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  1. #1
    hmzimelka's Avatar
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    Making some Parodinal, but would appreciate more insight...

    Dear all,

    This would be my first post, but I've been hovering around here for about 2 years.

    I've tried my best to read up as much as I could before posting, and I have gotten quite far in creating my home brew Parodinal developer. I now need to fine tune the recipe, but my non existent knowledge of chemistry combined with all the internet posts out there (at least the ones I've found and/or understood) are failing me to get what I want...

    What I have stocked:
    - Sodium Sulphite (anhydrous)
    - Sodium Carbonate (anhydrous)
    - Sodium Ascorbate
    - Ascorbic Acid
    - Paracetamol Powder (Ph Eur 7.0) - I bought this from a pharmaceutical manufacturer.
    - Distilled water (I have a small distiller)
    - Sodium Hydroxide. (small clean white flakes form the hardware store)

    I own have a jeweller's scale measuring in 0,1gr increments, with a max of 500gr.
    I also have a digital thermometer with a 15cm thin metal probe.

    On Saturday (Aug 25th) I made my first two batches follwing ZorkiKat's method;

    Parodinal Batch 25082012-01:
    1) Sodium Sulphite (50gr) was added into 125ml of water and dissolved as best as possible. Much of it didn't.
    2) Sodium Hydroxide (20gr) was mixed into a separate amount of water (100ml). This, once dissolved, reached a temperature of approx 49ºC.
    3) Paracetamol powder (15gr) was added to Hydroxide mixture, which quickly dissolved and took on a clear pale pink colour. This solution was stirred and cooled in a cool water bath.
    4) While cooling solution in Step 3. the solution suddenly became cloudy and viscous at +/- 23ºC, at which the temperature rose by +/- 0,4ºC.
    5) At this point, the saturated sulphite solution (with all precipitation) was added to the thick and cloudy Hydroxide+Paracetamol mix. The end result soon became clear and took on a light amber colour. The liquid fas filled to 250ml mark with distilled water, and bottled. (Bottle was a cleaned 500ml R09 Rodinal bottle)

    Parodinal Batch 25082012-02:
    This batch was made in the similar way as 01, but...
    1) 50gr of Sodium Sulphite was added to 150ml of water, mixed well, and 125ml was decanted and put aside (no sediment).
    2) Sodium Hydroxide (20gr) was mixed into a separate amount of water (100ml). This, once dissolved, reached a temperature of approx 49ºC.
    3) Paracetamol powder (15gr) was added to Hydroxide mixture, which quickly dissolved and took on a clear pale pink colour. This solution was stirred and cooled in a cool water bath.
    4) The 125ml of saturated Sulphite solution was poured into the Hydroxide+Paracetamol while still hot, and stirred. The solution, which was clear in colour, was filled to 250ml mark with distilled water, and bottled. (Bottle was a 200ml amber glass bottle, filled to the brim and the difference was disposed of)

    On Monday (Aug 27th) I made two more batches.
    Parodinal Batch 27082012-01:
    Same Procedure as Parodinal Batch 25082012-01:, except I used half the Sodium Sulphite this time.
    Solution was clear and amber in colour.
    (Bottle was a 200ml clear glass bottle, filled to the brim and the difference was disposed of)


    Parodinal Batch 27082012-02:
    1) 50gr of Sodium Sulphite was added to 150ml of water, mixed well, and 125ml of this was decanted.
    2) The Paracetamol was mixed into the Sulphite solution, which didn't dissolve very well.
    3) Sodium Hydroxide (20gr) was mixed into a separate amount of water (100ml). This, once dissolved, reached a temperature of approx 49ºC.
    4) The Sodium Hydroxide solution was added to the Paracetamol+Sulphite mix, which dissolved fairly quickly into a clear and colourless solution.
    5) The level was filled with distilled water up to 250ml, and bottled.
    (Bottle was a 200ml clear glass bottle, filled to the brim and the difference was disposed of)

    Here is a pic of the two solutions from Monday:



    Now, the observations on Monday Aug 27th:
    Parodinal Batch 25082012-01: Dark red probably due oxidation in bottle. Solution had longish crystals amongst the sulphite sediment.
    Parodinal Batch 25082012-02: Colour not determined, but it certainly didn't seem darker than on Saturday. Many long crystals had formed at the base, and solution was clear. (Sunday evening showed no signs of any crystals!)

    On Monday afternoon, I was annoyed by seeing so many crystals in Parodinal Batch 25082012-02:, so I emptied the bottle into a small measuring jug, and slowly added up to a total of 7gr NaOH, which slowly dissolved the crystals, but a new sediment formed soon after which resembled that of a saturated sulphite solution. The solution was put back into the amber bottle. Please don't ask me why I added the extra NaOH I though it was a good idea at the time. I have probably ruined a good thing here...

    The observations on Tuesday morning Aug 28th:
    Parodinal Batch 25082012-01: Crystals seem unchanged, but solution seemed a little darker
    Parodinal Batch 25082012-02: The base of the bottle was now full of long crystals again. Solution colour unchanged and still clear.


    Parodinal Batch 27082012-01: No crystals yet. Solution is a clear amber colour with very feint and very little sediment.
    Parodinal Batch 27082012-02: No crystals yet. Solution is a clear, slightly yellow in colour, with very feint and very little sediment, but a little more than Parodinal Batch 27082012-01:


    OK, So, thanks to all that have made it this far...

    To those who know more than I do about chemistry, and also to those with greater experience in making this home-brew, is there anything I have been doing wrong or something you recommend me to change? My greatest concern is the amount of crystal volume in Parodinal Batch 25082012-02:. Are these amount of crystals that normal? Is there any ingredient I should/could increase/decrease to minimise this crystal growth to minimum? - I realise these crystals play a role, and that they are good to have, but not so many right?

    I realise that my asking help may come a little early and that I may seem impatient... forgive me

    I will report back when Monday's batches have developed crystals, which is something I'm expecting to see by tomorrow morning.

    Thank you for your time and any help would be greatly appreciated!

    Martin
    Last edited by hmzimelka; 08-28-2012 at 11:22 AM. Click to view previous post history.

  2. #2
    hmzimelka's Avatar
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    Today, given the good weather, exposed 3 rolls of 35mm film on a test scene. Images were bracketed 1-stop both ways. Film was EFKE 50, with intentions to develop the film for 6min in 1:25 dilutions.

    Today, I cut two strips from a test film, and developed one in commercial R09 Rodinal (From MACO Germany). The other was developed in Parodinal Batch 25082012-01:.
    The negs are drying as I type, but look almost identical. Scanned results will come later after negs have dried. Any difference will be noticeable in the scan.

  3. #3
    Steve Smith's Avatar
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    Don't worry about the oxidisation. All Rodinal including clones and DIY types quickly get to this colour.


    Steve.
    "People who say things won't work are a dime a dozen. People who figure out how to make things work are worth a fortune" - Dave Rat.

  4. #4
    hmzimelka's Avatar
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    Steve,

    Thank you. It's not so much the colour I'm worried about, but rather the amount of crystals that form after day 2 of a bottled batch. They seem excessive.
    I'll be developing the films with every batch hopefully, so at least I'll have visual representation of what I did...

  5. #5
    Steve Smith's Avatar
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    I think there are reports of deposits in most types of Rodinal too.

    What do refer to as excessive? Can you post a picture of a bottle with crystal deposits in?


    Steve.
    "People who say things won't work are a dime a dozen. People who figure out how to make things work are worth a fortune" - Dave Rat.

  6. #6
    hmzimelka's Avatar
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    It's the last image in my initial post, but here it is again.
    hard to see, but they occupy a large volume of the bottle

  7. #7

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    http://photo.net/black-and-white-pho...g-forum/00UxmB
    Efforts to improve PaRodinal included reducing suspended solids and also crystals.
    IMO they are not entirely successful,the clear form in the link deposits crystals eventually,they may be sodium aminophenolate.
    So well done for your work but I don't think you will get a crystal free solution.
    Making it clear does not IMO affect the developing properties but it looks better.

  8. #8
    hmzimelka's Avatar
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    Quote Originally Posted by Alan Johnson View Post
    http://photo.net/black-and-white-pho...g-forum/00UxmB
    Efforts to improve PaRodinal included reducing suspended solids and also crystals.
    IMO they are not entirely successful,the clear form in the link deposits crystals eventually,they may be sodium aminophenolate.
    So well done for your work but I don't think you will get a crystal free solution.
    Making it clear does not IMO affect the developing properties but it looks better.
    Indeed, it does look better.
    The first batch already developed some negs, so it does work... :

  9. #9
    hmzimelka's Avatar
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    Right, it's Wednesday morning here, and still no crystals in both Monday's batches. Hmmm
    Parodinal Batch 27082012-2 has become a little more yellow since yesterday.

    Here is a comparison image of commercial Rodinal R09 One-Shot (Purchased from MACO) and Parodinal Batch 27082012-2. (Link to the full res version is HERE)


    Interestingly enough, the Parodinal developer created ever so slightly denser negatives, which is something I only noticed after scanning.

    The negs were scanned on my Imacon 343. The film was EFKE 50, shot with Nikon F5 and 50/1.8D, exposed at 1/400sec f/5.6 as per incident meter reading, and developed in dilution 1:25 for 6min at 20ºC.
    Apologies for the dark negs, I don't work with this film very often, so film speed rating developing times are taken using recommendation by massive dev.

    Please note, these images come straight out the scanner, with only cropping applied. Sharpening was set to zero, and levels were kept as is at 0, 1.0, and 255.
    Last edited by hmzimelka; 08-29-2012 at 03:39 AM. Click to view previous post history.

  10. #10

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    Looking at the full res images it's hard to tell them apart.
    The original liberated Rodinal formula used potassium not sodium though:
    http://www.apug.org/forums/forum37/2...elligence.html
    It is said the sodium version is slightly softer working.
    The PaRodinal that is sold in the Phillipines uses potassium.
    In the clear version of Parodinal the crystals may take months to appear but disappear again in hot weather.
    IDK if the potassium version avoids the crystals,but many potassium salts are more soluble than sodium salts.

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