Ferric Oxalate

Andrew O'Neill · Mar 10, 2007

I'm hoping that Sandy King or someone else with lots of experience with kallitypes will respond. I am mixing up some FO for the first time in distilled water at about 52 C. It's sitting on a hot plate.
Man, they weren't kidding when they said it takes a long time to go into solution.
When I mixed in the FO it looks creamy coloured. I'm mixing mixing mixing...getting pretty sick of mixing. It's still hasn't mixed in. When it is finally in solution, is it clear? What does it look like?

donbga · Mar 10, 2007

Andrew O'Neill said:
I'm hoping that Sandy King or someone else with lots of experience with kallitypes will respond. I am mixing up some FO for the first time in distilled water at about 52 C. It's sitting on a hot plate.
Man, they weren't kidding when they said it takes a long time to go into solution.
When I mixed in the FO it looks creamy coloured. I'm mixing mixing mixing...getting pretty sick of mixing. It's still hasn't mixed in. When it is finally in solution, is it clear? What does it look like?

Andrew,

A 20% mixture of FO for kallitype should go into solution fairly quickly if you start with distilled water heated almost to boiling. You may have to keep the solution heated (@ 170-200F) and shake it a few times to get it to dissolve. With fresh powdered FO I can get mine dissolved in a few minutes working with water this hot.

When the FO dissolves it should be clear not milky. If it hasn't dissolved completely over night and it's still cloudy you may have some bad FO.

Don Bryant

Andrew O'Neill · Mar 10, 2007

Well, I had the solution up to about 76 Celcius, stirring occasionally. Don't know if it all went in as I was working under a very weak light. I let it cool and bit and then poured it into a little brown bottle. I'll let it sit until tomorrow morning. If it hasn't cleared, I'll try it one more time starting with the solution at 76 (about 170 F) and then complain to the place I got the FO from if it still doesn't work.
Thanks for your help!

clay · Mar 10, 2007

When and from whom did you get the ferric oxalate? I got one strange batch from B&S last July that just would not go into solution.Even after on and off stirring and heating over a two week period. Another batch I got later goes into solution in less than an hour. I sent the goofy batch back to them for an exchange, which they were glad to do.

sanking · Mar 10, 2007

Andrew O'Neill said:
I'm hoping that Sandy King or someone else with lots of experience with kallitypes will respond. I am mixing up some FO for the first time in distilled water at about 52 C. It's sitting on a hot plate.
Man, they weren't kidding when they said it takes a long time to go into solution.
When I mixed in the FO it looks creamy coloured. I'm mixing mixing mixing...getting pretty sick of mixing. It's still hasn't mixed in. When it is finally in solution, is it clear? What does it look like?

It seems that a lot of weird FO is going around. I don't understand it at all. I was using a batch late last year from Artcraft that had previously gone into solution with no problem. Then, the next batch I tried to mix would not go into solution at all, in spite of much patience, stirring and heat. I was pretty desperate since I needed to make some prints and Clay saved my butt by sending me some of his mixed FO.

Since then I tried another batch (not going to mention suppliers here because I have had problems withi FO from all three of the big one) and it would not go into solution either.

I took all of this as a sign from the gods that I needed to go back to carbon printing and leave all of this heavy metal printing to greater minds.

One thing that did seem important to me was a note from one of the B&S boys, can't remember if it was Kevin or the hard-working one, to the effect that you should only heat the solution once, since in the B&S researcha and data they had seen some negative with regard to results from multiple heatings.

Sandy King

Andrew O'Neill · Mar 10, 2007

Thanks for replying, Sandy.
I went down into my darkroom to take a look at my FO. I could see a little light mocha-coloured sludge on the bottom of the bottle. I poured a wee bit of the liquid out into a glass and it is kind of a light yellowish colour. Does that sound normal?
I purchased the FO from Jdphotochemical in Quebec, Canada.

bill schwab · Mar 10, 2007

Andrew O'Neill said:
.. it is kind of a light yellowish colour. Does that sound normal?

That sounds right.

Bill

Andrew O'Neill · Mar 12, 2007

I spent all day in my darkroom. I mixed up the sensitizer and brushed it on my paper. Exposed for about 7 minutes, developed in sodium citrate, cleared in EDTA (I didn't have any citric acid), and fixed. Didn't bother with toning. I'll worry about that when I nail down exposure/dev and processing.

Just by looking at the print I can tell that I over exposed it. The highlights are too dark. I backed off on the exposure quite a bit but highlights still have slight reddish/brown tinge. Is this the stain that needs to be removed by the clearing bath? Is citric acid better than EDTA? The paper I used was good for Van Dykes...I even gelatin sized it.

Also, the darkest areas are a bit spotty...not grainy...detail is lost. Any ideas what could be causing this?

Man this is hard when one is on ones own and one has no real kallitype to look at...

donbga · Mar 12, 2007

Andrew O'Neill said:
I spent all day in my darkroom. I mixed up the sensitizer and brushed it on my paper. Exposed for about 7 minutes, developed in sodium citrate, cleared in EDTA (I didn't have any citric acid), and fixed. Didn't bother with toning. I'll worry about that when I nail down exposure/dev and processing.

Just by looking at the print I can tell that I over exposed it. The highlights are too dark. I backed off on the exposure quite a bit but highlights still have slight reddish/brown tinge. Is this the stain that needs to be removed by the clearing bath? Is citric acid better than EDTA? The paper I used was good for Van Dykes...I even gelatin sized it.

Also, the darkest areas are a bit spotty...not grainy...detail is lost. Any ideas what could be causing this?

Man this is hard when one is on ones own and one has no real kallitype to look at...

Can you post a scan of the print? Which paper are you using? Generally there should be not need to gelatin size the paper.

sanking · Mar 12, 2007

Andrew O'Neill said:
I spent all day in my darkroom. I mixed up the sensitizer and brushed it on my paper. Exposed for about 7 minutes, developed in sodium citrate, cleared in EDTA (I didn't have any citric acid), and fixed. Didn't bother with toning. I'll worry about that when I nail down exposure/dev and processing.

Just by looking at the print I can tell that I over exposed it. The highlights are too dark. I backed off on the exposure quite a bit but highlights still have slight reddish/brown tinge. Is this the stain that needs to be removed by the clearing bath? Is citric acid better than EDTA? The paper I used was good for Van Dykes...I even gelatin sized it.

Also, the darkest areas are a bit spotty...not grainy...detail is lost. Any ideas what could be causing this?

Man this is hard when one is on ones own and one has no real kallitype to look at...

Regarding exposure, remember the mantra, expose for the shadows, develp for the highlights. In alternative printing what you do is first determine the correct exposure to give maximum density, then adjust development so that the exposure scale of the process matches the DR of your negative. If we do this, the highlight should have the right density when the print is given the shortest exposure needed to get maximum density in the shadows. If this does not happen you will need to adjust the contrast, either by developing your negatives for more contrast, or adding dichromate to the developer to give more contrast in the print.

Grainy look results from pape choice. Most papers that work for pt/pd work equally well for kallitype. Lots of grain suggests that the paper you chose does not have a good sizing.

Gelatin sizing is not needed in kallitype and pt/pd printing. In fact, it can cause a lot more problems. Some of the early work done with kallitype a century or so ago have formulas for including gelatin in the coating, and it can be made to work, but not easily.

Sandy King

clay · Mar 12, 2007

Unless you are using di-sodium EDTA, you may not be clearing the paper. The more commonly available tetrasodium EDTA has a basic pH, and if used alone, will lock the ferric into the paper for keeps. I would always make sure that your first clearing tray has a clearing solution with a pH below 7 - whether that is citric acid, phosphoric acid, di-sodium EDTA or muriatic. If you hit that just-developed paper with a basic (pH>7) solution, you are going to be creating only headaches for yourself.

Andrew O'Neill said:
I spent all day in my darkroom. I mixed up the sensitizer and brushed it on my paper. Exposed for about 7 minutes, developed in sodium citrate, cleared in EDTA (I didn't have any citric acid), and fixed. Didn't bother with toning. I'll worry about that when I nail down exposure/dev and processing.

Just by looking at the print I can tell that I over exposed it. The highlights are too dark. I backed off on the exposure quite a bit but highlights still have slight reddish/brown tinge. Is this the stain that needs to be removed by the clearing bath? Is citric acid better than EDTA? The paper I used was good for Van Dykes...I even gelatin sized it.

Also, the darkest areas are a bit spotty...not grainy...detail is lost. Any ideas what could be causing this?

Man this is hard when one is on ones own and one has no real kallitype to look at...

Andrew O'Neill · Mar 13, 2007

The print is actually not grainy...just a bit spotty in some places. After careful examination, the spottyness appears to be the texture of the paper. I read somewhere that gelatin sizing is supposed to help increase Dmax...this paper worked well when I did Vandykes.
Does anyone know if humidity is important? The humidity was about 70 in my darkroom. Thanks for all your help.

Andrew O'Neill · Mar 13, 2007

Thanks for that info, clay. Very interesting.

Alan Davenport · Mar 13, 2007

clay said:
The more commonly available tetrasodium EDTA has a basic pH, and if used alone, will lock the ferric into the paper for keeps.

If all you have is the tetrasodium version, a solution with equal spoonfulls of tetrasodium EDTA and sodium bisulfite or metabisulfite will give you a pH of about 6.5.

Alan

Alan Davenport · Mar 14, 2007

Andrew O'Neill said:
Does anyone know if humidity is important? The humidity was about 70 in my darkroom.

Yes, the relative humidity in your darkroom is very important! A relative humidity of 70% is envyable. When I started coating this winter I purchased a wet-dry bulb hygrometer and the RH varies between 85% on wet days and 65% on dry days. I'm waiting to see what summer will bring.

I see we both live on the west coast.

clay · Mar 14, 2007

Yep. the bisulfite is acidic and will lower the pH. That is why homebrew hypoclear needs this in addition to the sodium sulfite to be effective in clearing. Good point!

Alan Davenport said:
If all you have is the tetrasodium version, a solution with equal spoonfulls of tetrasodium EDTA and sodium bisulfite or metabisulfite will give you a pH of about 6.5.

Alan

Lukas Werth · Mar 14, 2007

Let me come back to the non-dissolving FO: could it be that what does not go into solution is just ferrous oxalate? In powder form, it looks just the same!

A text to find out is: forget about heating the FO, but make up some concentrated oxalic acid by heating that, pur a little into the would-be solution, add some peroxide dropwise until a visible reaction occurs, stir, repeat until the content in the beaker becomes an amber-coloured, transparent solution. Then test for traces of ferrous.

If this works, you had a significant amount of ferrous oxalate in your batch (which you now removed in the solution).

Andrew O'Neill · Mar 23, 2007

Thanks guys, for all your help. I've been in the darkroom playing around with the process and love it. It doesn't always work but when it does...since I've got a ton of EDTA of the wrong type, I'll try adding sodium sulfite to it. Thanks!
I like using sodium citrate as the developer. Ran out of it so tried a combo of rochelle salt, borax, and tartaric acid (lots of borax and very little rochelle salt)...really nice colour but I think I'll stick with sodium citrate when it ever decides to arrive at my door.

One observation I've made:

Prints that are exposed and process soon after coating (dry but cool to the touch) seem to clear faster.
coated papers that had a good day sitting in the dark before exposure and processing seemed to take much much longer to clear or not totally clear at all. Also, upon pouring in the developer on the exposed print I noticed that some of the coating on areas outside of the negative had a washed out look.
Has anybody noticed this before?

And a question:

I work under a safelight and a very weak tungsten light...how bright can I have my darkroom when coating and processing? It's difficult to see if paper has totally cleared unless I put the light up bright.

One more question:

When will all this bloody rain END?? Alan, are you getting lots of rain down there??

Alan Davenport · Mar 24, 2007

Andrew O'Neill said:
Also, upon pouring in the developer on the exposed print I noticed that some of the coating on areas outside of the negative had a washed out look.
Has anybody noticed this before?

...how bright can I have my darkroom when coating and processing? It's difficult to see if paper has totally cleared unless I put the light up bright.

When will all this bloody rain END?? Alan, are you getting lots of rain down there??

Andrew,

Are you leaving enough paper around the margins of your image in order to extend the coating out away from the image? If not you may be thinning out the coating near the edges of your image.

I have one 60w bug light over my coating area and another as a general room light screwed into the ceiling.

It has nice here Thursday but it has been raining most of today. It is supposed to rain through the weekend and on into next week.

Alan

Andrew O'Neill · Mar 24, 2007

rain rain...nothing but rain...oh well.

Yes, I'm leaving plenty of room outside of the image area. I tried again this morning and it didn't happen...gremlins, I tell ya.
I sorted out the yellow staining...If my exposures are too long it happens. I'll have to do more testing at the negative side of things. I'm developing my film in pyrocat-HD. I'll have to cut way back on dev time. My xtol developed negs print nicely. More testing. Perfect for weather like this!

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