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Author Topic: How to make Ferric Ammonium Citrate?  (Read 19647 times)

Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #50 on: 01/07/2012 17:40:06 »
Well, I'm back where I was before it went belly up.
To recap:
23.5 g of steel pipe was added to a solution of 50ml (86g) of drain cleaning grade H2SO4  in 200 ml of water.

This was kept warm and left to react. ( I warmed it up each hour or so and left it in an insulated bucket between warmings)
Most of the reaction took 4 hrs but I left it overnight to finish. (I left the reaction outside- the fumes smell pretty bad and I suspect they contain some arsenic hydride.)
The solution had cooled overnight and quite  a bit of FeSO4.7H2O had crystallised out.
I warmed the solution to dissolve this then filtered it.
Then I added H2O2
The stuff I have is 17.5% bought from a hydroponics' supply shop.
In theory I needed 7.2 grams to oxidise all the iron to Fe(III) but I used a bit more than twice that much (100 ml)
because part of it will decompose before it reacts.
This step in the reaction gets quite hot and fizzes like crazy.
I left this to cool and for any excess H2O2 to decompose.
Then I added 60 g of( NH4)2SO4  and heated the solution to get it to dissolve
(I used stuff recrystallised from fertiliser grade material. The purity of things isn't that critical yet)
Added a ;littl nickel carbonate to see if I ca remove it again.
I'm now going to let it cool down before I add the ammonia.
The stuff I bought doesn't state a concentration. I'm guessing its about 10% but I will measure the density and see how that tallies.
« Last Edit: 01/07/2012 18:27:20 by Bored chemist »
 

Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #51 on: 02/07/2012 19:42:55 »
Well, left to cool overnight the mixture produced some nice looking crystals of ferric ammonium sulphate. (Iron alum)
That's likely to be nice and pure (most of the other ions present wouldn't fit into the crystal properly).
So, I think I will cool it in the fridge and collect the crystals and use them. They yield might not be good enough, but I will see how that goes.
 

Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #52 on: 03/07/2012 03:39:41 »
I have ordered a Silver Egale and a Silver Maple Leaf as well as some nitric acid for the silver nitrate.
I also ordered some H2SO4.

Living in the sticks means the whole world is 5-7 UPS shipping days away.
You can find anything one may need, but it always takes a week to arrive.

« Last Edit: 03/07/2012 03:42:35 by AllenG »
 

Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #53 on: 03/07/2012 20:13:49 »
It seems I'm a slight idiot. I only thought to order some citric acid on Sunday. However, with luck it will be here soon enough.

The ferric ammonium sulphate is rather pretty violet crystals.
I poured the liquid off and added excess ammonia.
I'm filtering off the precipitated iron hydroxide from that  (The liquid is blueish green so the nickel has stayed in solution and only the iron has precipitated. Goody)
I will dissolve the alum and precipitate the iron hydroxide from that later probably with sodium hydroxide- that's cheap and since the iron alum has enough ammonia in it and is fairly pure already I can keep the rest of the ammonia solution for later .

 

Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #54 on: 03/07/2012 21:20:55 »
Excellent.
I'm still waiting for my chemicals to be delivered. With the Fourth of July holiday tomorrow everything is going to be a day or more delayed.

Good news, I was in a town about 20 miles away doing some business and happened to drive by a pawn shop that had in small print at the bottom of their sign, Coin Dealer.  So I stopped.  The proprietor did have Silver Eagles and a few in poor condition as far as a numismatist would be concerned and I was able to purchase a few for the price of the silver alone.  As I turned to leave I noticed a wall full of meteorites.  Turns out the owner is a science geek and collects meteorites.  The only meteorite dealer within hundreds of miles from me happens to be located in the next town over. 

Not only does he have Sikhote-Alin meteorites, he also had a handful of Campo del Cielo samples as well.  The Campo del Cielos have been polished too, so no crust of oxidation.  Not wanting to pass on serendipity I bought a 29.563g sample (and for half the price I found the Sikhote-Alin online).

 
Sikhote-Alin (L.), Campo del Cielo (R.)
 

Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #55 on: 05/07/2012 14:47:15 »
Ran into a snag.  The company I ordered my chemicals from will only ship to a business address that is zoned for industrial use and not to a residence.  I work from home and they will only ship to me if my darkroom is physically separated from my property. Need to find a new source now.
 

Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #56 on: 05/07/2012 16:08:21 »
Bother!
I sometimes find ebay sellers are less concerned about such matters.
Anyway, I'm currently washing all the Fe(OH)3.
 

Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #57 on: 05/07/2012 17:03:09 »
Good news, I'm a step closer to getting my NASA press pass.  I want to photograph an Atlas rocket launch and print that in meteorite.
 

Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #58 on: 08/07/2012 03:42:46 »
Ebay did the trick. Thanks.
 

Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #59 on: 08/07/2012 19:12:56 »
Bother!
I sometimes find ebay sellers are less concerned about such matters.
Anyway, I'm currently washing all the Fe(OH)3.

How did it turn out?
 

Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #60 on: 08/07/2012 19:31:55 »
Well, its sitting in a coffee filter waiting for me to work out what to do next. Redissolve it in dilute H2SO4 I think , but I'm still trying to find a definite answer about how much iron there is in "ferric sulphate solution"  according to the pharmacopoeia. There seem to be two answers, 10% or 14%, depending which pages you look at.
 

Offline Geezer

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Re: How to make Ferric Ammonium Citrate?
« Reply #61 on: 09/07/2012 01:07:11 »
Ran into a snag.  The company I ordered my chemicals from will only ship to a business address that is zoned for industrial use and not to a residence.  I work from home and they will only ship to me if my darkroom is physically separated from my property. Need to find a new source now.

I was hoping to find the exploding darkroom scene from Kind Hearts and Coronets on Youtube, but no luck I'm afraid.
 

Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #62 on: 09/07/2012 17:13:22 »
Someone sent me this link:http://holoforum.org/oldforum/viewtopic.php?f=2&t=6561
Interesting, but I think it makes a blob of both green and brown forms of FAC.
 

Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #63 on: 09/07/2012 21:13:13 »
Well, if it works then it works but I'd be worried by the impurities that come from the metal and also from the effect of the electric current on the citrate ions.

Anyway, I (re) started with 23.5g of steel.
That's pretty close to 23.5 g of iron which is 0.42 moles.
If it were pure and I didn't lose any when I did the dissolution etc then I'd have 0.42 moles of Fe(OH)3

I could react that with exactly 1.5 times as many moles of acid (i.e. 63 grams) to dissolve it then dilute it with water to get the 10%( or 13% I haven't quite made up my mind yet) solution I'm after for that recipe.
However I know that the iron wasn't pure and I will have lost some.

So I will use a smaller known amount of acid and stir that up with the Fe(OH)3 sludge.
It makes that maths easy if I use 0.5 moles of acid.
That's 48 grams of pure acid.
The  drain cleaner I have is about 98% (based on the density which I measured as  of 1.83 or 1.84g/ml).
So I need about 50 g of the  98% stuff.
I measured that out and added it to about 50ml of water then stirred in the Fe(OH)3 sludge.
The acid will dissolve the hydroxide and give the sulphate. There will be some left over sludge which I can filter off.
If I run water through the sludge then I will transfer all the  ferric sulphate (pretty close to 2/3 times 0.5 moles) to the solution and so I will have a good idea of the concentration.

It sounds complicated, but It's often taken me as long to type up this stuff as to actually do it.
« Last Edit: 09/07/2012 21:15:38 by Bored chemist »
 

Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #64 on: 14/07/2012 06:14:05 »
My nitric acid came in finally.
I have an ounce of silver dissolving now.  It's going to take quite a while it seems.  It's moving quite slowly.
 

Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #65 on: 14/07/2012 11:19:03 »
Make sure you don't breathe the fumes.
 

Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #66 on: 14/07/2012 11:51:34 »
It is set up in the back garden and I won't approach it without my respirator. There is also a good breeze.
Although the breeze is probably the most important part of that.

The ridges on the side of the coin and the face are gone this morning.  It's going to take days.  Kind of a shame that the heat wave we just had has passed.  It is only going to be 33º today.  It was 42º the other day. That would have sped things up.
« Last Edit: 14/07/2012 12:10:53 by AllenG »
 

Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #67 on: 25/07/2012 04:35:03 »
My first (and probably only) batch of silver nitrate is almost complete.
I had access to a fume hood.  I vacuum filtered it several times and now the batch is sitting in a desiccator drying out. 
I'll make a small batch of VanDyke sensitizer and make a few test prints with it directly.

« Last Edit: 25/07/2012 06:04:52 by AllenG »
 

Offline AllenG

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Re: How to make Ferric Ammonium Citrate?
« Reply #68 on: 04/08/2012 20:56:30 »
Fresh from the print washer

Shoemaker test print-1

This is a kind of Kallitype print called a VanDyke. It is an Iron/Silver print.
The silver came from this US Silver Eagle, and the iron is from the meteorite on the right.

The meteorite is a Campo del Cielo meteorite that fell 4000-5000 years ago in Argentina.
 

Offline Bored chemist

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Re: How to make Ferric Ammonium Citrate?
« Reply #69 on: 04/08/2012 21:54:31 »
Very pretty.
(incidentally I have been away for a couple of weeks)
 

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Re: How to make Ferric Ammonium Citrate?
« Reply #69 on: 04/08/2012 21:54:31 »

 

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