Ferric Oxalate 1 - yellow???

Discussion in 'Alternative Processes' started by sly, Jun 17, 2009.

  1. sly

    sly Subscriber

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    Previously I have used Bostick and Sullivan premixed solutions in little brown bottles for Pt/Pd printing, Na2 method. The ferric oxalate solution from them was slightly coloured, but clear. I ordered powdered chemicals from JD Photochem this time. I have just mixed up 15 grams of Ferric Oxalate with 1 gram of Oxalic Acid and 55 ml of water - as per recipe in CZ Anderson's book "Alternative Processes Condensed". The FO powder is a very pretty yellow colour, and the "solution" is also a very pretty yellow colour. It looks like paint. I don't think any of the powder dissolved - and suspect it will all settle out. Does it need to be heated? Have I got the wrong formula?

    Thanks in advance for your help.
     
  2. JLP

    JLP Subscriber

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    Ferric Oxalate is a pain to dissolve and you need to keep it around 150 degrees for quite some time. Continue to agitate and eventually it will dissolve.
    Good luck.
     
  3. Don12x20

    Don12x20 Member

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    Get one of the plug-in coffee mug warmers(one of those flat ones with a cord...) -- put the bottle on top of that. Shake frequently (loosening the cap after shaking each time) ...it will dissolve in less than an hour.
     
  4. michael9793

    michael9793 Member

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    sounds like a pain, let B&S do it and get a consistent mix every time. I want everything the same every time I have to order Fe.
     
  5. sly

    sly Subscriber

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    I don't know if you've seen the other thread about ordering stuff from the States for delivery in Canada - the crap shoot of delivery charges, duty charges, taxes etc. That's a pain too. (Aside - B&S have been very good in the past about making sure it got here as inexpensively as possible.) I ordered a few hundred dollars worth of chemicals, paper, and other stuff last summer to be sent to a friends in Washington. That worked fine, but Washington is not a place I get to often.
    I try to order within Canada as often as possible.
     
  6. Andrew O'Neill

    Andrew O'Neill Subscriber

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    Hi Sly,

    I have ferric oxalate from JD Photochem, too. It will go into solution but only with great effort. I reheat it in the bottle and then shake the hell out of it until it goes in. The next day if there is some sediment at the bottom of the bottle, I heat up again and give it a good shake. It'll go in eventually. The ferric oxalate from B&S is far superior and goes in with less effort.
     
  7. nworth

    nworth Subscriber

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    Most iron compounds are yellow, as are most of their solutions. More concentrated solutions are more decidedly yellow, but all are pretty distinctly so. I'm not sure what effect the oxalic acid would have, except to dissolve any stray hydroxide that might have formed.
     
  8. sly

    sly Subscriber

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    Well, I dug out the double boiler, put it on the stove and fiddled until I had water at 160 degrees. I put in the jar of FO, warmed it up and shook it alot, put it back in the water when it felt like it was cooling down and repeated the process, over and over for about two and a half hours. As I sit here typing I'm watching the undissolved yellow powder slowly settle to the bottom. There is some dissolved in the water, but it looks to me like the majority is settling out.

    Bedtime now. Should I try again tomorrow? Use a higher temperature? IS THE FORMULA WRONG? Throw it all away and give up?

    PS I think the oxalic acid is supposed to be a preservative.
     
  9. Loris Medici

    Loris Medici Member

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    I used only B&S ferric oxalate, which dissolves completely overnight. I just mix the solution w/ room temperature distilled water, stir/shake well every couple of hours until I get to sleep, it's completely clear in the morning. Some prefer to add small amnts. of oxalic acid and/or EDTA to facilitate dissolution - which indeed does so...

    Regards,
    Loris.
     
  10. tim_bessell

    tim_bessell Member

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    It's an exercise in patience.

    I used some from Artcraft Chemicals, two days later, completely dissolved. I gently warmed and stirred it in my pocket.
     
  11. colrehogan

    colrehogan Member

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    My Ferric Oxalate solutions from B&S are yellow. But I bought the solutions pre-mixed.
     
  12. sly

    sly Subscriber

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    Yellow yes, but transparent. This morning there is 1/2 inch of opaque yellow sludge in the bottom of the jar and 1 and a half inches of yellow transparent fluid on top. Maybe I'll try adding a bit more oxalic acid, if that helps it dissolve better.
     
  13. timgray@rogers.com

    timgray@rogers.com Member

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    I've never run into any inconsistency in having B&S delivered to Toronto. UPS expedited and taxes have always been consistent and I've never had to pay any duties. One trap is UPS "cheap" you end up having a brokerage charge on top that makes it no less expensive than expedited.
     
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  15. Andrew O'Neill

    Andrew O'Neill Subscriber

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    Sly,

    Are you sure that you are heating the solution up enough? I make sure my solution is about 70 C before pouring in the ferric oxalate. A microwave makes this so much easier.
     
  16. sly

    sly Subscriber

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    I wasn't sure if it would be safe in a microwave. The water was room temperature when I added the powder, the heat came later. Does that make a difference? I've got it back in the double boiler now, with an extra gram of oxalic acid. Last night I held the temperature at 70C (155F). Tonight I'm trying at 85C (about 190F).

    I've sent an email to the supplier to ask advice as well.
     
  17. tim_bessell

    tim_bessell Member

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    After all that mucking around, I'm sure you will find that if you just give it several days, it will go into solution on its own. At that time, you will make a fresh batch, for fear all the heating, added chems, and what not have spoiled or altered your FO beyond use.:wink:
     
  18. Andrew O'Neill

    Andrew O'Neill Subscriber

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    It's safe in a microwave. You really should start with hot water before putting the ferric oxalate in. If you do have to reheat, do not boil!!
     
  19. Dana Sullivan

    Dana Sullivan Advertiser Advertiser

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    Just a note. I've found that you should only heat the ferric oxalate solution once to disolve the powder into solution. My experience has shown that multiple heatings will cause the ferric oxalate to break down and a massive amount of grain to appear in your images.

    When I make up quantities of liquid ferric oxalate for sale, I measure out distilled water in a glass beaker, which I then stick in a microwave oven until boiling. I remove the beaker from the microwave and add the powdered ferric oxalate and stir for a minute or two.

    I don't have problems disolving all of the powder using this method, but if I did, I would allow all of the undisolved particles to settle to the bottom, and decant the solution off the top.

    This is the first I've heard of JD photochem, so I'm not familiar with their product. Are they manufaturing their own, or re-selling someone elses ferric oxalate?
     
  20. Andrew O'Neill

    Andrew O'Neill Subscriber

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    Dana, as far as I know, JDPhotochem does not manufacture ferric oxalate. A lot of times when I order certain chemicals, they have to get them from a supplier. That includes ferric oxalate. JDPhotochem is in Quebec, Canada.

    http://www.jdphotochem.com/

    Their website hasn't been updated for quite a few years...
     
  21. photomc

    photomc Member

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    This is method I have used and find it works very well. I shake rather than stir...and may have to repeat 1 more time, but have not had to reheat since changing to this method of using very hot distilled water.
     
  22. sly

    sly Subscriber

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    Thank you Dana and everyone for your advice. I tried again. No luck.

    I tossed the concotion that has been sitting undissolved for a week and started from scratch
    Distilled water - heated in microwave to just boiling, premeasured ferric oxalate and oxalic acid added, stirred briefly, poured into glass bottle and then shaken non-stop for 1/2 hour (until it had completely cooled).

    It's been sitting for over an hour now and the sludge is settling. Bottom half of the contents is sludge, the top half liquid. Doesn't seem to be any more dissolved than the first batch.

    I'll decant the stuff on top and try a test print, but it really looks like most of the ferric oxalate did not dissolve.

    I keep wondering if the formua I have is all wrong. Either that, or there's something wrong with the ferric oxalate.
     
  23. pateeid

    pateeid Member

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    i wonder how long can we keep #1?
     
  24. sly

    sly Subscriber

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    I've read about 6 months - if it is refrigerated between uses. The ferric oxalate I bought last summer (premixed) worked fine through the fall. It was useless in March.
     
  25. colrehogan

    colrehogan Member

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    When you say it was useless, what happened? Did you try to print and get nothing? What happens when FO has died, so to speak? I'd really like to know.
     
  26. sly

    sly Subscriber

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    Exposures were much longer (with same lights) than before. 20+ minutes rather than 5-10 as previously. Prints were flat, impossible to get any contrast to them.