Testing fiber prints for residual hypo

[logan2z]

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I recently started using a Versalab print washer and purchased the Photographer's Formulary residual hypo test to see if I am washing my fiber prints sufficiently.  For reference, I'm using Ilford's Rapid fixer at 1+9 and fixing for 2 minutes as per Ilford's instructions, and I'm leaving the prints to soak for 10 minutes (with intermittent agitation) in Ilford's Wash Aid before putting them in the print washer.  I'm leaving them in the washer for 30 minutes.  Paper is Ilford Multigrade Fiber.  Unfortunately, after this procedure the hypo test shows a rather dishearteningly dark brown stain on the border of my prints.  FWIW, I also washed the prints in the print washer for 60 minutes without the wash aid and got a similar result.  Here's a picture of the stain after blotting:

 

 

This seems rather unacceptable to me.  I am not sure which part of my workflow I should adjust to ensure more thorough washing, but I seem to be following a pretty standard fix/wash procedure.  I could wash for longer but I was told by Ilford that I should stick to a maximum of 30 minutes in the print washer to ensure that the emulsion doesn't become damaged.  Any thoughts/suggestions on where I might be going wrong?

Edited August 8, 2018 by logan2z

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[Tmx]

I think the chronological order in your process is not correct. The ilford aid wash bath (which I don’t use) should be the last station of the process and not the starting point. This may cause the issues

[logan2z]

I think the chronological order in your process is not correct. The ilford aid wash bath (which I don’t use) should be the last station of the process and not the starting point. This may cause the issues

Sorry if I wasn't clear, the wash aid portion of my workflow is immediately following the fix stage and immediately followed by the wash. I believe this is the correct sequence.

[Tmx]

I don’t think so. I mean the correct way is: fixing, regular washing and the wash aid as the second and the final wash as the last step

 

Edit: I wouldn’t go with the fixed print directly to wash aid

Edited August 8, 2018 by Tmx

[Lukas F.]

Tmx is apparently right, check out the Ilford Washaid's data sheet.

 

Is the water warm enough (20°C or higher)? Washing with colder water isn't as efficient.

[otto.f]

Are you sure that fixing in 1+9 for 2’ is enough? My experience with Ilford’s fixers is that they don’t seem very strong either, I prefer Moersch at the moment.

Edited August 8, 2018 by otto.f

[logan2z]

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Are you sure that fixing in 1+9 for 2’ is enough? My experience with Ilford’s fixers is that they don’t seem very strong either, I prefer Moersch at the moment.

According to their data sheet it is:

 

Material Dilution Time (minutes)

General purpose film 1+4 2–5

RC paper 1+4 1/2

RC paper 1+9 1

FB paper 1+4 1

FB paper 1+9 2

[otto.f]

I know, I was referring to my experiences

[logan2z]

Tmx is apparently right, check out the Ilford Washaid's data sheet.Is the water warm enough (20°C or higher)? Washing with colder water isn't as efficient.

That's right, the data sheet says a 5 minute wash, followed by 10 mins in the wash aid followed by a final wash. It also points out another option of a single 60 min wash and no wash aid. I tried that before using the wash aid and had the same result. I can try splitting the wash as the data sheet and tmx suggested and see if that works any better. FWIW, I soak the prints in a static fresh water bath until my printing session is over, so technically I'm not going straight from the fix to the wash aid (although it's not a wash).

[logan2z]

I know, I was referring to my experiences

So you've experienced issues due to insufficient fixing when following Ilford's guidance?

[otto.f]

Yes, the last time more with film because I don’t use Ilford chemicals for paper, but I had to re-fix films that had been done in Ilford fix. The only thing I’m wondering about is that the stain is so local, wasn’t there some knob that touched the paper during processing?

Edited August 8, 2018 by otto.f

[logan2z]

Yes, the last time more with film because I don’t use Ilford chemicals for paper, but I had to re-fix films that had been done in Ilford fix. The only thing I’m wondering about is that the stain is so local, wasn’t there some knob that touched the paper during processing?

The stain is local because I used a residual hypo test that calls for a drop of the test solution to be placed on a white portion of the print (after the print surface has been wiped dry), left for 2 minutes and then blotted off. The stain is where the drop was placed.

[logan2z]

Tmx is apparently right, check out the Ilford Washaid's data sheet.

 

Is the water warm enough (20°C or higher)? Washing with colder water isn't as efficient.

The water temp is about 74 degrees Fahrenheit.

[adan]

Some thoughts:

 

"Hypo" or fixer is heavier than water. It will tend to collect in the bottom of a holding or washing tank or tray. Thus those should drain from the bottom, so that the weight of water above "pushes" any accumulated fixer out the drain first. Fixer just really loves to stick to paper fibers and gelatin like glue, so keep that in mind in reading the following.

 

The Versalab has a weird syphon design, where the outflow tube leads from the bottom up to the top, for drainage overboard. You might want to doublecheck that that is correctly installed and functioning, and not perhaps leaking some "used" wash water back into the tank. Additionally, try testing a print on both the top and bottom edges as it stood in the washer, just to see if the bottom is retaining more fixer.

 

The Wash Aid procedure, as for most such hypo-clearing aids, is correct as published: a relative brief rinse (1-2 minutes) to remove "standing" fixer on the paper, then a 10-minute soak in the Wash-Aid to "unlock" the fixer molecules from the paper fibers and gelatin, and then a 20-minute wash to wash away all of the "loosened" fixer.

 

Make sure the water flow through the washing tank is adequate - at least 3-4 complete changes in water during the washing time. That can be tested (with no prints installed!!) by adding a drop of food coloring to the tank as it operates, and making sure the food dye disappears completely within 4-5 minutes or so.

 

With regard to a holding tray, I would make sure that is getting a lot of water replenishment, not "static." If not running water all the time, at least an emptying and refilling with fresh water every time a new print is added. "Static" holding is OK for relatively impermeable RC paper (and even then, with a lot of water - I used a bathtub), but with fiber paper, you really want to make sure that you're not upping the fixer proportion in the holding tray via "carry-over" from each newly-fixed print added to the stack. Again, fixer's "weight" will mean the bottom-most sheet in the holding tray will get the highest dose of waste fixer, if it is allowed to collect.

 

The longer fiber paper lies in fixer (no matter how diluted) the stronger the bond between any fixer molecules and the paper becomes. Once a print's fixing is done, get it away from any possible additional fixer contact.

 

Finally, I note that the Photographer's Formulary sells similar packets of both residual hypo test, and residual silver test. You might just check that you were shipped the right stuff. The silver test is to check that fixing was complete, the hypo test is to make sure the washing was complete. Your sample "stain" does look more like the correct residual hypo test result - but check every variable.

[logan2z]

Some thoughts:

 

"Hypo" or fixer is heavier than water. It will tend to collect in the bottom of a holding or washing tank or tray. Thus those should drain from the bottom, so that the weight of water above "pushes" any accumulated fixer out the drain first. Fixer just really loves to stick to paper fibers and gelatin like glue, so keep that in mind in reading the following.

 

The Versalab has a weird syphon design, where the outflow tube leads from the bottom up to the top, for drainage overboard. You might want to doublecheck that that is correctly installed and functioning, and not perhaps leaking some "used" wash water back into the tank. Additionally, try testing a print on both the top and bottom edges as it stood in the washer, just to see if the bottom is retaining more fixer.

 

The Wash Aid procedure, as for most such hypo-clearing aids, is correct as published: a relative brief rinse (1-2 minutes) to remove "standing" fixer on the paper, then a 10-minute soak in the Wash-Aid to "unlock" the fixer molecules from the paper fibers and gelatin, and then a 20-minute wash to wash away all of the "loosened" fixer.

 

Make sure the water flow through the washing tank is adequate - at least 3-4 complete changes in water during the washing time. That can be tested (with no prints installed!!) by adding a drop of food coloring to the tank as it operates, and making sure the food dye disappears completely within 4-5 minutes or so.

 

With regard to a holding tray, I would make sure that is getting a lot of water replenishment, not "static." If not running water all the time, at least an emptying and refilling with fresh water every time a new print is added. "Static" holding is OK for relatively impermeable RC paper (and even then, with a lot of water - I used a bathtub), but with fiber paper, you really want to make sure that you're not upping the fixer proportion in the holding tray via "carry-over" from each newly-fixed print added to the stack. Again, fixer's "weight" will mean the bottom-most sheet in the holding tray will get the highest dose of waste fixer, if it is allowed to collect.

 

The longer fiber paper lies in fixer (no matter how diluted) the stronger the bond between any fixer molecules and the paper becomes. Once a print's fixing is done, get it away from any possible additional fixer contact.

 

Finally, I note that the Photographer's Formulary sells similar packets of both residual hypo test, and residual silver test. You might just check that you were shipped the right stuff. The silver test is to check that fixing was complete, the hypo test is to make sure the washing was complete. Your sample "stain" does look more like the correct residual hypo test result - but check every variable.

 

Thanks so much for taking the time to reply.  I hadn't really thought enough about the fact that I was contaminating the holding tray every time I inserted a print in there from the fixer.  I will definitely keep this in mind going forward. 

 

The last couple of prints I made I followed a slightly different methodology.  I put the print in a fresh water bath so that I could examine it without it being covered in fixer, then put it immediately into the print washer that was filled with fresh water.  I washed the print for 5 minutes, then put it immediately into the wash aid for 10 minutes.  I then put it back into the print washer (refilled with fresh water) for 20 minutes.  This exactly follows the Ilford instructions.  The result of testing these prints with the hypo test was better than before, but still showed a bit of a stain - but much lighter than my earlier prints.  I upped the final wash time to 30 minutes but that didn't seem to make much of a difference.  So a definite improvement but I still don't get zero stain as some people claim to be getting.

 

>> Finally, I note that the Photographer's Formulary sells similar packets of both residual hypo test, and residual silver test. You might just check that you were shipped the right stuff. The silver test is to check >> that fixing was complete, the hypo test is to make sure the washing was complete.

 

Yes, I'm definitely using the hypo test.  

 

>> Your sample "stain" does look more like the correct residual hypo test result - but check every variable. 

 

When you say 'correct' stain, do you mean 'acceptable stain' or do you just mean that it indicates that the hypo test, rather than the silver test is being used?  I assume you mean the latter as that stain looks too dark to me.

[otto.f]

Try Kodak Hypo Clearing Agent and see what happens, isn’t that expensive

Edited August 20, 2018 by otto.f

[adan]

Yep, your assumption is correct. You very probably have the correct testing chemical.

 

What is the character of your washing water? Hard water? Softened water? Naturally soft water? City water? Rural well water? That might affect how rapidly your wash aid and water can remove fixer. The whole fixing/fixer-removal cycle is all about mineral content.

 

The background on washing aids in general is that they were discovered during WW 2. US Navy photographers on board ship washed their prints and film in sea water to save on precious fresh water supplies, and discovered that "salt water" removed fixer faster than fresh water.

 

A little research revealed that the mineral "salts" in sea water were doing the job described in my previous post - they could nudge aside the sodium or ammonium thiosulfate (fixer) molecules clinging to the paper (and to a lesser extent, the gelatin), with more soluble metal-sulfite molecules, which then themselves washed away more easily.

 

More technically accurate, there is an ion-exchange reaction that, more less, turns an attached fixer thiosulfate molecule in the paper into an easily-dissolved sulfite molecule (while turning an already-dissolved sulfite molecule in the wash aid water into a thiosulfate molecule). Kinda like breaking a prisoner out of jail by giving him your ID, and then getting it back once you are both outside the jail. But you can see where the mineral quality, or the presence of other ions from water-softening (also an ion-exchange reaction), may affect the magic trick.

 

Commercial wash aids are thus "artificial sea water" salted specifically with ammonium or sodium sulfite (sometimes with traces of other chemicals - bisulfites, metabisulifites, for pH control).

 

I've always like Heico PermaWash because of its "clean, Windex-y™" dilute ammonium scent. But they all work about the same.

______________________

 

Geek stuff: Sulfates are one sulphur atom holding on to 4 oxygen atoms - SO₄. If they stay in the photo paper/film, they can eventually combine with hydrogen from environmental water vapor (H₂O) to form H₂SO₄ (sulphuric acid) which will start to dissolve the precious silver image, and yellow and harden the paper itself (like old crumbly newsprint). Usually turning the silver brown first. The hypo test chemical also turns gray-brown in the presence of residual sulphates.

 

Thiosulfates are sulfate with an extra sulphur atom replacing one of the oxygens - S₂O₃ - even more likely to turn into sulphuric acid over time.

 

Sulfites are SO₃ - one sulphur atom holding on to 3 oxygens (one via a double bond), or using the extra bond to link up with an ammonium ion (NH₄) or sodium (Na) or other ions. They dissolve or ionize in water faster than thiosulphates.

[logan2z]

What is the character of your washing water? Hard water? Softened water? Naturally soft water? City water? Rural well water? That might affect how rapidly your wash aid and water can remove fixer. The whole fixing/fixer-removal cycle is all about mineral content.

 

 

We're on town/city water and it's relatively hard.  

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