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Sulaiman
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Ideas for iron powder
To make some FeS for H2S generation I bought 500g of 300mesh iron powder,
the smallest economical quantity I could conveniently buy.
I will not be using all of the iron powder for this experiment so
Can anyone suggest an interesting experiment with iron powder?
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macckone
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Make pyrophoric iron from the oxylate.
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Maurice VD 37
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If you put a horizontal paper sheet or board over a magnet, and if you drop some iron powder from above, it will fall down and make nice images on the
board. These images look like lines or flower petals, looking as if they were getting out of the magnetic poles. It is worth the trouble doing it.
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morganbw
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I really do not have a handle on the chemistry that you really enjoy but there are some metal dissolving reductions which could be really cool.
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clearly_not_atara
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The reduction of internal nitroalkenes to ketones with iron powder and hydrochloric acid is well-known. It's speculated that this reduction proceeds
via an oxime, but I have never seen a report where the oxime was isolated.
Usually strong acid is used, which would hydrolyse the oxime. I wonder if using more dilute acid or other ways of activating iron powder could give
some oximes. Successfully making an oxime this way would be an interesting novelty.
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karlos³
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Quote: Originally posted by clearly_not_atara  | The reduction of internal nitroalkenes to ketones with iron powder and hydrochloric acid is well-known. It's speculated that this reduction proceeds
via an oxime, but I have never seen a report where the oxime was isolated.
Usually strong acid is used, which would hydrolyse the oxime. I wonder if using more dilute acid or other ways of activating iron powder could give
some oximes. Successfully making an oxime this way would be an interesting novelty. |
I've actually seen such a paper!
Joe showed it to me who always had great interest in this reaction, for this purpose.
The yields weren't great, maybe 60%, and they've used no acid(or only a very small stoichiometric amount?) if my memory serves right.
The oxime was isolated though.
But I don't remember this paper, because my own interest in this reaction was always far from great... it was somewhat old, at most in the 19050's I
would say.
I have it somewhere among my files, but I would never find it... its been at least 2018 when I've seen this paper, and due to lack of interest I
haven't renamed it so that I could find it again easily.
Although it could be that I remember some details wrong and mix things up?
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Corrosive Joeseph
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I've actually seen three or four of them!
I'm not anywhere near my drives right now, but I was quite obsessed with a while. Let's see what I can recall from memory.
Here is the first one..
The paper -
https://www.erowid.org/archive//rhodium/pdf/nitro.alkene.der...
The patent -
https://chemistry.mdma.ch/hiveboard/palladium/pdf/US2233823....
/CJ
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Corrosive Joeseph
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Encyclopedia of Reagents for Organic Synthesis - Zinc and Acetic acid - https://doi.org/10.1002/047084289X.rz002
https://scihub.to/10.1002/047084289X.rz002
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α,β-Unsaturated nitro compounds can also be reduced.[Ref. 40]
Under mild conditions an oxime can be obtained (eq 13) [Ref. 40a]
[Ref. 40a - Baer, H. H.; Rank, W., Can. J. Chem. 1972, 50, 1292
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/CJ
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macckone
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Iron is supposed to be able to reduce chloroform to DCM without further reduction, you could give that a try.
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Corrosive Joeseph
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| Quote: |
Bouveault and Wahl have shown that nitroolefins of the structure R--C=C-N02 could be reduced to the aldoxime with zinc powder and acetic acid. Hass
and Susie have reported that subsequent workers have been unable to repeat the work of Bouveault and Wahl, but we have found that the reduction of
(secondary) nitroolefins of the structure R--C=C(NO2)-R’ to the ketoxime proceeded smoothly with a 50-60% yield in most cases.
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Nightingale, D., & Janes, J. R. (1944). The Preparation of Ketones from Nitroölefins.
Journal of the American Chemical Society, 66(3), 352–354.
doi:10.1021/ja01231a009
https://sci-hub.ee/10.1021/ja01231a009
/CJ
[EDIT] - Whoops, those two were with zinc and acetic acid but very similar dissolving metal reduction.
[Edited on 25-8-2020 by Corrosive Joeseph]
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Corrosive Joeseph
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More related papers...
Senkus, M. (1948). Iron Reduction of Some Aliphatic Nitro Compounds.
Industrial & Engineering Chemistry, 40(3), 506–508.
doi:10.1021/ie50459a035
https://sci-hub.se/10.1021/ie50459a035
Johnson, K., & Degering, E. F. (1939). The Utilization of Aliphatic Nitro Compounds. (I) The Production of Amines and (II) The Production of
Oximes.
Journal of the American Chemical Society, 61(11), 3194–3195.
doi:10.1021/ja01266a061
https://sci-hub.se/10.1021/ja01266a061
/CJ
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Corrosive Joeseph
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/CJ
Attachment: EROS - Iron.pdf (53kB)
This file has been downloaded 344 times
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Sulaiman
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Thanks for the ideas,
I'll give the pyrophoric iron a miss - for now,
no high temperature source available.
I was playing with magnets and wires and iron filings >50 Years ago 
I tried recently with NdFeB magnets... too strong.
The rest will need some more reading,
and a way to determine if reactions occur as expected, or not.
Great stuff.. thanks
................................
Regarding Fe + S - > FeS ;
Which is better, at 3 molar scale, igniting,
or heating until S melts then more until auto-ignition?
What is a good ratio for excess S?
I'm considering +10% to allow for vaporisation and burning
and FeS is, according to Wikipedia, slightly stoichiometrically lower in iron than 1:1
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wg48temp9
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| Quote: Originally posted by Maurice VD 37 | If you put a horizontal paper sheet or board over a magnet, and if you drop some iron powder from above, it will fall down and make nice images on the
board. These images look like lines or flower petals, looking as if they were getting out of the magnetic poles. It is worth the trouble doing it.
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Or perhaps for a more convenient method mix the iron powder with clear paraffin oil then put the oil between two glass or plastic sheets separated by
a few mm and sealed at the edges.
Some like the pic below.
I am wg48 but not on my usual pc hence the temp handle.
Thank goodness for Fleming and the fungi.
Old codger' lives matters, wear a mask and help save them.
Be aware of demagoguery, keep your frontal lobes fully engaged.
I don't know who invented mRNA vaccines but they should get a fancy medal and I hope they made a shed load of money from it.
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Sulaiman
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I watched that YT video some time ago, interesting but not worth the effort, for me.
....................
When I opened the jar of iron powder I found a lot of Fe2O3 so I'm returning it for a refund 
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clearly_not_atara
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| Quote: Originally posted by macckone | | Iron is supposed to be able to reduce chloroform to DCM without further reduction, you could give that a try. |
A massive upgrade of chloroform! Where'd you hear this?
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monolithic
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https://sci-hub.tw/10.1021/es00061a012
http://www.sciencemadness.org/talk/viewthread.php?tid=78041&...
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AJKOER
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You could try making FeO(OH) assuming you have an old fish air pump around. A thread (with pictures) available here https://www.sciencemadness.org/whisper/viewthread.php?tid=15... .
The compound may have also interesting photocatalytic abilities (not explored in the cited thread).
At least the review of the underlying chemistry is likely sufficient for those having trouble falling asleep to be an effective and safe sleep aid.
[Edited on 10-9-2020 by AJKOER]
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Frankenshtein
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Seems it takes a lot of time, pure nitrogen on hand, and would be low yielding. Maybe it could be sped up with heat. I saw another google result that
seemed to be speeding this up with a bacteria, a further implication that it's not viable as is. Seems there's easier ways already as with the Zn.
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Dr.Bob
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If you mix it with oxidants, you can make gold colored fireworks... Good for waterfalls, willows, and gold brocades.
A great use of chemicals.
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Sulaiman
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yup! I'll have a go at some pyrotechnics.(but don't tell anyone - illegal here)
_________________________________
My new order for iron powder arrived and inspired by the photos recently posted by EthidiumBromide I had a quick play;
2.8g of iron powder (c1/20 mole) dissolved in 10ml 34% HCl with c40ml water.
(I had to add a little extra 34% HCl to get all of the iron to dissolve)
Half of this Fe(II) solution is in the 25ml beaker marked B on the left.
the other half was put into the 25ml beaker marked A then oxidised to Fe(III) using c10ml 50% H2O2.
c1ml from 25ml beaker A added to water in 50ml beaker B
added c10g KOH to c75ml domestic bleach in 100ml beaker A, then added c10ml from 25ml beaker A.
c1.5ml from 100ml beaker A added to water in 50ml beaker A.
So, from left to right, very approximately,
1M Fe2+, 1M Fe3+, 0.02M Fe3+, 0.1M Fe6+, 0.003M Fe6+
Now considering disposal 
[Edited on 29-9-2020 by Sulaiman]
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TriiodideFrog
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You can carry out an electrolysis of FeCl2 solution by dissolving an iron nail in HCl (Fe+2HCl=FeCl2+H2). After that you would have to scrape the iron
of the electrodes and grind them into powder. This might be a rather messy and a not so economical method. Hope my suggestion can help you.
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Sulaiman
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Yes, electrolysis ... unlimited oxidising power. I may try soon.
The above was just a quick play, I would like to make some anhydrous Fe6+ sometime.
Aqueous Fe6+ synthesis is easy, but from reading other threads here on SM,
recovery and purification is non-trivial...later...maybe...
P.S. judging by colour, overnight most of the Fe6+ has converted to Fe3+.
[Edited on 30-9-2020 by Sulaiman]
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TriiodideFrog
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If you are looking for a experiment with iron powder, making iron sulfide is not a bad idea. You can just mix iron powder and sulfur powder in the
ratio 7:4. You need to make the powder relatively homogenous, so I suggest pouring the powder back and forth. Do not use mechanical stirring or
grinding with a mortar and pestle as it could lead to the mixture spontaneously combusting. The best and most impressive way is to heat up a glass rod
to a little over 100°C, which is the melting point of sulfur, and stick it into the mixture. This reaction should only be carried out on something
that can withstand high heat, so I would strongly advise against a watch glass or any porcelain. Just a warning, iron sulfide is pyrophoric so you
probably should not powderise it. You can reaction the iron sulfide with HCl to for Hydrogen Sulfide gas.
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Corrosive Joeseph
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The Bechamp is a classic with some interesting historical significance.
https://en.wikipedia.org/wiki/Bechamp_reduction
/CJ
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