Sciencemadness Discussion Board

Making iron sulfide

bluamine - 13-3-2017 at 11:52

Hi everyone!
I want to make iron sulfide, & I just would like to know what are the materials I can try the reaction on.. I have some plaster & red bricks, can I use them or I should buy some cement instead?
Another thing to say can I use an iron rod to heat the mixture? Instead of a glass rod (like the one in Nile red's video)

Elemental Phosphorus - 13-3-2017 at 12:30

On top of a red brick should be fine if you are using Nile Red's procedure for FeS. An iron rod can be used to initiate the reaction.

bluamine - 13-3-2017 at 12:49

I was looking online to know the heat resistance of red clay but unfortunately didn't find anything interesting
I guess the iron rod will not react because it's a relatively big piece

Sulaiman - 13-3-2017 at 12:55

I did this recently http://www.sciencemadness.org/talk/viewthread.php?tid=64759&...

Elemental Phosphorus - 13-3-2017 at 13:03

The iron rod will not react because its surface area is nothing compared to homogeneous powders. Red clay can resist a good amount of heat. I used standard bricks to cover a furnace lid where they were exposed to very high heat. Note that a brick cannot continuously take orange-yellow heat but for an application like this it will be fine. Firebrick is for the continuous-heat applications, but brick is reasonably heat resistant as well.

Edit: Just read Sulamain's post and a metal container, like he and Nile Red used works as well (not aluminum, magnesium, zinc, lead etc. !)

[Edited on 13-3-2017 by Elemental Phosphorus]

bluamine - 13-3-2017 at 13:06

Quote: Originally posted by Sulaiman  
I did this recently http://www.sciencemadness.org/talk/viewthread.php?tid=64759&...

You did it in a tin can! Are you sure it's not made of steel?

[Edited on 13-3-2017 by bluamine]

Elemental Phosphorus - 13-3-2017 at 13:08

Tin cans are nowadays made of steel.

Sulaiman - 13-3-2017 at 13:30

A steel can that previously had baked beans in it.

place the can on soil, ignite the mixture (I used a cigarette lighter/mini-torch)

I did it in the late evening to see the orange glow,
and hopefuly the neighbours windows were all closed (its winter)

Next time I will try a 3:2 weight ratio for Fe:S

bluamine - 14-3-2017 at 06:11

Quote: Originally posted by Elemental Phosphorus  
Tin cans are nowadays made of steel.

I think in my country, I think cans are probably still made of tin, I'm not sure though, tin is expensive like everywhere else in this world xd but I can't imagine a steel can being that easy to crash with a small hammer..
Quote: Originally posted by Sulaiman  
I did this recently http://www.sciencemadness.org/talk/viewthread.php?tid=64759&...

Based on what you reported, I must use about 10% excess of sulfur to have a better yeald?
Molten sulfur is supposed to reactwith oxygen in the air

[Edited on 14-3-2017 by bluamine]

bluamine - 14-3-2017 at 08:43

As well I would like to know how can I grind the product (or at least crash into small pieces)? I thought about doing it under water!

[Edited on 15-3-2017 by bluamine]

Sulaiman - 14-3-2017 at 11:02

I just ground mine with mortar and pestle
I guess that you are concerned about the reported pyrophoric nature of FeS
so far I have had no problem
also
no need to grind to a fine powder,
HCl attacks whole lumps
and finely powdered FeS gets up my nose.

Sulaiman - 14-3-2017 at 11:06

As far as I know, pure tin has never beed used for 'tin cans' https://en.wikipedia.org/wiki/Tin_can
they were steel, plated with tin for corrosion protection.
Modern 'tin cans' often have a thin plastic coating inside for the same reason.

P.S. sulfur vapourises and burns, I do not know what the 'best' ratio of iron to sulfur is,
it will depend upon how much sulfur is 'lost' in your setup.

I pushed the lid down to leave only a small gap for gases/fumes to escape,
I do not know if it helps or not.


TinCan.jpg - 22kB

[Edited on 14-3-2017 by Sulaiman]

bluamine - 14-3-2017 at 19:49

Quote: Originally posted by Sulaiman  
I just ground mine with mortar and pestle
I guess that you are concerned about the reported pyrophoric nature of FeS
so far I have had no problem
also
no need to grind to a fine powder,
HCl attacks whole lumps
and finely powdered FeS gets up my nose.

It's not that pyrophoric we should fear, I already crashed some of it without any problem, as well it doesn't burn during the reaction
Man, I breathed a lot of sulfur dioxide after one night of breathing a bit of chlorine, I'm impressed I'm still alive xd
Quote: Originally posted by Sulaiman  
As far as I know, pure tin has never beed used for 'tin cans' https://en.wikipedia.org/wiki/Tin_can
they were steel, plated with tin for corrosion protection.
Modern 'tin cans' often have a thin plastic coating inside for the same reason.

P.S. sulfur vapourises and burns, I do not know what the 'best' ratio of iron to sulfur is,
it will depend upon how much sulfur is 'lost' in your setup.

I pushed the lid down to leave only a small gap for gases/fumes to escape,
I do not know if it helps or not.




[Edited on 14-3-2017 by Sulaiman]

Thank you so much for the informations about tin cans
I will report my experience in this topic:
I used 258.5 g of iron fine powder (all the quantity I had) & 178,5 g of sulfur (with a large excess of more than 20%). I had two rods & I used both of them but they didn't work well. So I decided to use 4 different steel spoons, & it worked well after several tries. In the end I obtained 361 g of product with some impurities of of red clay, some organic residue, but mainly unreacted materials (I suppose at least about 90-95% of materials reacted successfully because the majority of the mix stayed red hot for probably about 30 min or more I'm not sure about time, in addition I didn't see many chunks of reactants since the mix's color is obviously gray!) So I think about 77 g of sulfur was burnt in the air.
For my purpose I need 2,5 mol (3,5 if I want an excess) so I think I obtained what I want, but I think I will retry it using 1,5 mol of iron..
Note: I lost some product as dust & small chunks when I cleaned my tools, also I still have some other chunks on the red brick I used!
By the way, I see the product is slightly soluble in water! I supposed it is insoluble before

Sulaiman - 15-3-2017 at 01:29

once your FeS is crushed/powdered, a lot of the un-reacted iron can be removed with a magnet :)

You used 258.5/55.845 = 4.63 moles of Fe, and 178.5/32.06 = 5.57 moles of S
so you should easily have more than your required 3.5 moles of FeS

Side note: you will end up with moles of Fe(II)Cl2 which may be worth keeping ?
(assuming that you use HCl to produce H2S from your FeS)

Your FeS has the potential to produce 100 litres of H2S gas ...
From Wikipedia;
0.00047 ppm or 0.47 ppb is the odor threshold, the point at which 50% of a human panel can detect the presence of an odor without being able to identify it.[33]
10 ppm is the OSHA permissible exposure limit (PEL) (8 hour time-weighted average).[16]
10–20 ppm is the borderline concentration for eye irritation.
20 ppm is the acceptable ceiling concentration established by OSHA.[16]
50 ppm is the acceptable maximum peak above the ceiling concentration for an 8-hour shift, with a maximum duration of 10 minutes.[16]
50–100 ppm leads to eye damage.
At 100–150 ppm the olfactory nerve is paralyzed after a few inhalations, and the sense of smell disappears, often together with awareness of danger.[34][35]
320–530 ppm leads to pulmonary edema with the possibility of death.[25]
530–1000 ppm causes strong stimulation of the central nervous system and rapid breathing, leading to loss of breathing.
800 ppm is the lethal concentration for 50% of humans for 5 minutes' exposure (LC50).
Concentrations over 1000 ppm cause immediate collapse with loss of breathing, even after inhalation of a single breath.

at this scale (4.5 mol) death from ONE lungfull = 1000 ppm equivalent to 100,000 litres = 4m x 5m x 5m = greater than the volume of a typical amateur lab :o
OR
100 litres H2S @ 0.47 ppb = able to stink up an entire football stadium :P

I just felt that I had to mention this in case less experienced readers have a go.







[Edited on 15-3-2017 by Sulaiman]

bluamine - 15-3-2017 at 09:45

Quote: Originally posted by Sulaiman  
once your FeS is crushed/powdered, a lot of the un-reacted iron can be removed with a magnet :)

You used 258.5/55.845 = 4.63 moles of Fe, and 178.5/32.06 = 5.57 moles of S
so you should easily have more than your required 3.5 moles of FeS

Side note: you will end up with moles of Fe(II)Cl2 which may be worth keeping ?
(assuming that you use HCl to produce H2S from your FeS)

Your FeS has the potential to produce 100 litres of H2S gas ...
From Wikipedia;
0.00047 ppm or 0.47 ppb is the odor threshold, the point at which 50% of a human panel can detect the presence of an odor without being able to identify it.[33]
10 ppm is the OSHA permissible exposure limit (PEL) (8 hour time-weighted average).[16]
10–20 ppm is the borderline concentration for eye irritation.
20 ppm is the acceptable ceiling concentration established by OSHA.[16]
50 ppm is the acceptable maximum peak above the ceiling concentration for an 8-hour shift, with a maximum duration of 10 minutes.[16]
50–100 ppm leads to eye damage.
At 100–150 ppm the olfactory nerve is paralyzed after a few inhalations, and the sense of smell disappears, often together with awareness of danger.[34][35]
320–530 ppm leads to pulmonary edema with the possibility of death.[25]
530–1000 ppm causes strong stimulation of the central nervous system and rapid breathing, leading to loss of breathing.
800 ppm is the lethal concentration for 50% of humans for 5 minutes' exposure (LC50).
Concentrations over 1000 ppm cause immediate collapse with loss of breathing, even after inhalation of a single breath.

at this scale (4.5 mol) death from ONE lungfull = 1000 ppm equivalent to 100,000 litres = 4m x 5m x 5m = greater than the volume of a typical amateur lab :o
OR
100 litres H2S @ 0.47 ppb = able to stink up an entire football stadium :P

I just felt that I had to mention this in case less experienced readers have a go.







[Edited on 15-3-2017 by Sulaiman]

Thank you for the good idea to separate iron from the product
I still have about 23 g of sulfur so may be I'll react them together for the second time.
As well I will crash the chunks on my red brick.
The density of H2S & is about 1.36g/l according to Wikipedia. But I think it will be bigger because it's cold now (15-19 in average)

[Edited on 15-3-2017 by bluamine]

Aqua-regia - 16-3-2017 at 06:19

The question is what is your goal with FeS. You want producing H2S gas? In this case one of the worst solution homemade FeS. The reaction with Fe + S is never completly. I woult say the really yield were max 60-70%. If you destroying this with HCl you get a lot H2 too. Try to do the reaction instead Fe with Al dust .This is very succesful and easier. The product is almost pure Al2S3.
If in your country avaiable lithopone pigment , choosing this. This is OTC and cheap. (containt: ZnS+BaSO4)

AJKOER - 18-3-2017 at 17:30

If the goal is indeed H2S, the most direct path, per one source, does work (see http://www.encyclopedia.com/science-and-technology/chemistry... ):

"It may be made by reacting hydrogen gas with molten sulfur or with sulfur vapors"

In other words, burning sulfur continues to react in an atmosphere of hydrogen forming H2S. Similarly, a H2 generator (Al/NaOH or Zn/HCl) with an expelling tube of hydrogen gas placed in molten sulfur makes H2S. These, by nature, may be a small scale path, but in the case of highly toxic and obnoxious H2S, this could be a good thing!

Note, depending on the relative H2/S ratio, one may get a mix of gases containing, for example, H2, H2S and H2S2.

I do recommend avoiding this gas as it toxicity is generally underestimated (around 4 times the dosage of HCN with respect to the 1st observed lethal effect for 30 minutes of exposure, see https://www.doctorfire.com/toxicity.html ) being absorbed both by skin exposure and inhalation. The rapid deadening of the sense of smell can lead to fatal doses even the person exposed is unaware of his eventual fate (literally a walking dead)!

[Edited on 19-3-2017 by AJKOER]

Sulaiman - 18-3-2017 at 23:30

I see the great danger of H2S in the petrochemical industry where huge volumes are handled,
in the home lab H2S MUST be made in small quantities or at a low flow-rate,
and a scrubber used ... unless you have no nearby neighbours :P

So I doubt that any of us (behaving sensibly) will get to the stage where we poison ourselves
... other than unfortunate and/or stupid accidents.

How many cases of H2S induced death have been reported in small scale labs ?

JJay - 18-3-2017 at 23:59

I remember reading about how to make H2S in World Book Encyclopedia supplement as a child.. they said to mix steel scrubbing pads with sulfur and heat it in an oven and then drop hydrochloric acid on it... they had some kind of experimental procedure that was considered suitable for children....

Sulaiman - 19-3-2017 at 00:38

During my childhood, one our neighbours was mean, always moaning, never returning balls, toys etc. that ended up in their garden,
one day during my early teens, my parents were out, and my neighbours were relaxing in their garden on loungers, with tea and cakes, and all their windows open for ventilation,
a lovely summer's day with a gentle breeze blowing from our side to theirs ......

A quick trip to my 'lab' and within minutes a 250 ml beaker of FeS and HCl was bubbling away in my garden ....
I wish I could fully describe the commotion next door :D

One of my favourite childhood memories.

So
under conditions that we are likely to create, the stink will get you well before danger levels.
If you do not hear from me again then I may be incorrect :(

bluamine - 19-3-2017 at 08:41

Quote: Originally posted by Aqua-regia  
The question is what is your goal with FeS. You want producing H2S gas? In this case one of the worst solution homemade FeS. The reaction with Fe + S is never completly. I woult say the really yield were max 60-70%. If you destroying this with HCl you get a lot H2 too. Try to do the reaction instead Fe with Al dust .This is very succesful and easier. The product is almost pure Al2S3.
If in your country avaiable lithopone pigment , choosing this. This is OTC and cheap. (containt: ZnS+BaSO4)


You are right. It was so boring to use my magnet to separate iron, so I stopped when I had about 91 g (I'm not sure but I guess it contains some iron sulfide..)
The best thing about it is that it contains probably most of iron small pieces contained in iron dust (about 11 g)
I think I had to use calcium/sodium sulfide instead. When it comes to aluminum dust I had to wait until next weekend to obtain it so I bought 350 g of sulfur & I will make iron sulfide again

[Edited on 19-3-2017 by bluamine]

AJKOER - 20-3-2017 at 09:31

This may be interesting experiment with those with some sulfur and just regular aluminum foil on hand.

Start by making a perturbed flame by simply jarring the lid on a gas stove, creating a noisy flame. Apparently the perturbed flame is also hotter and more easily can bring aluminum foil to a glowing red, creating a weakened gamma aluminum oxide coating on the underlying aluminum metal. Crumpled up the heated aluminum foil (wearing gloves) to form a weakened aluminum oxide coated aluminum powder. Mixed the latter with sulfur and heat/ignite to create aluminum sulfide.

I would expect a reaction less exothermic (and possibly less dangerous) than the usual fine powder Al and sulfur thermite.

Al2S3 will react with water vapor, water (or a weak acid) to produce H2S gas and Al(OH)3.

bluamine - 22-3-2017 at 14:57

Quote: Originally posted by bluamine  

You are right. It was so boring to use my magnet to separate iron, so I stopped when I had about 91 g (I'm not sure but I guess it contains some iron sulfide..)
The best thing about it is that it contains probably most of iron small pieces contained in iron dust (about 11 g)
I think I had to use calcium/sodium sulfide instead. When it comes to aluminum dust I had to wait until next weekend to obtain it so I bought 350 g of sulfur & I will make iron sulfide again

[Edited on 19-3-2017 by bluamine]

By thé way calcium sulfate reduction with carbon (Muller Kuhne process) requires high temperatures (>1000 °C)..
I tried with iron but I guess it won't work very well especially because I found relatively big amounts of both unreacted sulfur & iron.. So I will make some aluminum sulfide
Actually I did it using small pieces of aluminum foil but it doesn't seem to work well, i repeated it several times & have better results in some of them though
Anyway I noticed that the product doesn't react! With water (at least the reaction should be very slow, which makes it hard to see when using small amounts) what do you think about it guys?

[Edited on 22-3-2017 by bluamine]

ferrousexplosive - 12-7-2017 at 18:56

I know this is little off topic, but always i make this reaction it is considerably slow, thought beautiful, can one somehow manage to turn it into a flash powder similar to the mixture of zinc powder and sulphur?

And how you obtain your iron powder? I normally use a automatic sanding machine to get the powder from a solid bulk of iron. I have wondered if one can reduce an iron hidroxyde to a fine iron powder, but i have never found anything on it :(

I ask this because zinc powder is considerably laborious to me to obtain, since I don´t have how to obtain turnings of zinc to ballmill them, i have to convert zinc metal to the white oxide by electrolysis, then the oxide is 'disolved' in water with the help of sodium hydroxide and electrolyse that to have zinc sponge or crumbly powder to finally ballmill it to obtain a enough
fine powder.