Problem with R09

Discussion in 'B&W: Film, Paper, Chemistry' started by wclavey, Sep 3, 2007.

  1. wclavey

    wclavey Member

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    There is probably an "I told you so..." somewhere in all this, so I am bracing myself.

    I have been using R09 to develop my Arista.EDU 100 ASA 120 film for the past few months now with no problems. I just finished my first bottle that I purchased from Freestyle and I usually develop 2 rolls at a time. I finished shooting a roll this morning and just attempted to develop this roll plus another I shot last week.

    When I took out the bottle of R09 concentrate, a dark precipitate had formed in the bottom of the bottle. I had noticed this preciptate forming the last time I used it. I looked up the threads here on APUG that talked making a Rodinal-like developer and they all commented that a precipitate would form when you mixed it and that all the precipitate would not disolve. I figured that as the R09 concentrate bottle got emptier and, this being TX where our normal inside temperature is above 80, the vapor pressure change was causing some preciptate to form. I mixed and developed as usual and there were no problems. Negatives looked great.

    So this time, the amount of precipitate was greater, I warmed the bottle in running water, shook it vigorously, and most but not all of the precipitate disolved back into solution. I mixed the developer and proceeded to develop.

    Both rolls came out absolutely blank - - completely... not a shadow or hint of anything on the film... as if I had developed 2 completely unexposed rolls (which I have done by mistake in my almost 50 years of doing this) ...so completely blank that I checked the camera and back to make sure it is working (...it is).

    So this being the first bottle of R09, my questions are something like: Obviously, whatever preciptated out was an active ingredient that was not the same once I warmed it and shook it back into solution. What should I have done? Toss the bottle and opened a new one? Any thoughts?

    Thanks.
     
  2. Tom Hoskinson

    Tom Hoskinson Member

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    I would toss the bottle out and open a new one. Sounds to me like your warming and shaking procedure may have oxidized the p-aminophenol.
     
  3. gainer

    gainer Subscriber

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    The precipitate in Rodinal, if it is there, is white. Rodinal changes color after exposure to air, the color being red-brown. I have seen it work as new when you could not see light through the stock solution. Tom is probably right. Next time, run a piece of exposed film leader through the working solution before attempting to develop a roll. The film should turn black in 2 minutes.
     
  4. bluenote

    bluenote Member

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    Hi, I am having the exact same problem with R09 .

    Last two rolls of film I've finnished went totally blank after processing in R09.
    The bottle was opened and half empty for some time.. 3 months maybe more...
    Both rolls from different cameras. Now, I am confused and my next rolls are going to be developed in photolab.


    Jiri, Czech rep.


     
  5. AgX

    AgX Member

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    The manufacturer states that the white precipitate could/should be filtrated.
     
  6. wclavey

    wclavey Member

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    Jiri, mine had been open and a little more than half gone for about 3 months, as well (...I have been shooting more 400 speed which I develop in Microdol-X). I think I may convert my original post to an email and send it to the manufacturer to see if they have any ideas. As it is, though, I have thrown away the final concentrate and will open a new bottle next time.
     
  7. rtuttle

    rtuttle Member

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    I don't know I have never heard of a developer so bad it didn't give any results. Maybe it was the film. I don't believe warming a concentrate and shaking precipitate back into a liquid would make that happen.
     
  8. bluenote

    bluenote Member

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    Yes, after the first roll came out blank I thought this is a problem of a film (Ilford FP4+) , but the second one, Ilford HP5 cleared this out. Blank as well.
    I keep my rolls in a fridge, for sure they were in good condition.




     
  9. Fotohuis

    Fotohuis Member

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    R09 (Calbe) and I think Fomadon R09 (also) can fail after some period of use.
    They have not an equivalent storage time than the Rodinal from Agfa/A&O.

    We started some aging test 4 years ago for Rodinal.
    Recently we compared Fomadon R09 and Rodinal:
    http://www.flickr.com/groups/rodinal/discuss/72157601393747142/
     
  10. wclavey

    wclavey Member

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    I see in the link to your test that your R09 was 1.5 years old at the beginning of the test. Did any very dark brown precipitate accumulate in the bottom of the bottle during that time? I looked at it closely and it was very hard and formed into the bottom corners of the bottle and came out only with difficulty.
     
  11. Fotohuis

    Fotohuis Member

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  12. wclavey

    wclavey Member

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    I am using the Fomadon R09, as well.
     
  13. Fotohuis

    Fotohuis Member

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    OK. The bottle must have a batchnr. and exp. date (use before). Further the storage of this developer must be between 10-25 degrees C. Maybe this last item will be a problem in Texas.

    The sales of R09 in the Netherlands was never an issue because the "equivalent" Rodinal was/is easy available. R09 should survive around two years while the lifetime of Rodinal is much much longer.

    Further Rodinal is packed in silar plastic bottles and R09 in PE-HD (Polyethyleen high density) written on the bottom of the bottle. But a lot of things are depending on how full/empty is the bottle when you're stocking it over a longer time.
     
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  15. Rolleijoe

    Rolleijoe Member

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    Yep, since you're ordering from Freestyle anyway, why not get real Rodinal? I'm only about 100mi East of you, and my Rodinal is still going strong. The bottle of R09 I purchased over a year ago has never been opened, and my darkroom stays @ 68F year round (AC). But I would have tossed that bottle & opened a new one, especially if the images were not reproducable.
     
  16. Soeren

    Soeren Member

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    IIRC some crystals are meant to be there. I read this somewhere but it'll take some time to dig it up again.
    Kind regards
    Søren
     
  17. AgX

    AgX Member

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    Søren,

    See post 5.
     
  18. Soeren

    Soeren Member

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    Yes but the OP talks about a dark precipitate and thats what I believe should be precent in the bottle. Again my memory could trick me and Im rather busy at the moment so finding the info will have to wait.
    Kind regards
    Søren
     
  19. AgX

    AgX Member

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    The manufacturer of Calbe R09 (maybe of the Foma R09 too) refers to a white precipitate, from what I conclude that a dark precipitate is not to be expected within working condition.

    Maybe the OP tells us what the industry replied to him.
     
  20. wclavey

    wclavey Member

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    I must apologize, but I have been traveling for work and have not had the chance to send a request for information to the manufacturer. I threw out the old bottle and opened a new one. I will see if the situation repeats itself. It is the Foma R09.

    It was absolutely a dark, almost black, precipitate, and it formed into a very hard block that assumed the shape of the corners of the bottle. It was very hard to break up, even with the back of a spoon. I put some chunks of it on a paper towel, and dropped hot water on it. A brown, coffee-colored liquid (which looks like the R09 itself) came off and was absorbed into the paper towel.
     
  21. AgX

    AgX Member

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    I guess, just a guess, that precipitate is just the white stuff Calbe hints at, which in your case had been coloured/covered with oxidized developing agent while the concentrate had deterioted beyond its limits.
     
  22. k_jupiter

    k_jupiter Member

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    Were there any frame numbers on the side of the film? Are you sure you didn't fix before develop (don't ask)?

    Seems like perhaps there is a three month open shelf life or so on this developer, next time perhaps use.... Rodinal.

    tim in san jose
     
  23. Xmas

    Xmas Member

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    The concentrate of a Rodinal clone should last for ever in a quarter full bottle if you replace the closure and it is airtight. If you remove the residue it wont last. If you mix your own you have to ensure you get a residue.

    For ever >25 years, it will be like black coffee, after 25 years.

    Noel
     
  24. AgX

    AgX Member

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    Correction !


    That reference of Calbe Chemie to a white precipitate, which is of no chemical harm but should be filtrated (which is only to be found in the german language version) is linked to a working solution and not to the concentrate!


    Sorry, that I mixed things up.


    But how many precipitates exist in R09?? Are there good and bad ones??
     
  25. poutnik

    poutnik Member

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    bluenote (my brother-in-law) had no frame numbers on the side of the film. When he asked me about this problem, the first thing I suggested was the same as you ask here. He was swearing that he mixed fresh working solutions of both, checked the solutions and did use them in the correct order. The next day he developed another roll (different film type this time) and the same problem. And he was paying hell of attention to not mix up the order of the chemicals used.

    But since then we think we have tracked the problem down (also speaking to photo-store clerk that still deals in classic film stuff - and knows something [a lot of thinks] about her stuff, too :smile: ):
    The problem is most likely oxidation of long opened bottle of R09, that is greatly sped up by light. In case of storage in light place and half full bottle, it can go to shit in mere months. In case of storage in dark place and half full bottle, half a year should not be that much of a problem. It is also important to squeeze the bottle of concentrate to let out as much air as possible before longer storage.

    Since this disaster of my in-law I started doing this as a precaution to damaging my films: prior to any development I use a strip of cut sheet film to test the mixed developer solution - dip the strip in the dev for one or two minutes (in full light) - it should turn black, then throw it away. If it does not turn black, something is wrong...
     
  26. Soeren

    Soeren Member

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    Correction II :smile:

    I had time to look into the film development cookbook last night.
    It states that "A FEW CRYSTALS" should be present in the bottle. So only a few crystals and not a precipitate. On the other hand, when mixing the developer from scratch there will form a dark precipitate at some point in the end of the procedure. This precipitate would desolve when adding the last amount of water to the solution. Could it be the evaporation of water due to the heat in Texas that caused the forming of the precipitate, which BTW is the (para-aminophenol?sp)?
    Kind regards
    Søren