Autochrome Recipe from Metropolitan Museum of Art

[Mustafa Umut Sarac]

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

 

[Kirk Keyes]

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

 

[Ian Grant]

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

 

[Photo Engineer]

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

 

[AgX]

...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).

 

[Mustafa Umut Sarac]

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

 

[Mustafa Umut Sarac]

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

 

[Photo Engineer]

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

 

[Mustafa Umut Sarac]

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.

 

[dwross]

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

 

[Mustafa Umut Sarac]

dwross , thank you very much indeed , my e mail address is mustafaumutsarac@gmail.com
If you can scan with optical character recognition software , scanning took few hours but the file size becomes very small.
If you scan it with picture jpeg format , it takes 80 mb or so . My e mail account accepts less than 20 mb posts. So you might use 4 mails least.
I hope your scanner is fast and dont make you tired.
I thank you again , this book is so expensive that I never be afford it at this winter time

Thanks again

 

[Photo Engineer]

Denise, Mustafa;

I know of no one doing successful work on Autochromes. I see the results at that web site and I can say that they look nothing like the Autochromes I have in my posession and none that I have seen at exhibits. This is apart from coating flaws which I expect in this type of work.

I have been told by respected workers in the field that there were parts of the process that were not documented, and were "trade secrets", not Immaculate Conception! There is a difference. These trade secrets involve the use of that black pigment and the formation of lenticules out of the starch grains under pressure. There were apparently several more steps that were also omitted from the published documentation. People I know of have actually visited the site where the last of their machines is preserved and no one there knew how to operate the equipment, nor was there any documentation beyond the patents that the brothers published.

I guess it is not impossible, but very very difficult, and this person has a long way to go to get to the level of the original. I don't want to discourage anyone, but I personally am not going to work on this approach as it is far to difficult. Remember, an appendix can be removed via the mouth. Difficult but doable. There are easier ways to remove an appendix just as there are easier ways to achieve color.

My belief is that dye bleach is probably a better approach. I would also like to add that doing a Dufay type color material is rather easy and straightforward. I have seen it done.

Best wishes to those who wish to experiment on either approach.

PE

 

[Mustafa Umut Sarac]

May be We can overcome with press problem with pressing the dyed grains before the coating in homemade smaller press in very small batches.

Than we collect all flatten grains ,

coat a flat glass with this flat grains , and of course they will lie on the glass surface with lots of angles.

We apply vibration or we close a second teflon plate on to the surface and hand press the grains with this second teflon plate while moving it to the right left .

Whenever we sure that every grain is parallel to the glass plate , we remove the teflon plate and take the adhesived autochrome plate and make them kiss .

And another question to you :

Do autochrome plate we made , contact copy the original French one exactly the same ?

If yes , We can make experiments until get the correct materials and methods until we get twins.

Best ,

Mustafa Umut Sarac

Istanbul

 

[Photo Engineer]

The currently posted Autochromes lack density, contrast and color saturation when compared to the original Autochromes that I have. They also lack the distinctive grain pattern evident even viewing an original Autochrome by eye.

The first 3 can be attributed to the silver quantity coated, the lack of the black pigment grains, and perhaps spectral sensitivity or dye quantities used. The second item may be attributed to the resolution of the scan, the fineness of the silver halide grain or the size of the starch particles.

As you see, there are too many things to ponder here to sort them out just by this simple viewing over the internet. The appended photos are the original box of stereo Autochromes that are in my posession and a scan of a 6x6 singlet from a pair that pretty much duplicates what the eye sees in terms of color and grain.

PE

 

[Mustafa Umut Sarac]

Ron , Where can buy from such a exposed plate ? Are they very expensive ?

 

[Photo Engineer]

I have seen plates like this and up to 5x7 in the price range of $20 - $60 US. They are rather common at photo shows which is where I picked these up.

One of the most beautiful was a 5x7 plate, a portrait of a young girl circa 1920 or so. Very beautiful. Of course, the grain appears to go down as the size of the plate increases.

PE

 

[Mustafa Umut Sarac]

http://3.bp.blogspot.com/_l5YNpRMm2eA/S06UimxEAgI/AAAAAAAAABg/RpG-Zz1N9IY/s1600-h/DSC01481.JPG

Ron , look at this image , I took it with summitar Leica II F.
I know what you mean with quality

Do you sell me one ?

Mustafa Umut Sarac

 

[Photo Engineer]

Mustafa;

The color range in that photo is so limited, it is difficult to evaluate. The grain is exceptionally fine though. You should read the treatment of "grain" in this type of system in "History of Color Photography".

As for my slides, they are a complete set. I don't want to break the set.

PE

 

[Athiril]

PE: Out of curiousity, how would you dye a single layer emulsion that would hold the dye during processing?

 

[Photo Engineer]

PE: Out of curiousity, how would you dye a single layer emulsion that would hold the dye during processing?

I would use an anionic dye and mordant it in place with a divalent or trivalent metal or use a cationic mordant. So, for example, I would dissolve a sulfonate of an azo dye in water + gelatin, then I would precipitate it in-situ with Aluminum or Calcium Sulfate, wash our the excess Sulfate, mix with the emulsion and coat.

This is exactly what I have done to make multi and single color coatings for dye bleach and it is quite simple.

PE

 

[Athiril]

Ah.

I was hoping it might be possible to take an existing pan film and dye bleach it in some kind of fogging development with the needed dyes before bleaching, dry and using

 

[Photo Engineer]

This could be done, but you would need 3 sheets of film for the R/G/B record and a 3 color beam splitting camera such as used about 100 years ago for color.

PE

 

[Ian Grant]

This could be done, but you would need 3 sheets of film for the R/G/B record and a 3 color beam splitting camera such as used about 100 years ago for color.

PE

Ron, they were still made in the 1950's, that's in quite a few here's lifetime but their heyday was the 1930's and 40's with the growth of colour litho printing.

The Eve's One Shot was available in 1954 in 2 sizes 5"x4" and 6x9cm.

Ian

 

[Photo Engineer]

Thanks Ian, but I am fully aware of that time scale. This subject often comes up on the Dye Transfer Forum where I post from time to time. I was referring to the heyday of tricolor separation photography.

PE

 

[dwross2]

I love learning new things. I wasn't aware of Lavedrine's book in French specifically on Autochrome. I don't own that one. The book I have is a survey of all historical processes. Anyway, I put together the info I have access to here: http://thelightfarm.com/Map/Books/Temporary/BookReview.htm

Also, I could use a little help from old APUG hands. My computer had a nervous breakdown this week and I finally gave up and rebuilt it (rather more truthfully, my husband did ) I have long ago forgotten my APUG password and getting back in under my original user name defeated me. I kept being sent to APUG form pages that then said I couldn't be there. ?? Help! :confused: I miss my racoon avatar and being able to read my pm's. Thanks.

Denise