Amidol/Propylene Glycol stock solution tests

Discussion in 'B&W: Film, Paper, Chemistry' started by Tom Hoskinson, Jul 13, 2004.

  1. Tom Hoskinson

    Tom Hoskinson Member

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    On June 22, I tried dissolving 8 grams of Amidol in 150ml of Propylene Glycol (PG). I put 150ml of PG in a 300ml Pyrex beaker dropped in a stirring magnet (Teflon coated) and poured in 8 grams of Amidol. Some of the Amidol slowly went into solution at room temperature (dark blue solution color). I increased the temperature with continuous magnetic stirring (under a vented chemical hood). Most of the Amidol dissolved by the time the solution reached 170 deg. F. I continued heating and stirring until the solution reached 270 deg. F. I could see that there was still some undissolved residue at that temperature. I slowly cooled the solution and decanted it into a bottle. There was about a gram (estimated) of undissolved material left in the beaker. I added 30ml of methanol to this residue, stirred and it dissolved (violet color). I added this to the PG mix (now a indigo color) and saw no color change. I have been watching this solution for changes (color, activity, etc).

    It has now been 22 days since I mixed the solution of Amidol (8 grams) in a mixture of 150ml propylene glycol and 30ml methanol.

    The color of the concentrated Amidol/PG mixture remains an indigo blue (unchanged from the time I mixed it).

    Today (7/13) I mixed a small amount (about 80ml) of a dilute Amidol working developer solution. I used about 2 - 3ml of the concentrated Amidol stock solution. The rest of the working solution followed Michael Smith's Azo formulation.

    I used the leader off an old (1989 Expry) roll of 35mm Tech Pan. I cut the leader into 2 pieces, fixed one piece and dropped the other piece into the beaker containing the dilute Amidol solution. The film piece turned black in about a minute. I left it in the Amidol for another minute, then washed it, fixed it in TF-4 (probably a mistake), washed and dried it with its fixed-only companion piece.

    The developed piece is obviously stained, the stain color is green/black. The stain is not uniform and I suspect the TF-4 fixer may have removed some.

    Color transmission densitometry of the developed piece shows:
    Visual Channel Density = 1.17
    Blue Channel Density = 1.46

    The fixed-only piece shows:
    Visual Channel Density = 0.13
    Blue Channel Density = 0.10

    I covered the beaker and will check the developer activity again after 8-10 more hours.
     
  2. Francesco

    Francesco Member

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    Thanks for that Tom. Can you explain what your procedures are going to achieve and what you are hoping to find or not as a result? Are you simply testing for whether or not the developer is still as active as when first mixed? Will you be trying this out on some "scenic" negatives as well? Many thanks for sharing your research with all of us.
     
  3. Tom Hoskinson

    Tom Hoskinson Member

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    Yes Francesco,
    I am preparing to do Azo/Amidol printing of some of my 8x10 negs next Saturday and I wanted to run a developer activity "proof test" on my Amidol/PG stock solution before then. There are a lot of stories about how Amidol solutions can "go bad" without changing color.

    I also have 8 new sheets of Efke 100 to process (probably Thurs. night). All are landscapes/nature subjects and some were multi-second exposures made with my Polarfleece Sock/Shutter.
     
  4. Donald Miller

    Donald Miller Member

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    Tom,
    Thanks for the update. The question that I have is why use film to check amidol activity?, or is this simply because the film is much more susceptible to determination of Amidol activity?, or... are you wanting to arrive at a new film developer based on Amidol? Thanks again for your continued service...
     
  5. Tom Hoskinson

    Tom Hoskinson Member

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    Hi Don, I used film as an activity/no-activity test article because it was convenient - it's what was immediately available in the lab I was using.

    My Amidol interest at this point is in the development of Azo contact prints - not film.

    My observation (today) that the developer produced substantial visible stain on the piece of test film led me to check it out with the densitometer.
     
  6. bmac

    bmac Member

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    <smartass> Darn, I was looking forward to developing my film in Amidol and souping my prints in Don's Pyro. Much easier than doing my film in pyro and my prints in Amidol... </smartass>
     
  7. Tom Hoskinson

    Tom Hoskinson Member

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    Hey Brian!
    What started this exercise off was my desire to perform comparative tests between Amidol, Don's PPPD, Ansco 130 and Phenidone/Ascorbic (Gainer's PC-TEA)on Azo contact prints.

    The Amidol/PG stock solution is because I want to minimize my handling of dry Amidol.

    I need to run a second set of test prints through Don's PPPD (I fouled up the first set) and run an additional set through Michael Smiths's Amidol for comparison.

    Lord only knows where all this will lead... :tongue:
     
  8. gainer

    gainer Subscriber

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    Interesting. Did you notice tanning as well as staining? I think amidol is listed among the moderately tanning agents. I'm don't know what other ingredients you added, but would assume sulfite to be among them.
    Color is sometimes dependent on grain thorugh diffraction as well as staining. Could that be a factor?
     
  9. Tom Hoskinson

    Tom Hoskinson Member

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    Hi Pat,
    The basic formulation is Michael Smith's Azo contact paper developer formulation, so: 30 grams/liter sodium sulfite, 3 grams/liter citric acid, 2ml 10% KBr/liter. The Azo recipe calls for 8 grams/liter Amidol. I just poured in a small dollop (maybe 3 ml) of my ~ 4% Amidol/PG stock solution. The rest of the chemistry is faithful to the proportions in Michael Smith's formulation.

    Since the test pieces of film are uniformly exposed to diffused light (thus no coherent image) it is difficult to judge if tanning or proportional staining is taking place. There is definitely blackened silver plus a dark olive green stain. I'll take a look with a microscope and see what else I can see.

    BTW I developed a second test piece of film this evening when the solution was 8 hours old and saw no difference in activity. I fixed this piece in home brew Kodak F - 24 non-hardening fixer. The stain was very uniform this time.

    I am tempted to try a roll of Efke 100 with real images. That should make it much easier to determine if tanning and/or proportional staining is happening.

    Hey! Did I just step out onto a slippery slope?
     
  10. juan

    juan Subscriber

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  11. lee

    lee Member

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    I may be speaking out of another orphis than my mouth, I seem to remember that Amidol as a film developer really dumped shadow detail. Is this true?

    lee\c
     
  12. gainer

    gainer Subscriber

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    No, you just looked outside the box. There are all kinds of marvelous things out there.

    It ocurred to me, and probably to you, that it would be a convenience to be able to keep amidol in a glycol solution and the rest in water, mixing just enough at a time to do a sheet of film or paper in a tube.

    The amount of sulfite may give some control over the color. You may not need the citric acid. Anyway, you have enough variables to keep you busy for a while.
     
  13. gainer

    gainer Subscriber

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    I meant to address that last post to Tom, who wondered if he had stepped on a slippery slope.
     
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  15. Tom Hoskinson

    Tom Hoskinson Member

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    Yes Pat, I have the Amidol as a PG stock concentrate and everything else as a water based stock concentrate.

    I'm a little surprised that I am seeing stain with 30 grams/liter of sulfite.

    I have been thinking about trying a TEA option for the "B" bath. Any advice?
     
  16. Jorge Oliveira

    Jorge Oliveira Member

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    Anyone for amidol + phenidone?

    Jorge O
     
  17. Tom Hoskinson

    Tom Hoskinson Member

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  18. garryl

    garryl Member

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  19. Tom Hoskinson

    Tom Hoskinson Member

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    Easy enough to try - so why not?

    Another possibility is amidol + ascorbic acid and maybe some TEA to get the pH back into the neutral to slightly alkaline range??
     
  20. gainer

    gainer Subscriber

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    I haven't played much with amidol. It is potent enough to be used in acidic solutions. You might or might not gain by adding TEA, but first I would start from nothing but some sulfite. I think the citric acid is mostly for preservation, but it naturally reduces pH somewhat. Rather than leave it in and add TEA or other alkali, I would go with the simplest solution for starters and see what has to be added to make it better. In philosophy there is the principle of Occam's (sp?) razor that says the simplest theory that works is the best. Shave it down and let it grow if necessary.
     
  21. Tom Hoskinson

    Tom Hoskinson Member

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    Ah yes! William of Occam. I have recommend the use of his razor to a lot of people over the years. Most stare blankly at me and say - What?

    It's probably because I have a beard... Started growing it in 1969 - it was black then (white now).

    My understanding is that addition of a bit of citric acid to the working developer was the empirical result of a lot of experimentation by Michael Smith - confirmed by others.

    Amidol is known to work well as a developer in a slightly acid pH environment.

    There is an indication that Pat Dignan favored Ascorbic acid over Citric with amidol. I haven't been able to verify this yet and I have most of the Dignan notes.
     
  22. gainer

    gainer Subscriber

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    I just recently shaved off my white beard. Made me look 10 years younger... than dirt, that is.
     
  23. Jorge Oliveira

    Jorge Oliveira Member

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    That's why i haven't shaved mine - I can't find Occam's razors for sale anywhere! :smile:

    Jorge O
     
  24. gainer

    gainer Subscriber

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    I forgot to say that ascorbic acid and amidol are almost certainly synergistic. If so, the ascorbic acid will reduce the pH and INCREASE activity. What it does to image tone, etc, I won't try to guess. I have a feeling, though, that you would not be any better off than with ascorbic acid and metol, p-aminophenol or phenidone but would be spending more money.
     
  25. Tom Hoskinson

    Tom Hoskinson Member

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    Thanks, Pat - that's also my feeling.

    Jorge - sounds like there's a potential eBay market for Occam's Razors!
     
  26. garryl

    garryl Member

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    >Jorge - sounds like there's a potential eBay market for Occam's Razors!<

    What do you all use to sharpen those with- a Mobius strap?