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  1. #1
    Mustafa Umut Sarac's Avatar
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    Autochrome Recipe from Metropolitan Museum of Art

    I received below mail from Luisa Casella from Metropolitan Museum of Art.
    I sent a mail her couple of hours ago about the preperation of starch grains , tinting them and finding from the market.

    Luisa Casella

    Sherman Fairchild Center for Works on Paper and Photograph Conservation

    The Metropolitan Museum of Art

    1000 Fifth Avenue

    New York, NY 10028-0198

    T. +1 212 396 5524

    F. +1 212 650 3811

    E. luisa.casella xxxxxxxx metmuseum.org


    APPENDIX I: PREPARATION OF THE LAYERS1



    Selecting the starch grains

    Autochrome starch grains were in the range of 10 to 20 microns in diameter. Resolution of the image is not critical for the present experiment. A separation by flotation will be done to avoid larger grains2.

    Fill a large container with 2 liters of distilled water and 75 grams of potato starch.

    Stir vigorously. Allow it to set for 15 minutes. The majority of grains are deposited in the bottom, while the smaller particles remain in suspension. Using a plastic tube, siphon the intermediate layer as best as possible (avoiding being to close to the top or the bottom).

    Filter this solution using a Büchner funnel covered with filter paper, recovering a few grams of starch grains. Rinse these in ethanol and air dry.

    After dry, gently pestle the grains in a mortar to separate lumps.


    Tinting of starch grains:

    Dilution of the dyes in distilled water will be done according to original dilutions in autochrome plates:


    Orange-red grains:

    Distilled water – 100 ml

    Erythrosine – 14,5 g

    Rose Bengal – 2,6 g

    Tartrazine – 19,7 g

    Green grains:

    Distilled water - 100 ml

    Ammonia - 9 g

    Tartrazine - 21 g

    Patent Blue - 10 g

    Sodium Sulfate - 21 g

    Violet-blue grains:

    Distilled water - 100 ml

    Crystal Violet - 7 g

    Malachite Green - 1 g


    Tartrazine was used in different concentrations both in the orange-red (19,7g) and in the green grains (21g); the concentration for this experiment will therefore be the approximate average - 20g.

    In the case of the dyes present in the green dye (tartrazine and the patent blue) ammonia and sodium sulfate are added so the ionic environment provided by the starch would adsorb the colors.


    Tinting:

    The selected starch grains are mixed to its mass equivalent in dye-saturated solution.

    The solutions so far are:

    1.

    100 ml water

    Erythrosine – 14,5 g

    2.

    100 ml water

    Rose Bengal – 2,6 g

    3.

    100 ml water

    Tartrazine - 20 g

    Ammonia - 9 g

    Sodium Sulfate - 21 g

    4.

    100 ml water

    Patent Blue - 10 mg

    Ammonia - 9 g

    Sodium Sulfate - 21 g

    5.

    100 ml water

    Crystal Violet - 7 g

    6.

    100 ml water

    Malachite Green - 1 g


    The ratio in the original recipe was of starch to dye is:

    - 2,3g dye to 3g starch for the orange (Erythrosine, Rose Bengal, Tartrazine)

    - 2,24g to 3g starch for the green (Patent Blue, Tartrazine)

    - 2,25g dye to 3 g starch for the blue-violet (Crystal Violet, Malachite Green)


    In the present experiment the dyes are individually added to the starch. The ratio will be maintained as above, except for Tartrazine of which an average value will be used (2,27g).


    Stir the mix for 30 minutes to one hour until there are no white starch grains. This is done at room temperature, except for Crystal Violet and Malachite Green which need to be at 30°C using a double-boiler. Strain the solution through Whatman filter paper and air dry.


    Preparation of Varnish Layers

    First varnish:

    Toluene - 100 g (87 ml)
    Natural rubber - 1,5 g
    Dissolve the rubber in toluene for 24 hours.

    Add:

    5,6 ml of the 10% solution of dammar residue in toluene (see second varnish) - this solution is obtained from the mixture described in the second varnish (ethyl acetate and dammar) after rinsing with 60ml of ether and let dry. Make a 10% solution in toluene3.


    Second varnish: 4

    In a container, add:

    Ethyl acetate – 300 ml
    Dammar gum – 28,8 g
    Let dissolve for 24 hours, stirring occasionally. An insoluble residue is left in the bottom. Recover this residue using filter paper. Use the residue for first varnish.

    Add to the filtered solution:

    7,2g nitrocellulose
    Stir until complete dissolution (few days) and add:

    Castor oil – 4,536 g
    Strain using filter paper.





    APPENDIX II: INFORMATION ON DYES USED FOR THE EXPERIMENT



    1.

    CI #: 19140

    Name: Tartrazine

    Family: Azo

    Other Names: Acid Yellow 23

    CAS#: 1934-21-0

    Supplier: Fluka/ Sigma-Aldrich

    Name given by supplier: Tartrazine

    Solubility: 0.5gr/ 10ml*


    2.

    CI #: 42025

    Name: Malachite Green Ortho-chlorinated

    Family: Triarylmethane

    Other Names: Setoglaucin, Basic Blue 1

    CAS#: None

    Supplier: Salor/ Sigma-Aldrich

    Name given by supplier: Rhoduline Blue 6G

    Solubility: No known value*


    3.

    CI #: 42051

    Name: Patent Blue

    Family: Triarylmethane

    Other Names: Acid Blue 3

    CAS#: 3536-49-0

    Supplier: Fluka/ Sigma-Aldrich

    Name given by supplier: Patent Blue V calcium salt

    Solubility: Water soluble*










    4.

    CI #: 42555

    Name: Crystal Violet

    Family: Triarylmethane

    Other Names: Basic Violet 3

    CAS#: 548-62-9

    Supplier: SIAL/ Sigma-Aldrich

    Name given by supplier: Crystal Violet

    Solubility: 0.01-0.1gram/ 100 ml at 15.5°C*


    5.

    CI #: 45430

    Name: Erythrosine

    Family: Xanthene

    Other Names: Acid Red 51

    CAS#: 568-63-8

    Supplier: National Aniline & Chemical Co.

    Name given by supplier: Erythrosin, Bluish (Iodin Eosin)


    6.

    CI #: 45440

    Name: Rose Bengal

    Family: Xanthene

    Other Names: Acid Red 94

    CAS#: 632-69-9

    Supplier: Aldrich/ Sigma-Aldrich

    Name given by supplier: Rose Bengal

    Solubility: 100mg/ ml*




    *Data provided by Sigma-Aldrich technical services based on their experiments.

    Filter
    Dye
    C.I. Number
    Other Names
    Appearance

    Orange-red
    Erythrosine B
    45430
    Acid Red 51
    Yellow

    Rose Bengal
    45440
    Acid Red 94
    Magenta

    Tartrazine*
    19140
    Acid Yellow 23
    Red

    Green
    Patent Blue
    42051
    Acid Blue 3
    Blue

    Tartrazine*
    19140
    Acid Yellow 23
    Red

    Violet-blue
    Crystal Violet
    42555
    Basic Violet 3
    Purple

    Setoglaucine or Malachite Green Orthochlorinated
    42025
    Basic Blue 1
    Blue

    * Tartrazine was used both in the red-orange and the green grains




    Best ,

    Mustafa Umut Sarac

    Istanbul

  2. #2

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    Mustafa - thanks for getting that info. There's some really solid details there!
    Kirk

    For up from the ashes, up from the ashes, grow the roses of success!

  3. #3
    Ian Grant's Avatar
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    Mustafa,

    Back in the 70's I worked with(employed as a consultant) someone who had family connections with the Autochrome process, his mother was French and her family had owned the Lumière company, before it was bought by I think Tellko AG, later to become part of Ciba Geigy, and later an Ilford plant. Technically it still exists as the sales arem of Ilford in France..

    Tim had quite a lot of reference materials I'll try and contact him when I'm next in the UK and see what he has.

    The secret of the process is the pressure used to squash and compact the starch grains, Autochrome plates and also films where still being made in 1939, I'm not sure when they stopped.

    Ian

  4. #4
    Photo Engineer's Avatar
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    There was a 4th black dye added to the above mix and all 4 of them had specific ratios to prepare the correct color. The nature of the mix was determined by the spectral sensitivity of the film itself.

    They dyed starch grains were applied to the varnish layer by a raking process to spread them evenly and randomly across the varnish and then the material was rolled or pressed flat under pressure that flattened the grains. The emulsion was then coated on top.

    Part of this is described in the textbook "History of Color Photography".

    PE

  5. #5
    AgX
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    Quote Originally Posted by Ian Grant View Post
    ...Autochrome plates and also films where still being made in 1939, I'm not sure when they stopped.
    Lumière offered film based on random filter particles up into the 50's as it was cheaper than its competitors based on the subtractive filter layers system (chromogenic development).

  6. #6
    Mustafa Umut Sarac's Avatar
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    I forgot to tell that she advised to me to buy Bertrand Lavedrine’s book. I asked again the mixing ratios of these dyed colors also. I hope She answers. Ian , please do that, this is very important. PE , You hit the bulls eye again , film sensivity and the mixing ratio relation is very important trick
    If I oeder this book , it tooks 2 months to understand it is lost or reached to customs. Is there someone who owns the book and write here some recipes ?

    Best ,

    Mustafa Umut Sarac

    Istanbul

  7. #7
    Mustafa Umut Sarac's Avatar
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    I reecieved below message from Metropolitan Museum of Art again . Here is the Autochrome dyed grains mixing ratios from 1930.

    Luisa Casella says :

    Since I used the dyes individually, my ratio is a little different.

    The ratio depends on the year of manufacture.

    The ratio I had from Bertrand from 1930 was:



    ratio mass of starch in mg/ for solution in mg

    for orange grains 1.3

    for green grains 1.34

    for blue-violet grains1.33

    Best ,

    Mustafa Umut Sarac

    Istanbul

  8. #8
    Photo Engineer's Avatar
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    In spite of all of this information, no one has been able to duplicate the work of the brothers Lumiere! This has truly been an impossible project that no one has gone to the finish line with since the Autochrome line shut down all those years ago. This is coming from an expert in the subject matter who sent me a note on this thread from George Eastman House.

    PE

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    Mustafa Umut Sarac's Avatar
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    http://www.autochromes.fr/english/004_champlan2.html

    Look at Frederic Mocellin from France. I contacted with him and he says he tried to collect all information to create a autochrome for years and than French book - I gave the writers name in this thread - came to life and he used all the information from the book. He says it is too long to tell the whole process at the mail football and he says this book is the bible and everyone can do with it.

    Look at the pictures , absolute success .

    May be the new lenses are too sharp or differently sharp for this process.
    If someone tries all and calibrate the colors , there will be success with old lenses.

    pe , you know this guy , I found at your older posts.

  10. #10
    dwross's Avatar
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    Quote Originally Posted by Photo Engineer View Post
    In spite of all of this information, no one has been able to duplicate the work of the brothers Lumiere! This has truly been an impossible project that no one has gone to the finish line with since the Autochrome line shut down all those years ago. This is coming from an expert in the subject matter who sent me a note on this thread from George Eastman House.

    PE
    Well, good grief. It wasn't Immaculate Conception! I'm damn glad I haven't been listening to the 'It's-as-good-as-impossible' mantra.

    Mustafa. I have the Lavedrine book. I'll get the autochrome pages scanned tonight or tomorrow morning and pm them to you. Good luck! I'm sure you'll make it happen.

    d

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