloride

And sodium hydroixde.

Would this then displace to give

 

lead hydroixde

Tin hydroxide

sodium chloride

?

Thats what the white stuff is isnt it?

:/

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ok, Woelen.

 

1`st things 1`st, in your replication of this experiment, being saturated or Not with NaCl soln is not essential, neither is the Voltage, I`ve tried All combos and all works just the same, only dif is that some are faster than others.

 

solder ingots in almost Any reasonable conc of NaCl soln and any voltage between 17V and 2.5v is going to work.

my psu is rated at 5A continuous and 7A surge 0v-36V.

 

you Will find that if your electrode touch the Base of the vessel, that a conductive layer will form UNDER the white preciptate! you`ll NOT see it!

and will stop the reaction and probably danage your PSU! (I`m sitting by mine reading the meter so nothing can happen unless I take my eyes off the ball.

 

thus far All is going exactly the same as it did 1`st time I ran this.

 

oh yeah, and you`ll need to cranck up the voltage after about 4 mins, the bubbles at the cathode slow to an almost stop, the Anode gets warm and you DO get lead metal at the cathode (eventualy).

 

that`s about it for now :)

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no, not really, this reaction`s still running, I`ve had to change electrode a few times (swapping top to bottom for more metal etc...)

 

all`s still running the same as it did last time, only dif is. is that after a time the dark grey stuff comes to the top, and the thick white ppt seems to dissolve at 17v, so I`m at about 10v now, but nothings altered.

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I'm lost one whats happening, (sorry I've read the thread,)

Ignore my comment about the sodium hydroixde and tin chloride deplacing (silly me)

So wouldnt the tin electro out first?

As the lead is lower (reactive) but the tin would.

So wouldnt the lead just drop out?

 

so you would have sodium hydroixde and tin chloride in water soln. but how to remove the sodium hydroixde.

an I following this right?

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I tried that way back at the beginning of this, I get a Gell Gloop :(

 

thus far the reaction as stated above is complete, and all the data there is Sound.

Ive done the HCl bit, it`s started to work, but I ran out AGAIN.

nothing`s lost though, I`ll just have to wait until I get another quiet period before I can make some more (oh yeah, and I got My sodium Nitrate back so, I`ll be making some Nitric acid too).

 

as for now, all`s at a stop.

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