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Ideas for iron powder

Sulaiman - 24-8-2020 at 05:00

To make some FeS for H2S generation I bought 500g of 300mesh iron powder,
the smallest economical quantity I could conveniently buy.

Shopee_cfe272be8b96e52e106add54bdd74e9f.jpg - 184kB

I will not be using all of the iron powder for this experiment so

Can anyone suggest an interesting experiment with iron powder?

macckone - 24-8-2020 at 07:29

Make pyrophoric iron from the oxylate.

Maurice VD 37 - 24-8-2020 at 08:53

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.

morganbw - 24-8-2020 at 12:42

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.

clearly_not_atara - 24-8-2020 at 13:34

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.

karlos³ - 24-8-2020 at 14:00

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?

Corrosive Joeseph - 24-8-2020 at 14:55

Quote: Originally posted by karlos³

I've actually seen such a paper!

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

Corrosive Joeseph - 24-8-2020 at 15:04

Encyclopedia of Reagents for Organic Synthesis - Zinc and Acetic acid - https://doi.org/10.1002/047084289X.rz002
https://scihub.to/10.1002/047084289X.rz002

Quote:

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

/CJ

macckone - 24-8-2020 at 15:22

Iron is supposed to be able to reduce chloroform to DCM without further reduction, you could give that a try.

Corrosive Joeseph - 24-8-2020 at 15:28

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.

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]

Corrosive Joeseph - 24-8-2020 at 15:55

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

Corrosive Joeseph - 24-8-2020 at 20:13

/CJ

Attachment: EROS - Iron.pdf (53kB)
This file has been downloaded 344 times

Sulaiman - 25-8-2020 at 02:07

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

wg48temp9 - 25-8-2020 at 03:54

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.

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.

Sulaiman - 1-9-2020 at 10:07

Quote: Originally posted by wg48temp9

Some like the pic below.

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

clearly_not_atara - 1-9-2020 at 10:09

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?

monolithic - 1-9-2020 at 12:31

Quote: Originally posted by clearly_not_atara

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?

https://sci-hub.tw/10.1021/es00061a012

http://www.sciencemadness.org/talk/viewthread.php?tid=78041&...

AJKOER - 10-9-2020 at 03:31

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]

Frankenshtein - 20-9-2020 at 14:08

Quote: Originally posted by monolithic

Quote: Originally posted by clearly_not_atara

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?

https://sci-hub.tw/10.1021/es00061a012

http://www.sciencemadness.org/talk/viewthread.php?tid=78041&...

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.

Dr.Bob - 22-9-2020 at 17:03

If you mix it with oxidants, you can make gold colored fireworks... Good for waterfalls, willows, and gold brocades.

A great use of chemicals.

Sulaiman - 29-9-2020 at 00:55

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]

TriiodideFrog - 29-9-2020 at 03:56

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.

Sulaiman - 29-9-2020 at 05:09

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]

TriiodideFrog - 2-10-2020 at 01:34

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.

Corrosive Joeseph - 2-10-2020 at 06:46

The Bechamp is a classic with some interesting historical significance.
https://en.wikipedia.org/wiki/Bechamp_reduction

/CJ

Herr Haber - 2-10-2020 at 07:14

If you decide on making some iron cement (which contains S and Fe) dont be a lazy ass and go get water. Do not use the vinegar in front of you even if it contains mostly water !

Sorry Sulaiman, that was meant for the idiot me from 30 years ago who knew about FeS but didnt think a lot about what he was doing

Sulaiman - 2-10-2020 at 21:40

Quote: Originally posted by TriiodideFrog

If you are looking for a experiment with iron powder, making iron sulfide is not a bad idea...

my plan is to investigate the stoichiometry a little as I read that FeS is commonly slightly stoichiometrically deficient in Fe,
so first I'll try a stoichiometric mix of Fe and S, (at about one molar scale) and measure weight loss,
then try to quantify the amount of H₂S produced with HCl and a small sample
by precipitating a metal sulphide and weighing it,
then try again with excess sulphur.
_______________________________
The bulk of the FeS produced will be stored for later production of H₂S
_______________________________
Because I'm not at home with all my chem. stuff but staying at my sister-in-law's house,
I have to plan H₂S and SO₂ safety even more carefully than normally.
(I'm not ready yet)
======================================
@Herr Haber :
All warnings gratefully received, especially anecdotes that make me feel I'm not alone

I'm still at the stage where a little knowledge may be dangerous ... never too old to do dumb stuff

[Edited on 3-10-2020 by Sulaiman]

TriiodideFrog - 2-10-2020 at 23:25

Glad my suggestion could help.

TriiodideFrog - 2-10-2020 at 23:39

If you are interested, you can try making iron chloride. Ferrous chloride is prepared by addition of iron powder to a solution of hydrochloric acid in methanol. This reaction gives the methanol solvate of the dichloride, which upon heating in a vacuum at about 160 °C converts to anhydrous FeCl2. The net reaction is shown: Fe + 2 HCl → FeCl2 + H.

Cou - 2-10-2020 at 23:39

Making iron pentacarbonyl by streaming carbon monoxide gas over iron powder.
https://en.wikipedia.org/wiki/Iron_pentacarbonyl
You can generate carbon monoxide from decomposition of formic acid.

I'm not sure about safety. I don't have a fume hood, but I would hope it's safe to do outside with ventilation.

Using the search function, you can find directions to sources with more detail on this interesting coordination compound.

[Edited on 10-3-2020 by Cou]

TriiodideFrog - 3-10-2020 at 00:01

Yes, if you need iron pentacarbonyl. However, be careful with formic acid. Its fumes often give me a headache.

Tsjerk - 3-10-2020 at 04:05

When making iron pentacarbonyl a formic acid headache should be one of your lesser worries.