Author Topic: How to make Ferric Ammonium Citrate? (Read 5343 times)

distimpson · **Reply #25 on:** 25/06/2012 23:58:08

maybe a contact print of Meteor Crater using a Canyon Diablo meteorite?

or a picture of El Chaco with a Campo? http://direcciondefauna.blogspot.com/2010/07/mas-de-500-turistas-visitaron-el.html

agreed, great project, lots of fun.

AllenG · **Reply #26 on:** 26/06/2012 00:10:10

Quote from: distimpson on 25/06/2012 23:58:08

maybe a contact print of Meteor Crater using a Canyon Diablo meteorite?

or a picture of El Chaco with a Campo? http://direcciondefauna.blogspot.com/2010/07/mas-de-500-turistas-visitaron-el.html

agreed, great project, lots of fun.

Don, you are going to make me start searching out grants talking like that.

AllenG · **Reply #27 on:** 26/06/2012 00:33:15

Quote from: AllenG on 25/06/2012 23:54:35

BC, there is a man in Michigan who makes meteorite Damascus steel straight razors (they are stunning by the way). He hand forges and hammers them. Would the scale produced in that blacksmithing process be Iron(II)?

If so, my first step may be to trade him my meteorite sample for some of his floor sweepings.

http://www.classicshaving.com/i/Z%20razors/TZnew13e.jpg
^^^
That's a pic of one of one of the meteorite razors, btw. Off topic, but I use a straight razor and really lust after that thing.

RD · **Reply #28 on:** 26/06/2012 03:03:27

Quote from: AllenG on 25/06/2012 23:54:35

there is a man in Michigan who makes meteorite Damascus steel straight razors

been done before ... http://www.britishmuseum.org/explore/highlights/highlight_objects/loan_in/l/lance_with_a_blade_made_from_m.aspx

Bored chemist · **Reply #29 on:** 26/06/2012 05:59:40

It's probably a mixture of Fe(III) and Fe(II) but a lot of oxides formed at high temperatures are rather slow to react with things.
Dilute acid will certainly oxidise the metal to Fe(II), and also dissolve it at the same time.
Do you have access to hydrogen peroxide?

AllenG · **Reply #30 on:** 26/06/2012 06:08:54

What percent? I can order it.

Bored chemist · **Reply #31 on:** 26/06/2012 18:14:22

Hang fire on ordering it. I might as well check if it works nicely first.
Mass of iron lump now 16.2 g

AllenG · **Reply #32 on:** 26/06/2012 20:26:46

Thank you.
The hydrogen peroxide I have is the stuff in the medicine cabinet one purchases from the pharmacy.

Bored chemist · **Reply #33 on:** 26/06/2012 20:47:46

That might do the job. As I say, I will think about it then play about (aka experiment). We need an oxidising agent to get the iron to the ferric state. H2O2 is clean- the other products are water and oxygen.
An alternative would be nitric acid but that's not easy to get over the counter and also it will give lots of nasty fumes.

I think we will need a fairly clean product to be sure that this will work.
I wonder if anyone reading this has any thoughts on this plan of mine
.
Dissolve the meteorite in dilute sulphuric acid.
Add hydrogen peroxide to convert the iron to Fe(III)
Add ammonium sulphate then excess ammonia to produce Fe(OH)3
The sulphate should keep the mixture acidic enough to avoid precipitating magnesium and a few others. The ammonia will keep the nickel cobalt and copper in solution.

That should give fairly clean Fe(OH)3
Add water + pour it off or filter it off a few times to wash the Fe(OH)3
Add a known quantity of H2SO4 to dissolve most of the Fe(OH)3 and filter it ( that gives a known quantity of iron in solution and also leaves Mn2O3 behind).

From there it's essentially a matter of following the old recipe from the book.

Can anyone see if I done anything dumb?
If it looks like it will work I will calculate the quantities etc.

AllenG · **Reply #34 on:** 26/06/2012 21:30:02

Fe(III)? Don't I need Fe(II)?

AllenG · **Reply #35 on:** 26/06/2012 23:26:04

I herby dub this, The Shoemaker Process.

Shoemaker print: (n.) A photograph printed with meteoritic iron.

Bored chemist · **Reply #36 on:** 27/06/2012 06:14:40

Ferric ammonium citrate is Fe(III).

AllenG · **Reply #37 on:** 27/06/2012 06:54:42

My apologies. I'm doing my best to [strike]relearn[/strike] learn my chemistry, and I'm at least a full step behind where I feel like I should be on the learning curve.

AllenG · **Reply #38 on:** 27/06/2012 20:28:15

The meteorite came in today.
It is a Sikhote-Nlin Meteorite. It fell in 1947 in Primorskiy kray, Russia.

AllenG · **Reply #39 on:** 28/06/2012 02:06:45

After I photograph this thing may I presume my best first course of action would be to put the sample in my vice, go at it with a file and rend some filings to facilitate dissolving it in the acid solution?

Actually, it should be a piece of scrap iron for a proof of concept run.

Bored chemist · **Reply #40 on:** 28/06/2012 13:02:07

Well, there's about 8.5 grams of my lump of metal left.
but I'm bored of waiting so I'm heating the stuff up to speed the reaction.

It looks to me as though that meteorite has a layer of oxide on the surface which could be rather resistant to acid.
Hacksawing it in half would probably help (and it would be a lot less tiresome than turning it into iron filings.)

A proof of concept with a lump of scrap is a very good idea.
It looks like the lump I have would dissolve in a bit less than a week.
YMMV
(Your meteorite may vary.)

According to this
http://en.wikipedia.org/wiki/Sikhote-Alin_meteorite#Composition_and_classification
there's quite a lot of nickel in it, and I doubt that would help the photography any.

Once I have dissolved my lump of scrap I will add some nickel, just to see if I can remove it again.

AllenG · **Reply #41 on:** 28/06/2012 19:04:51

It was heat blued during atmospheric entry. Better job than what was done on a few of my antique black powder rifles too.

AllenG · **Reply #42 on:** 29/06/2012 01:50:17

One more step forward today. I purchased some Potassium Ferricyanide so I may have a part B for making meteoritic cyanotypes. With that addition to my supplies I should have the materials to create about 5 different types of iron based prints.

I also ordered a quantity of nitric acid for making silver nitrate. Tomorrow I'll look for a manky sterling spoon or some coin silver to render. I'm going to jinx myself here, but compared to F.A.C., silver nitrate looks like it will be rather simple to synthesize.

Bored chemist · **Reply #43 on:** 29/06/2012 08:46:29

Watch out for the fumes when you dissolve it.
Oxides of nitrogen have a nasty reputation of being delayed action poisons.
Simple answer is to set it up outside and walk away.
Anyway, the lump of mild steel has dissolved and I'm filtering the solution before I add some hydrogen peroxide to convert it to ferric sulphate.

Bored chemist · **Reply #44 on:** 29/06/2012 10:18:42

I just checked and I'm out of ammonia.
If I can't find some for sale today when I'm in town I will use sodium hydroxide and an excess of ammonium sulphate.

Bored chemist · **Reply #45 on:** 29/06/2012 17:36:06

Good news: found ammonia on sale.
Bad news: knocked stuff over + will have to start again.

AllenG · **Reply #46 on:** 30/06/2012 02:05:41

BC,
That's tragic and this is a lot of effort to go through. Your guidance has been invaluable (overwhelmingly kind to be honest). Don't go through the trouble of starting fresh on my account.

AllenG · **Reply #47 on:** 30/06/2012 02:12:10

I found some US coin silver (half a dozen pre 1965 quarters). They didn't have any Silver Eagles or Silver Maple Leaves. I'm going to hold out until I can find some of those because of their purity.
I think I am aso going to make some silver nitrate first because it is seemingly easier. Good practice for making the F.A.C.

Ok, up until now mixing my sensitizers has been dissolving ingredients in water--cooking not chemistry.
Is silver nitrate ~63% silver by weight?

Bored chemist · **Reply #48 on:** 30/06/2012 12:27:50

I don't think it's tragic: just a bit annoying (and a bit messy).
I'm going to do it again just to check up on the difficult bits- cleaning nickel etc out of the mixture and turning it into the citrate.
Getting pure silver is a good idea and yes AgNO3 is about 63% silver (107.87/168.7)

AllenG · **Reply #49 on:** 30/06/2012 12:49:37

Quote from: Bored chemist on 30/06/2012 12:27:50

I don't think it's tragic: just a bit annoying (and a bit messy).
I'm going to do it again just to check up on the difficult bits- cleaning nickel etc out of the mixture and turning it into the citrate.

Thank you for that.

Quote from: Bored chemist on 30/06/2012 12:27:50

Getting pure silver is a good idea and yes AgNO3 is about 63% silver (107.87/168.7)

Ha! Alright, I'm actually remembering my education.

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Author Topic: How to make Ferric Ammonium Citrate? (Read 5343 times)