DirtyDan
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Iron Oxide
Haha, im just now having my first expirements with electralysis, and with some weird results. Im attempting to obtain some FeO, by rusting a nail in
electrilized water. I added salt to increase conductuctivity, and am using a carbon rod as a cathode, Iron ( i think lol) nail as an anode. With a
handy 10.5V 12A powersupply, i recieved nice bubbles forming right away. Then, the color slowly started to change, and to green  Some orange-colored film also floated up to the top. I stopped after about 10 minutes
and am filtering the solution now. Is my nail some weird Iron-Alloy? Where is the green coming from? Does it have anything to do with the carbon, or
the added salt? Thanks, i appreciate the comments and any help
Just checked on it again, and the color seems to change to orange after drying. What the hell is going on?
[Edited on 16-4-2004 by DirtyDan]
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darkflame89
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the green coloration is due to formation of Fe2+ ions. Since you did it only for 10 min, it did not have much time to oxidise to what you want. by the
way, it is Fe2O3 NOT FeO
Ignis ubique latet, naturam amplectitur omnem.
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4s2
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you are making Fe2+ ions and Fe3+. If I remember right you need like 4.4 v for the formation of Fe2+, and 7 somehting volts for the Fe3+. While your
voltage excedes the requirement, your iron goes through a change as it is given the charge. If you let it run long enough you can get a fair amount of
both.
The blackish colored stuff that settles to the bottom is your Fe2+ I beleive, and your orange/rusty colored film on the top is the Fe3+. Anyone have
thoughts on that? Its been awhile since I had done that... I will grab some stuff and go try it now.
I haven\'t failed, I\'ve found 683 ways that don\'t work. -- Me.
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4s2
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Ok, so I just tried to replicate this (been going for 12 min now). I did this once before but never really understood all that was going on, maybe
someone can help us both.
I prepared the bath with Distilled water, and pure NaCl crystals. I dont have a pencil or any graphite laying around, so I used 2 nails for the anode
and cathode.
After about 12 min I see a greenish/skin like translucent gunk forming on the negative electrode. Correct me if I am wrong but I assume as the NaCl
dissolves, the ions move to their corisponding electrode (Na+ to the negative, and Cl- to the postative), in doing so, the charge is lost/gained and
it is no longer an ion. the element moves back into the solution where it becomes an ion once more, so in theory, the electrolytes should not be
collecting on the electrodes (not that Na forms green skin anyway). So what is this greenish gunk?
On the bottom there seems to be some sort of a black precipitate the Fe(II) I assume, and the top has the rusty colored film (the Fe(III)2O3 ?
If I was to seperate the two (iron nail) electrodes with a bridge of some sort(in two seperate baths), what would be the result in each bath?
How could just Fe(III)2O3 be produced then?
[Edited on 16-4-2004 by 4s2]
I haven\'t failed, I\'ve found 683 ways that don\'t work. -- Me.
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t_Pyro
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The "green gunk" would be ferrous chloride. If a substance formed during electrolysis is insoluble, it cannot enter back into the solution,
as in the case of ferrous/ic hydroxide. If you want pure FeO, you'll have to be careful that it does not get oxidised to
Fe<sub>2</sub>O,sub>3</sub>. Even exposure to air for a long time can do so.
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4s2
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| Quote: | Originally posted by t_Pyro
If you want pure FeO, you'll have to be careful that it does not get oxidised to Fe<sub>2</sub>O,sub>3</sub>. Even exposure
to air for a long time can do so. |
erm...
I haven\'t failed, I\'ve found 683 ways that don\'t work. -- Me.
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DirtyDan
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Ok, so the greenish stuff is and Fe + Cl compound?? I dried it all now, and am left with a mix of brown-orange chunks and black discoloration (maybe
its dark green). Would this be suitable for a thermite reaction, or do i have alot of contamanints? Im just getting started with different things and
trying my electralysis system out, not really expecting anything from my products yet, but if i can get a fair amount of Fe2O3 (not FeO, sorry about
that ) then i wont complain 
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hodges
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If you heat the insoluable precipitate strongly (say to 200 C) for an hour or so you will create iron oxide. Whether it is iron (2) or iron(3) oxide
will depend on whether you had iron(2) or iron (3) hydroxide in the precipitate to start with. But either one should work with finely powdered
aluminum to make thermite. You should wash your precipitate to get rid of impurities for best results.
A faster way to make iron oxide for thermite is to dissolve the nails in some acid, then add a base such as sodium hydroxide to precipitate iron
hydroxide. This precipitate can then be washed several times and heated to make iron oxide suitable for thermite. I have used this method before and
it works.
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DirtyDan
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In a curious attempt to drive off the water in my remaining filtered precipitate, i microwaved  it for a few minutes. The paper towel dried, and the iron hydroxide turned black. Before, in my first attempt, the
precipitate dried brown like i said. Did something decompose with the rays? Also, does the size of the aluminum particles matter as much in thermite
as it does in say, flash powder? I have made some using the method off of roguesci (blender w/ salt) and have not followed up with a ball milling or
anything, so it is not finely ground. Not hard to do, just wondering. Oh, and thanks for the help
OK, i looked this up Here: | Quote: | There are a number of iron oxides:
Iron (II) oxide (FeO) The powder in particular can cause explosions as it readily ignites. Colour black.
Iron (III) oxide, (Fe2O3) known in its natural state as Haematite, but also purified for use as a coating in magnetic audio and computer media, where
it is known as Ferric oxide.
Iron (II, III) oxide (Fe3O4), better known as the mineral Magnetite or lodestone. Colour black.
Iron Hydroxides
Iron hydroxide FeO(OH), found as the minerals Siderogel and Feroxyhyte. It also has a variant known as Lepidocrocite.
Iron (II) hydroxide Fe(OH)2. green colour.
Iron (III) hydroxide Fe3+O(OH) found as the mineral goethite. Red-brown colour.
Iron (III) hydroxide Fe(OH)3. Dark brown.
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After drying under a lamp and in the microwave, im left with a final black powder. Is this Fe3O4 or FeO? Or a hydroxide yet? Im not very sure of
anything at this point. I also noticed that my black powder is magnetic, are all forms or are the hydroxides not? Just a thought
[Edited on 18-4-2004 by DirtyDan]
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hodges
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Its hard to say what oxide you got because the hydroxide can react with oxygen in the air. For thermite it really doesn't matter much, and there
is not that much difference between the masses of the different iron oxides needed.
How do you plan to ignite your thermite? Even relatively large aluminum particles will work, but the finer the aluminum the easier it is to ignite.
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DirtyDan
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I just tried to ignite my 10g batch, no luck though. I used flash powder from firecrackers (lol) and either it burned to quickly to effectively heat
my thermite, or the Al chunks are too large. How would a KNO3 + Sucrose mix do to ignite it? I can make that easy enough, and from igniting it before
it seemed to burn very hot.
Also, i poured out the flash next to the thermite in a clump, so that if it didnt ignite i wouldnt end up with weird byproducts in my thermite. Would
intimately mixing flash with thermite be a better idea? My rust is fairly fine, and since there is some Al in the flash comp, i figure that could be a
good way to get it going easily
[Edited on 18-4-2004 by DirtyDan]
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The_Davster
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Flash powder does not create enough heat to ignite thermite. Try using a mix of 1:3 coal powder to KNO3(stumbled upon this mix myself) this burns
very hot, but I have never tried ingiting thermite with it, it may work though-ignite the coal/nitrate mix with a sparkler. I doubt that KNO3/sucrose
produces enough heat to ingnite the thermite.
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DirtyDan
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Thanks, ill have to try that. Ill need to go buy some KNO3, i just ran out.. 
Right now my only source is Grants Stump Remover since i couldnt find any fertilizers readily (didnt look too hard though) If i had a sparkler, i
would have tried that already, since it contains come magnesium. My friend has some left over, ill try to get a couple from him. Or when i go to
chemistry tomorrow, maybe i can grap some Mg ribbon thats been laying around. Will try then i guess, im out for now
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chemoleo
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Alternatively, you could just use your Al powder and mix it with a stoichiometric amount of oxidiser (KNO3, NaClO3 etc) and use that to ignite
thermite.
Tried that once with SiO2/Al thermite, works without a problem.
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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Darkblade48
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Something odd about Iron Oxide
I was making some iron oxide the other day using the electrochemistry method, and got some Iron oxide. Today, I also did it but I used the HCl + NaOH
method.
Now the odd thing I noticed was that when I produced the rust electrochemically, I got a magnetic powder, whereas when I did it chemically, I get a
non (ferro?)magnetic product.
I recall searching and found a post from (quite) awhile back saying that rust that was made electrochemically would have magnetic properties, but can
anyone explain why this might be so? I was always under the impression that rust was Fe2O3 and was non-magnetic.
Slightly related, but would the magnetic properties affect a thermite reaction?
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cyclonite4
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From what you say, I believe that rather than forming pure Fe2O3 from the electrochemical method, you have formed a mixture of FeO and Fe2O3.
Magnetic Iron Oxide is magnetite or 'Fe3O4', a mixture between Iron(II and Iron(III) Oxides (one mole of Fe2O3 per mole of FeO, therefore
the new empirical formula is Fe3O4).
The magnetic properties wont affect the reaction, but the fact the emprirical formula is different does, so you need to adjust your stoichiometry to
compensate.
\"It is dangerous to be right, when your government is wrong.\" - Voltaire
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Darkblade48
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Interestingly enough, before I heated up my Iron oxide that I made from the HCl and NaOH method, it wasn't magnetic.
However, after heating in my oven at ~230 C for a couple hours, and taking the iron oxide out and grinding it into a fine powder, I discovered that it
was magnetic
I'm kinda shocked and at a loss for words here. How can previously non magnetic iron oxide suddenly become magnetic after heating in an oven?
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frogfot
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I think there is a simple explanation. Both methods (chem and el chem) gives same product which is hydrated Fe(II). It can be readily oxidise to
Fe(III) by airs oxygen.
Fe(II) is not magnetic as opposed to Fe(III), because latter has a lone electron in it's d orbitals.
Generally dissolution of iron goes faster in acid than by electricity (if you weren't using huge currents). The majority of Fe(II) that was
formed by dissolution of iron in acid will not have time to be oxidised by air. Lumps of it wouldn't be able to oxidise at room temp since air
have only access to the surface of particles. So this gives non magnetic prod.
While iron dissolved electrochemically would majorly oxidise to Fe(III) during the electrolysis (air diffuses into the electrolyte freely). So
electrolysis will give magnetic product directly.
Once you heat your chemically oxidised product (hydrated iron) it will leave water and become porous.. so this will give free access to airs oxygen..
I'd guess... and thereby give magnetic Fe(III)..
[Edited on 16-4-2005 by frogfot]
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JohnWW
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About Fe(III) It has 5 unpaired 3d electrons in 5 orbitals, which is the maximum number for a d transition metal, unless it is complexed by ligands
sufficiently strongly bonding to cause spin-pairing in order for more electron-pairs from the ligand to bond to d orbitals on the Fe, reducing the
number of unpaired electrons (see L.E. Orgel's book on transition-metal chemistry). Fe(II) must have two of its 6 3d electrons spin-paiured in
one orbital, so reducing its maximum possible number of unpaired electrons to 4. So Fe(III) compounds are usually more paramagnetic than Fe(II) (and
Fe(I), (IV), (V) and (VI)) compounds.
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Nerro
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JohnWW I feel painfully stupid/uninformed after reading your post. I wish I were in university already. Ow well, just one summer between me and
enlightenment 
I have recently made ironoxide by reacting FeSO4 (in solution) with NaOH (also in solution). A green precipitate formed (Fe(OH)2 obviously.) which
turns orange (Fe2O3 I presume) if left in open air for long enough. When I dried the green precipitate I was left with a black powder which I presume
to be FeO. I have yet to discover any magnetic properties though...
Once all the green slurry has dried completely how should I proceed to turn it into Fe2O3? I think heating in the open air should do the trick. Do you
guys have any usefull suggestions on that?
[Edited on 4/5/2005 by Nerro]
#261501 +(11351)- [X]
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