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it seems to be a moot point anyway now, the metal precipitate that the Mg displacement is producing, it being destroyed shortly afterwards leaving a white gell like material again and a white precipitate, fortunately I have a good 100ml left, so I`ll try plating it out of soln using carbon electrodes, Mg displacement is Not working.

so there`s yet Another way Not to do it :)

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it seems to be a moot point anyway now' date=' the metal precipitate that the Mg displacement is producing, it being destroyed shortly afterwards leaving a white gell like material again and a white precipitate, fortunately I have a good 100ml left, so I`ll try plating it out of soln using carbon electrodes, Mg displacement is Not working.

so there`s yet Another way Not to do it :)[/quote']

lol. Well at least you learn something new everyday!!

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well... after making a huge Chlorine breathing black sponge monster at the anode, I did manage to get Some product at the cathode (shortly before the glue gun plastic melted) it`s not much, probably about the size of a match head when all squashed down, but it`s a grey sponge like material and it`s quite heavy as it sinks rapidly when I washed it in the test tube of water, I just cant tell if it`s Lead or Tin now, I do rem the lead product having a shiney metalic crystaline appearance, and this is perfectly dull and dark grey???

 

any ideas how to test without using Much of it up as it only made a little?

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1. dissolve solder in HCl to form a mixture of of PbCl2(aq) and SnCl2(aq)

2. then add some sulphuric acid and you should start to get a precipitate of PbSO4(s)

3. filter the lead precipitate and you should be left with a solution full of tin salts

4. electrolyse the hell out of it.

5. scrape off the tin.

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the Sulphuric acid route is interesting, I considered doin that but without the HCl step 1`st (just the solder in the acid and electrolised).

I`ll do your idea next then, as it seems a pity to waste this tin/ (and probably some lead) Chloride mix.

 

I`ve also added some 50% sulphuric acid to the grey product I obtained in my last post and heated it, it seems to have formed into a little spongey ball now, there wasn`t any noticable reaction either (yet) but there is a grey precipitate just bellow this ball and the rest is a clear liquid.

 

so I`m still non the wiser LOL :)

 

edit: i just added some more acid as the product was already in water, now on heating the ball floats and there are bubbles being formed in the ball causing it to bob up and down, so Some sort of reaction is taking place, just Very slowly, the precipitate is quite marked too :)

 

edit(2): I took this ball of "Stuff" out of the acid and flatened it between 2 sheets of glass, then heated it with a 100w gun type soldering iron, some tiny metal balls appeared then in an instant Ffft there was a sound and a tiny flash and the product was glowing orange inside and cooled leaving a white powder (probably an oxide)???

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Keep in mind that tin does not dissolve in hydrochlorid acid at any appreciable rate. A mix of tin and lead probably also does not dissolve easily. PbCl2 is quite insoluble and tin does not react at all with HCl.

 

I tried personally dissolving tin and it is really slow

 

The following may be interesting info: Google groups -- thread on tin

 

Testing whether a piece of metal is lead or tin is easy. Dissolve in conc. HNO3 and then dilute 10 to 20 times. If there is tin in the liquid, then a white precipitate is formed of SnO2. Add a solution of KI to the diluted liquid (whether this contains white precipitate or not does not matter for the test on lead). If there is lead in the liquid, then a beautiful bright yellow precipitate is formed of PbI2. So, in one go you can detect the presence of tin and the presence of lead.

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Thnx, Interesting about the H2O2 addition, I`ve just put some of that in the electrolyte as well now :)

I`ll wait until this last peice of solder has broken down in the HCl/H2O2 soln, and then leave it for a few days, Hmm as long as it`s taken me to write this, the soln has taken on a milky apearance and has thickened up to that Gell stuff again?

 

Soooo tempting to give up and just buy some :(

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Thnx' date=' Interesting about the H2O2 addition, I`ve just put some of that in the electrolyte as well now :)

I`ll wait until this last peice of solder has broken down in the HCl/H2O2 soln, and then leave it for a few days, Hmm as long as it`s taken me to write this, the soln has taken on a milky apearance and has thickened up to that Gell stuff again?

 

Soooo tempting to give up and just buy some :([/quote']

 

No dont give up!!!!

1001 ways to make milky gel. :D

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Thnx' date=' Interesting about the H2O2 addition, I`ve just put some of that in the electrolyte as well now :)

I`ll wait until this last peice of solder has broken down in the HCl/H2O2 soln, and then leave it for a few days, Hmm as long as it`s taken me to write this, the soln has taken on a milky apearance and has thickened up to that Gell stuff again?

 

Soooo tempting to give up and just buy some :([/quote']

Oh no... again you get the tin (IV) species :eek:? If you get that, then I would suggest you stop with it, because you cannot process it easily to make tin metal. As you may have experienced, tin is not easy to deal with at all.

 

As a last resort, if you have some of the SnO2 stuff, then you could try the following:

 

Dilute with water and let it settle at the bottom (may take several hours).

If you have a lab centrifuge, then use that.

Decant the clear liquid above the precipitate.

Add new HCl to the liquid. Now you have no (or just little) remains of H2O2 and lead-salts left.

Add some solid Na2SO3 and heat gently, but assure that the liquid remains highly acidic with HCl. The liquid is quite reducing now and you may see the gel dissolve. If that happens, then you can conclude that the tin is reduced to its +2 oxidation state and you have a solution of SnCl2 in HCl. If the sulfite does not work, then a stronger reductor may be needed, but I'm afraid you'll have to use powerful stuff like borohydride or dithionite in that case.

If the SnO2 dissolves, then boil the liquid for a few minutes to get rid of all SO2 from the sulfite and then carefully add NaOH in order to make it less acidic. Keep in mind though that Sn(2+) is very prone to hydrolysis and very easily forms a precipitate of basic salts and also is very easily oxidized to its +4 oxidation state when it becomes alkaline.

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I think I`ll start again in that case, I seem to be screwing up left right and center with this "seemingly simple" project/task I`ve set for myself.

 

I don`t have any of those reducing agents you mention either, there HAS TO BE a way to obtain Tin metal with reasonable ease, maybe using solder is a red herring?

the 60/40 Tin Lead looks So tempting at face value as a source, I`m begining to wonder now if it`s such a "great source" after all?

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I think I`ll start again in that case' date=' I seem to be screwing up left right and center with this "seemingly simple" project/task I`ve set for myself.

 

I don`t have any of those reducing agents you mention either, there HAS TO BE a way to obtain Tin metal with reasonable ease, maybe using solder is a red herring?

the 60/40 Tin Lead looks So tempting at face value as a source, I`m begining to wonder now if it`s such a "great source" after all?[/quote']

From a practical point of view, the Emovendo/eBay-way is the best. Very pure tin at acceptable cost... at the same time you can buy yourself some other elements as well.

 

Of course, from an intellectual point of view the Emovendo/eBay-way is not satisfactory at all. It does not give that sweet feeling of victory and mastering of the elements :D:rolleyes::D .

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Ive been soldering for about 1 year, and the only solder i use is silver solder. It is about 3% solder, and 96% tin and 1% copper. i ve colle cted every single scrap thats ever dripped. Now i have a huge puddle of silver solder. How would one seperate the silver?

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for the silver I`de dissolve the lot in nitric acid, then precipitate the silver out with a soluble Chloride and filter, the White stuff will be your silver chloride, heat or UV light will turn it back to silver metal again.

 

anyway this is Off Topic, make a new thread about it and we`ll help in that one too :)

 

as for carbon and heating it, I`m not sure, it doesn`t sound that simple in all honesty as the metal won`t sublime or boil at any temps I`m likely to acheive in a simple Lab.

 

and yeah Woelen, I can`t admit defeat JUST YET, it MAY defeat me in the long run, but I`ll have tried, and will be able to help some other poor sod that thought the same as me eventualy (I got alot of my information that way in the 1`st place, EXPERIMENT!).

 

I hope it does work, as I`m not after huge amounts, a quarter gram and I`de be happy :)

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Yt is you do manage to get tin oxide without lead or sorts init and dont want it etc etc, send it my way I'd have a go at smelting it and send it back to you If I do it.

I've got a furnace I'n my back yard. :)

(Homemade btw)

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I have the bricks to make a coke furnace too, it`s just that this year whith having the little one and all the attention that entails, I`ve not even had time to do all the weeding that I`de have liked to have done even, never mind build my furnace and Cold Smoker for my garlic and chilis etc...

 

thnx for the offer any way, but it would be just as easy for you to replicate all this at home and save the postal money, besides, I`de rather not send nameless "Gloop" through the postal system :)

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I have the bricks to make a coke furnace too' date=' it`s just that this year whith having the little one and all the attention that entails, I`ve not even had time to do all the weeding that I`de have liked to have done even, never mind build my furnace and Cold Smoker for my garlic and chilis etc...

 

thnx for the offer any way, but it would be just as easy for you to replicate all this at home and save the postal money, besides, I`de rather not send nameless "Gloop" through the postal system :)[/quote']

lol

Good point about the the blob. :D

I thought you lived in a flat and so didnt have a garden, I didnt in my old flat. :(

 

I've not got any of the chem that would be needed, but I will one day, :D

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If memory serves me right, isn't SnCl2 mostly covalent in terms of the bonding? I swear that I remember reading about how tin chloride is soluble in organic solvents. Is there anyway that you can take your tin/lead molten alloy and pass a stream of chlorine gas over it to convert everything into the chloride, then dissolve the mixture into an organic solvent. The lead chloride should remain insoluble in the organic phase while the tin chloride would readily dissolve. You then evaporate the organic phase which would leave you with relatively pure tin chloride. You could then melt the salt down and electrolyze it which should leave you with pure tin metal.

(Then again, that could have been tin iodide that I was thinking of).

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Hmmm... it MIGHT come to that, and yes I could do that proceedure without problems.

BUT...the organic solvent????

 

what are you thinking here, I`m limited to basics there namely; diethyl ether, acetone, methanol, ethanol, octane, parafins, naptha etc .. (the basic stuff).

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Okay, thinking back it is tin iodide that is soluble in organic solvents. What you could do is take your tin/lead solder and dissolve into a nitric acid solution. When the entire bit of solder has dissolved, start adding potassium iodide to the solution. At first some HI may form, but eventually all of the tin and lead will form their insoluble iodides. Now you just filter the insoluble iodides and add it to some distilled water. In a separatory funnel, mix the water/iodide mixture with some organic solvent. The tin iodide should separate into the organic layer. Now just remove the organic layer and let it evaporate. You should now have pretty pure tin iodide which you can melt and electrolyze into tin metal and iodine.

 

Basic organic is all you'd need. Acetone would probably be the best method. Try it on a small scale first, however, to see if it works.

 

edited by me ya lazy git, don`t double post, use the EDIT button in future! LOL :P

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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, 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).

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the white gel could be tin hydroxide or tin oxide(i think). perhaps tin oxide since it only formed when you added H202 although i can't be sure. try using more concentrated HCl.

It is tin oxide, but with tin in the +4 oxidation state. Remember, oxides at high oxidation states usually are not basic and need not react with acids. Tin (IV) oxide is a notorious example of a rather inert oxide. It can be dissolved in strong bases, however, where it acts as an acid and in solution it forms stannate (IV) anions.

 

Other examples of metal oxides which are acidic are chromium (VI) oxide, CrO3, vanadium pentoxide, V2O5 and molybdenum oxide, MoO3.

 

If tin (IV) oxide dissolves in HCl, then that is not due to an acid/base reaction, but due to a coordination reaction, where chloride ligands replace the oxo-ligands.

A nice example, where this reaction is strong is with mercury (II) oxide. This dissolves in an excess solution of KI, forming HgI4(2-) ions and the solution becomes alkaline. Unfortunately this effect is not strong with tin (IV) oxide.

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