How to make Ferric Ammonium Citrate?

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Offline AllenG

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How to make Ferric Ammonium Citrate?
« on: 23/06/2012 21:23:50 »
I'm an alternative process photographer.  Meaning I print my photographs with 19th century formulas.
I get great satisfaction from mixing my own forumlas.  I also like to tie my images directly to where they were originally captured.  For instance, the image below was shot on the bank of the Arno river. After I captured the image I went went down to the Arno and collected a gallon of water which I then filtered and used in the development process. I want to take this a step further.   I live on the coast of Georgia (state not country) and there is a goodly amount of iron in the sand.  I can collect it with a strong magnet. 

Can one make ferric ammonium citrate in a home lab?  And if so how would I go about accomplishing it?


This is a VanDyke print.  The formula I used was a 9% solution of ferric ammonium citrate, 1.5% tartaric acid, and 4% silver nitrate.  The water was distilled from the Arno, and then the print was developed in filtered Arno water. 

The above is really simple to do.  Dissolve the required chemicals (which can be purchased from many photography supply houses) to the desired solutions in distilled water, and then mix the three solutions together and one has VanDyke sensitizer.

If I can make my own F.A.C. one of the things I plan on doing is collecting micrometeorites and creating an image that is at least in part made of extraterrestrial iron.  My house has a few rain barrels and they always have a bit of sediment collected in the bottom, mostly bits of leaf and bird dirt, but if one runs a rare earth magnet through it, it always comes up with some ferric material.  Part of that material has to be micrometeorites.

Thank you for reading through my hair brained idea,

--Allen
« Last Edit: 24/06/2012 01:44:19 by AllenG »

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Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #1 on: 23/06/2012 21:53:50 »
I think I have a recipe somewhere. I will try to remember where and dig it out for you.
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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #2 on: 24/06/2012 01:06:36 »
I couldn't thank you more.

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Offline distimpson

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Re: How to make Ferric Ammonium Citrate?
« Reply #3 on: 24/06/2012 02:40:31 »
Hi Allen, really like your idea of using meteorite iron in the photographic process. I've got meteorite saw dust from cutting brenham pallasites, it is roughly a 50:50 mix of the metal (~90% iron and 10% nickel) and the magnesium/iron/nickel silicates. The saw dust is in mineral oil. I do not know how to convert the metal to the ammonium citrate. But if you can use some of this material i'd be happy to supply it for your project. don

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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #4 on: 24/06/2012 05:42:40 »
Hi Allen, really like your idea of using meteorite iron in the photographic process. I've got meteorite saw dust from cutting brenham pallasites, it is roughly a 50:50 mix of the metal (~90% iron and 10% nickel) and the magnesium/iron/nickel silicates. The saw dust is in mineral oil. I do not know how to convert the metal to the ammonium citrate. But if you can use some of this material i'd be happy to supply it for your project. don
Don,
That is astoundingly generous. PM me your contact info and I'll PayPal you the funds for its cost and shipping.
If I can get a working sensitizer I'm going to contact NASA and get my press pass reinstated.  I'll send you and Bored Chemist meteorite prints of the last rocket to ever be launched from the Cape.

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Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #5 on: 24/06/2012 12:31:57 »
Well, I have tracked down my copy of Bentley and Driver's text book of Pharmaceutical Chemistry (1951).
Now all I have to do is remember how to upload an image. (and see if I can resize it to fit)
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Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #6 on: 24/06/2012 12:32:44 »
And part II


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Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #7 on: 24/06/2012 12:33:47 »
Let me know if that makes any sense.
I realise that it's not the most accessible language.

According to this
http://www.google.co.uk/url?sa=t&rct=j&q=%22solution%20of%20ferric%20sulphate%22&source=web&cd=5&ved=0CFEQFjAE&url=http%3A%2F%2F
www.sciencemadness.org%2Ftalk%2Ffiles.php%3Fpid%3D140008%26aid
%3D6594&ei=Wi3nT4zKN4KLhQfqyanNCQ&usg=AFQjCNGrWhAaNUeSJ_yXH34E0iJr4LAt0g
the ferric sulphate solution contains 10% iron by weight so the 40 ml of it that the recipe calls for would need about 4 grams of iron. That's a lot of meteor dust.
Is this project still plausible if we use ordinary iron for most of it, and just a bit of stardust?
That 4 grams of iron would produce about 20g of ferric ammonium citrate. How much does the photography need?




I have edited the address above so (hopefully) it doesn't mess up the formatting of the thread any more. You will need to patch it together if you want to follow it.
« Last Edit: 24/06/2012 21:23:07 by Bored chemist »
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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #8 on: 24/06/2012 17:05:19 »
The recipe I use calls for 9 grams of ferric sulphate. 
For each print 8x10 I use about 4ml of sensitizer.


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Re: How to make Ferric Ammonium Citrate?
« Reply #9 on: 24/06/2012 18:05:44 »
ferric sulphate.  ?
Ferric Sulphate or ferric ammonium citrate?
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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #10 on: 24/06/2012 19:05:10 »
Ferric ammonium citrate.  Sorry. I was still in need of my morning caffeine when I wrote that.

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Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #11 on: 24/06/2012 19:18:42 »
9 grams of ferric ammonium citrate would imply about 1.9 g of iron. That's still rather a lot of meteorite.
(and I apologise for messing up the thread formatting with that long link.)
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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #12 on: 24/06/2012 19:46:42 »
Meteorites are cheeper than I would have thought.


This sample of Sikhote-Alin Iron Meteorite is 19 grams and is up for sale for ~30.

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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #13 on: 24/06/2012 20:56:01 »

Just bought this meteorite for the project. It weighs in at 22.5 grams.

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Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #14 on: 24/06/2012 21:09:28 »
Cool!
I guess that, since you make your own photographic chemicals that you have some sort of access to chemicals and equipment
 (or that, at least, you are not too frightened of them).


Incidentally, do you ever do "blue print" pictures? In that case the pigment that makes the image contains iron which could be derived from a meteorite too.
« Last Edit: 24/06/2012 21:21:30 by Bored chemist »
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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #15 on: 24/06/2012 21:23:53 »
Cool!
I guess that, since you make your own photographic chemicals that you have some sort of access to chemicals and equipment
 (or that, at least, you are not too frightened of them).
No real fear.  I'm going to proceed slowly, carefully, and as well informed as I can be and hope for the best.
My darkroom is pretty well equipped. Up until now I've been mostly dissolving chemicals in water and then mixing the
solutions to create my needed formulas. 
This will be my first try at more advanced chemistry since I was in school (I think one of the Henrys was king at the time).
 I may end up going to one of the local universities' chemistry departments and see if I can get a professor to help walk me
through the creation of the first batch.

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Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #16 on: 24/06/2012 22:28:38 »
I think the slow bit is going to be dissolving the metal in the first place.
You might want someone with a fume cupboard to help there, unless you are prepared for a long wait.
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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #17 on: 25/06/2012 01:59:16 »
Right.  Good point. 
I think finding the meteorite was the easiest part of this project. Now the hard part starts.

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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #18 on: 25/06/2012 02:07:07 »
Incidentally, do you ever do "blue print" pictures? In that case the pigment that makes the image contains iron which could be derived from a meteorite too.
I do make cyanotypes. I haven't in a while and I don't really know why. 
A blue picture from space.  I should make a portrait of the Tardis or Matt Smith for that.

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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #19 on: 25/06/2012 16:44:47 »
Once my meteorite arrives how does one go about determining its oxidation state?

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Re: How to make Ferric Ammonium Citrate?
« Reply #20 on: 25/06/2012 19:23:24 »
It's current oxidation state will be practically zero. It's a lump of metal.
I'm currently running an experiment to see how quickly a lump of steel weighing about 20g takes to dissolve in dilute sulphuric acid. (50 ml H2SO4 + 200 ml H2O) It's disappointingly slow at the moment, but I'm thinking about that one.
How does this idea of heating the meteorite to red hot and pounding it flat with a hammer grab you?
With cyanotypes you could certainly use meteorite iron for half the iron in the blue pigment, and for all of it if you don't mind using cyanides.
(Can we take the safety warnings as read here please. I'm a real live, trained, experienced chemist and I would probably shy away from using cyanides, especially at home)
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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #21 on: 25/06/2012 19:40:14 »
I have no problem at all grinding, heating, or doing whatever needs to be done with the meteorite. 
I don't mind using cyanides.  There are a goodly amount of chemicals that I use that need to be treated with respect. 

Again, thank you  so very much for your help.  It's been invaluable to me.

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Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #22 on: 25/06/2012 21:28:45 »
The iron is dissolving: slowly. It's generating something like 1 ml of hydrogen every 10 seconds. (To the nearest order of magnitude. It's hard to measure exactly.)
With 20 g of iron I will get something like 10 litres of gas in total. About a day to react (or maybe a week  with the poor accuracy of measurement).
And I suspect it's getting slower.
I'm putting it on something warm like a plant propagator.


And I'm happy to help by the way. This is a fascinating project.

Remaining mass 21.2g at 21:45
« Last Edit: 25/06/2012 21:43:38 by Bored chemist »
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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #23 on: 26/06/2012 00:05:30 »
I contacted NASA today and went through the motions to get my press pass reactivated. 
The last launch at the Cape is coming up at the end of the summer.  I think a series of the last Atlas rocket printed in meteorite will be a worthy subject for this project.

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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #24 on: 26/06/2012 00:54:35 »
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.

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Offline distimpson

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Re: How to make Ferric Ammonium Citrate?
« Reply #25 on: 26/06/2012 00:58:08 »
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.

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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #26 on: 26/06/2012 01:10:10 »
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.


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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #27 on: 26/06/2012 01:33:15 »
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.

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Offline RD

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Re: How to make Ferric Ammonium Citrate?
« Reply #28 on: 26/06/2012 04:03:27 »

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Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #29 on: 26/06/2012 06:59:40 »
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?
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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #30 on: 26/06/2012 07:08:54 »
What percent?  I can order it.

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Re: How to make Ferric Ammonium Citrate?
« Reply #31 on: 26/06/2012 19:14:22 »
Hang fire on ordering it. I might as well check if it works nicely first.
Mass of iron lump now 16.2 g
« Last Edit: 26/06/2012 20:52:49 by Bored chemist »
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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #32 on: 26/06/2012 21:26:46 »
Thank you.
The hydrogen peroxide I have is the stuff in the medicine cabinet one purchases from the pharmacy.

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Re: How to make Ferric Ammonium Citrate?
« Reply #33 on: 26/06/2012 21:47:46 »
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.
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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #34 on: 26/06/2012 22:30:02 »
Fe(III)?  Don't I need Fe(II)?

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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #35 on: 27/06/2012 00:26:04 »
I herby dub this, The Shoemaker Process.

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

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Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #36 on: 27/06/2012 07:14:40 »
Ferric ammonium citrate is Fe(III).
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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #37 on: 27/06/2012 07:54:42 »
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.

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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #38 on: 27/06/2012 21:28:15 »
The meteorite came in today.
It is a Sikhote-Nlin Meteorite.  It fell in 1947 in Primorskiy kray, Russia.

« Last Edit: 27/06/2012 22:50:24 by AllenG »

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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #39 on: 28/06/2012 03:06:45 »
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.
« Last Edit: 28/06/2012 04:03:28 by AllenG »

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Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #40 on: 28/06/2012 14:02:07 »
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.
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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #41 on: 28/06/2012 20:04:51 »
It was heat blued during atmospheric entry. Better job than what was done on a few of my antique black powder rifles too.


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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #42 on: 29/06/2012 02:50:17 »
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.
« Last Edit: 29/06/2012 05:34:55 by AllenG »

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Re: How to make Ferric Ammonium Citrate?
« Reply #43 on: 29/06/2012 09:46:29 »
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.
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Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #44 on: 29/06/2012 11:18:42 »
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.
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Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #45 on: 29/06/2012 18:36:06 »
Good news: found ammonia on sale.
Bad news: knocked stuff over + will have to start again.
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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #46 on: 30/06/2012 03:05:41 »
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.

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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #47 on: 30/06/2012 03:12:10 »
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?
« Last Edit: 30/06/2012 03:45:33 by AllenG »

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Re: How to make Ferric Ammonium Citrate?
« Reply #48 on: 30/06/2012 13:27:50 »
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)
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Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #49 on: 30/06/2012 13:49:37 »
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.

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.