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Sulaiman
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[*] posted on 24-8-2020 at 05:00
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.

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?




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macckone
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[*] posted on 24-8-2020 at 07:29


Make pyrophoric iron from the oxylate.
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Maurice VD 37
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[*] posted on 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.
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morganbw
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[*] posted on 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.
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clearly_not_atara
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[*] posted on 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.




[Edited on 04-20-1969 by clearly_not_atara]
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karlos³
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[*] posted on 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?
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Corrosive Joeseph
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[*] posted on 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




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Corrosive Joeseph
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[*] posted on 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




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macckone
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[*] posted on 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.
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Corrosive Joeseph
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[*] posted on 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]




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[*] posted on 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




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Corrosive Joeseph
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[*] posted on 24-8-2020 at 20:13


/CJ

Attachment: EROS - Iron.pdf (53kB)
This file has been downloaded 46 times





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Sulaiman
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[*] posted on 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




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[*] posted on 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.

fiflines2.jpg - 59kB




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.
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Sulaiman
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[*] posted on 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 :(




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clearly_not_atara
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[*] posted on 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?




[Edited on 04-20-1969 by clearly_not_atara]
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[*] posted on 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&...
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[*] posted on 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]
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[*] posted on 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.
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[*] posted on 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.
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Sulaiman
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[*] posted on 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+

Iron_II_III_VI.jpg - 327kB

Now considering disposal :P

[Edited on 29-9-2020 by Sulaiman]




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[*] posted on 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.:)
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Sulaiman
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[*] posted on 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]




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[*] posted on 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.
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Corrosive Joeseph
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[*] posted on 2-10-2020 at 06:46


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



/CJ




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