Tin (Sn) Metal

[YT2095]

no-one took it from me, I left it at another place a mile or 2 away.

 

the "Gloop" is just that, it`s the entire liquid, it became gell like. addind water just made it worse at 1`st, then it started to "thin out" and become managable in the way of pouring/filtering it.

 

it really isn`t the way to go, the NaCl for simple basic experimentaion is all that`s needed and seems to work great so far.

all I need to do is replicate the same again and do what I did last time and keep notes, and hopefully replicate the same happenings again

[jsatan]

aha, I think its finally clicked.

I've re-read the thread,

Yeah in that information about the guy who made tin chloride. He said he "switched the polarity once one electrode had dissolved" huh? you only have one electrode left, I take it he replace it with a carbon rode?

I get whats going on here, now.

But im not sure how he got from tin carbonate to tin chloride?

 

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.

Or was he making too soln?

:? sorry for all the questions.

[YT2095]

the addition of the HCl to the Tin Carbonate will make the Tin(II)Chloride and give off CO2 gas.

he then evaporated this soln until it formed the crystals.

 

and yes the solder electrode at the Pos side (anode) does dissolve. but before it`s "eaten away" entirely, you swap them over so the othe one starts getting "Attacked" thereby ensuring you waste nothing

[woelen]

YT,

 

The next weekend I have some time to experiment with the tin-stuff. I'll try to perform an experiment in a very controlled environment at a micro-scale and see what happens.

 

Especially the conductive layer under the white stuff is really intriguing. I'll see if I can manage to create a conductive bridge between the two electrodes. I've made such a thing once before from a solution of lead acetate. Really spectacular to see it grow.

 

The black stuff at the anode also intrigues me. I almost have the idea that the polarity of the electrodes was reversed for a while, so I'll certainly check out that. The black stuff certainly can be metal. Think of a precipitate of silver metal. It also is deep black. Look at B/W pictures, the black image is due to small silver particles. Many metals, especially if spongy, have a black appearance (I have tried and confirmed this with Pd, Ag, Ru, Co and Ni).

 

As soon as I have some interesting results I'll let you know.

[woelen]

I did some experiments, trying to repeat YT's results. I used all reagent-grade chemicals, except the soldering wire of course. Even the sodium chloride was reagent grade in my experiment in order to rule out all kinds of impurities.

 

Well, if I electrolyse with both the anode and the cathode, made of soldering wire, then a lot of hydrogen gas is produced at the cathode and the anode dissolves. You can really nicely see the difference in refractive index of the tin (II) salt and/or lead (II) salt, sinking to the bottom from the anode, and the solution of the sodium chloride.

 

After a while, when hydroxide, formed at the cathode, diffuses through the entiry liquid, a white precipitate is formed. At the anode, now a white precipitate is formed directly as well. I performed this experiment, until the anode broke into little parts.

 

At this stage, I had a white turbid liquid, with a lot of dark grey stuff lying at the bottom. It looks as if only the tin-part of the anode dissolved, the lead remaining as porous metal, which falls off as dark grey particles. So, indeed, you get two kinds of precipitate: white tin (II) hydroxide, finely divided in the liquid, and metallic lead, lying as a heavy and compact precipitate at the bottom. This most likely is YT's conductive precipitate, which at first was not noticed.

 

I swirled the liquid somewhat and waited a few seconds. This causes the darker particles to sink to the bottom very quickly, the white precipitate remains floating around in the liquid.

 

I decanted the white turbid liquid in a separate glass and added a small amount of hydrochloric acid, such that all of it dissolved.

 

Now I did another electrolysis, with both the anode and the cathode made of soldering wire. Now, again a gas is produced at the cathode, but when the voltage is adjusted carefully (to appr. 1.9 volts), then hardly any gas is produced, but a metal is plated. This metal forms a cohesive mass, which sticks to the cathode. The anode slowly dissolves again.

 

I stopped electrolysing at the point, where the metallic stuff has grown towards the anode almost completely.

 

Next, I took the cathode and anode from the liquid. I made pictures of them and attached them to this message. Look at how shiny the piece of metal is, which is attached to the cathode (the thick blob of metal, which almost reached the anode in the second electrolysis experiment).

 

I took the piece of metal and dissolved this in 50% HNO3. The liquid becomes a little turbid (apparently some SnO2 is formed). I diluted the liquid, such that it is not oxidizing anymore, due to high-concentration HNO3. Next, I added a solution of KI. Only a very weak ultrafine crystalline yellow solid was formed. This indicates that only a very small amount of lead was present in the plated metal. I also included a picture of the very fine yellow precipitate of lead iodide. I'm quite sure, that the metal, plated out at the cathode, contains at most of few 0.1%'s of lead, otherwise I would have had a much thicker and more coarse precipitate.

 

Next, I did the same experiment with the clear liquid, in which I did the electrolysis. This did not give a positive reaction on lead at all! After addition of KI, this liquid remained colorless.

 

I did a counter experiment with just a tiny amount of lead acetate dissolved in a lot of water and adding the KI-solution. Now I get a thick bright yellow precipitate of PbI2.

 

Both the electrolyte and the plated metal hardly had any lead. The lead apparently falls to the bottom as the dark conductive stuff, while the white stuff is Sn(OH)2. When lateron some acid is added (not too much, just enough to dissolve the Sn(OH)2), then it can easily be plated onto the cathode.

[jsatan]

aha, I've done almost what you did but missed a few things out.

I electrolysed my solder.

I got the same dark grey at the bottom (which falled of the node give off hydrogen.

I got a white matter from the other electrode.

 

No chlorine gass just hydrogen being given off.

 

I dont have any HCl so I couldnt add then.

But I replace the elctrodes with carbone I got chlorine gas and very slowly a dark matter. This looked just like the Pb.

But I was using a much high voltage, 7.5 I think.

 

So I need to get my voltage lower then that is needed to split sodium chloride.

Or use less salt and use just enough to eat the solder.

 

I'm still not sure why you need the HCl.

:/

[woelen]

I got the same dark grey at the bottom (which falled of the node give off hydrogen.

I got a white matter from the other electrode.

Both the dark stuff and the white stuff appeared at the SAME electrode' date=' being the anode. The white stuff is due to formation of SnCl2, which immediately is precipitated by the presence of OH(-) ions in the solution.

The black stuff most likely is the lead, contained in the solder wire. The tin dissolves and the lead remains as a porous solid, which falls from the anode.

The cathode hardly is attacked, it looses some of its shiny appearance.

 

No chlorine gass just hydrogen being given off.

Indeed, no chlorine gas. The anode material is more easily oxidized than the chloride ions in solution.

 

So I need to get my voltage lower then that is needed to split sodium chloride.

Or use less salt and use just enough to eat the solder.

No, not use less salt, but indeed lower your voltage. The tin ions are reduced more easily than water molecules. If the voltage is too high, then hydrogen gas is formed, together with tin metal, but this makes it hard to get a nice cohesive piece of metal, due to the disrupting bubbling. With a lower voltage, only the metal is plated out. This, however, only works nicely, if the liquid is clear and slightly acidic, otherwise you don't get a nice clean metal, but some impure black crap.

 

I'm still not sure why you need the HCl.

The HCl is needed to dissolve the Sn(OH)2 and making the liquid nice and clear again. Without the HCl, you may be able to plate out the metal, but you'll also include lots of other insoluble things. This is the reason that you don't get a nice shiny metal at the cathode, but some black gunk instead.

 

.

[jsatan]

cool. Thanks for the info.

lol

I knew I was thinking right when I said about if there was tin chloride it would deplace into tin hydroxide.

But no told me, lol

[YT2095]

Woelen from that point do the NaHCO3 neutralisation, fitering and washing, then add the HCl again to the collected material.

with the Hcl in slight excess, plate the tin out with carbon electodes, but not to it`s entirity.

Then use the solder electrodes again, and add strong NaCl salt soln to it.

it`s from This point that I noticed all the "Strange" stuff happening as posted a little while ago.

 

I still need to get some time to make more HCl, and weekends are major busy times for me, So I`ll pck up again with my half finished replication probably during the next weekdays.

 

so far your results are the exact same as mine were, Text Book stuff )

[woelen]

I still need to get some time to make more HCl

This really surprises me! You have to make HCl. Where do you live, that you cannot simply buy it???

 

YT, I'll try the next step with NaHCO3 as well. I'll keep you informated about that.

[Alchemist]

Yt2095, about your question of which one comes first in reactivity Sn or Pb, well:

If you have a solution of Pb 2+ ions and you placed Sn(s) in it you will get Sn 2+ ions with solid Pb.

However if you have a solution of Sn 4+ ions and you placed Pb(s) in it you will have solid Sn, Pb 2+ ions and Sn 2+ ions!

 

A solution of Sn 2+ with solid Pb placed in it, nothing will happen!

[YT2095]

Thnx Alchemist

 

Woelen, I`m in the UK, and I`ve never happened across it anywhere, that`s not to say it ISN`T available, it`s just that when I`m in a place that might sell it, I never think about it, and when I think about it...

 

well you know how it goes

 

edit: I`ve been out today on a mission to buy some HCl, I bought a Gallon of it (greater than 20%) for £3.91.

I`ve completed my dissolving of the tin chloride, and then came the addition of the sodium Bicarb.

Never have I seen such a mess in all my life! the damn stuff contains detergents! (so I thought). turn out that the HCl I make in a "normal batch" isn`t quite as conc as this stuff I bought, it`s closer to my Conc batches I make, so adding the quantity of Bicarb as I can with my "Normal batches) just makes it go crazy!

it didn`t help having the tin chloride get really conc by evaporation over the last week either (half volume) so there was plenty "White Stuff" in the bubbles too.

[jsatan]

Where you get your Hcl from YT?

after i move in a few days time I've placing my self a order for a few of staple chems, its about time I got around it it,

 

O btw,

I did the normla thing of zapping some solder with salt water.

I then added some phos acid until ph7 or slightly lower then zapped it again, I got some tin I think, hehe.

[woelen]

I'm surprised to read that HCl is not that common in the UK. Over here you can buy it almost everywhere, in 10% and in 30% concentrations.

 

@YT: Detergents? Did you means that is in some of your chems, or is it just looking as if there are some detergents in your chems.

 

If you have 20+ % HCl, then you have decent stuff. It is of moderate concentration, but enough for many experiments. Is that liquid colorless or somewhat green?

 

I have a bottle of 38% HCl. That is a pain to store. The bottle is somewhat pressurized, like a bottle of carbonated soft drink. If I open the screw cap, then I hear a hissing noise like you hear on opening a fresh bottle of coca cola. The pressurized HCl then comes out of the bottle giving a thick white choking fume.

 

For my normal experiments I use 30% HCl though. That also gives fumes, but at least it is not under pressure. It is sold in 5 liter jerrycans. We also have 10% HCl over here in hardware stores, that stuff is of high quality but relatively expensive. No colored impurities at all and on evaporation hardly any residue is left.

[YT2095]

J. I got it from Hughes & Holmes Limited, it`s called Mortex brick masonary & Patio Cleaner.

 

Woelen, this stuff is clear as water, I suspected it had detergent in it, because when you shake the bottle, it forms bubbles that take a while to go away, so it`s a physical apearance more than anything, I didn`t think HCl would be Frothy when shaken. eitherway I`m more than pleased with it.

as for its unavailablity, I`ve no idea, yesterday was the 1`st time I`de ever set out deliberately to buy some.

I`ve a nice batch of tin chloride soln now, so all being well if I get time later today, I`ll power up and see if I can get some metal from it

[woelen]

I`ve a nice batch of tin chloride soln now, so all being well if I get time later today, I`ll power up and see if I can get some metal from it

You definitely should keep some of the tin chloride for other experiments. Tin (II) forms many interesting complexes and precipitates. The most interesing one I have made so far is the deep orange/red [Pt(SnCl3)5](3-). It is so remarkable because of the SnCl3(-) ligands and besides that, it also is penta-coordinated, which is really special. But also if you do not have platinum-salts, there are many interesting experiments with it. E.g. add a very concentrated drop of solution of KI to a very concentrated drop of solution of SnCl2 and see what happens. You get a yellow precipitate, which after some time turns bright orange/red and also becomes dry and crystalline!

 

Tin (II) in general is an interesting fairly strong reductor.

 

 

BTW: Many concentrated solutions may indeed have a look as if some detergent is in them. HCl also is one of them. My 30% HCl keeps bubbles on the surface of the liquid for a long time, when it is shaken.

[YT2095]

I`ll bear that in mind for later experimentation, thus far I`ve got some fantastic metal crystals growing!

I`ve taken pics, but have no way of uploading them yet until I get chance to goto the photo-shop, I will post them though

 

I`m using carbon electrodes at 5cms distance apart (inside measurement) 2.75 volts seems to be the least needed to grow the crystals at an observable rate, I`m using 3 volts at the moment, it`s a slow growth but the blade like crystals seem to have quite a bit of strength to them when lited from the electrolyte, I could get a faster rate going but I want a slower one to ensure greater crystal purity.

I`m putting them into fiterpaper to be washed in water later.

from there I can either use the tin directly, or make the chloride any old time I need some.

my imediate goal was to get this procedure perfected, and so far it`s considerable better than originaly anticipated, I`m well pleased with the results

an interesting observation about the crystals is that not only are they blade like, but they like to be Edge upwards, perpendicular to gravity, and they also tend towards the anode until they get too heavy and slowly "Flop over", but directly from the cathode carbon, they grow out as needles, only 2 or 3 will actualy develop into a "blade", and then from a blade more blades are "born", fascinating to watch!

 

as for the HCl, that sounds about right, as the label says: Contains<20% Hydrochloric Acid, so it it could be any conc between 20 and about 38%. I suspect it`s Not that high though as it doesn`t fume exactly, but it will frost glass if left in the open for a while.

[YT2095]

I`ll bear that in mind for later experimentation' date=' thus far I`ve got some fantastic metal crystals growing!

I`ve taken pics, but have no way of uploading them yet until I get chance to goto the photo-shop, I will post them though

[/quote']

and as promised (the wife went to photo-shop this morning it`s cheaper if you have over 50 pics on the card) albeit delayed, Here is the best pic of the 3 I took:

 

it is indeed a Very beautiful metal to watch "grow"

Edited April 1, 2009 by YT2095

[woelen]

YT, that looks really great. That is an experiment I'm certainly going to repeat! How big is that white tub in which you have the liquid? Is this still the 5 cm you mentioned in your previous post?

[YT2095]

the tub`s about 7cms (3 inch), the min distance between the carbon electrodes was roughly 5cms yeah. to give an idea of scale, the cathode(left) is the carbon rod from a AA batt and the anode (right) is from a D cell.

and it`s a 250ml erlinmyer in the back.

[jwms]

Tin is the main (80%) componet of pewter. (20%copper) You can also reduce the tin oxide that was formed by adding the appropriate (molar wieght) of carbon and passing an electric current through the mix. A welder works well for the current draw. Keep oxygen out to keep it from "burning" due to the high temperatures produced. It must breathe to some extent as carbon dioxide is produced and must escape.

[bob000555]

Perhaps try using the solder as electrodes in as pure H2O2 as you can get and you should get lead and tin oxide, if it doesn’t work add a few drops of nitric acid to lower the oxidation number. Next magnetically separate the two oxides and do a termite reaction on the tin oxide(the one that is attracted to the magnet the lead oxide will be left behind)

[YT2095]

when did tin oxide become magnetic?

[bob000555]

all tin is magnetic....lol i just thught of somthing, you can grind the solder to a powder then magneticly separate it.

[woelen]

I'm not sure whether tin is magnetic or not (but let's suppose that is true), but when a metal is magnetic, then surely its compounds (e.g. oxide) need not be magnetic. Being magnetic is a property of a compound, just like color is a property of a compound. When a new chemical compound is formed, then the properties become totally different.

 

There also is a second misconception in bob's post. An alloy cannot be separated by grinding. E.g. when I have an alloy of iron with another non-magnetic metal, then one cannot grind it so fine, that the non-magnetic metal and the iron can be separated by magnets. Even the tiniest particles still have the iron and the other metal intimitely mixed (at the atomic level). One would have to break down the metal to the atomic level, but that implies making a new compound.