Diffusion Transfer Printing ("Polaroid" peel-apart) recipes

[alecrmyers]

I have not (yet) got a DEHA/uracil developer to work with a paper negative. Having said that, I haven’t spent a lot of time trying. I will give it a go tomorrow.

off the top of my head:

Your developer should likely be 15-20% by weight of -ium hydroxide.
CMC is at your discretion
Uracil looks about right, a little high maybe but not crazy
AEEA try half that
DEHA looks low but I suppose will depend on your negative material, so if you get a well developed negative then I wouldn’t mess with it too much

Receiver part A is merely a solution of PdCl2 in water, the acid is there only just enough to dissolve the salt (as the tetrachloropalladate ion), a little excess doesn’t hurt but it’s slow to dissolve so add a few drops at a time and leave it to stir for 20 minutes in between. 100 drops of HCl (you don’t say what concentration so I’m assuming hardware store “muriatic”, which is usually 31% by weight) seems very high.

Receiver part B looks massively too rich in palladium: I would try 5 drops of part A and work from there. Look for something between the colour of pale urine and a fine brandy after adding the borohydride.

 

[Qebs]

Thanks Alec, I really appreciate this.
I will try your suggestions.

Hydrochloric acid 0.1 M
And I found I needed a lot to get the PdCl2 to dissolve.

As well, I needed a lot of part A to work.
The day before I tried again at 25 and 35 drops of Part A and image quality was low. It was faded and low contrast.
I need to look at my notes, but I think 60-70 worked, but I did the less educated thing and just used 100.
Could too much PdCl2 or part A give bad highlights.
Either blown out or creamy/muddy?

 

[alecrmyers]

Thanks Alec, I really appreciate this.
I will try your suggestions.

Hydrochloric acid 0.1 M
And I found I needed a lot to get the PdCl2 to dissolve.

In that case use 10ml of your 0.1M HCl and 10ml of distilled water, and 20mg of PdCl2. Yes, it will take a while to dissolve.

A few drops of 0.1% PdCl2 is plenty for 20ml of silica. The problem is your developer, not your paper. Increase your hydroxide as I suggested and try again.

 

[analogwisdom]

This is the best I've been able to get with the Cellulose Acetate (CA)/palladium coating, so far:

View attachment 416839

This is with Dimezone S in the developer. It appears to give a speed increase over Metol when used on CA paper, but first tests suggest a loss of density on silica.

Looks good! I wonder if the speed increase over Metol is due to degradation of Metol in the alkali solution?

https://pdf.benchchem.com/52/Preventing_Metol_degradation_in_aqueous_solutions.pdf

Interesting little paper I found. When I have used metol the developer has instantly turned deep red when I'm mixing it in, so I must be doing something incorrectly.

 

[alecrmyers]

Looks good! I wonder if the speed increase over Metol is due to degradation of Metol in the alkali solution?

https://pdf.benchchem.com/52/Preventing_Metol_degradation_in_aqueous_solutions.pdf

Interesting little paper I found. When I have used metol the developer has instantly turned deep red when I'm mixing it in, so I must be doing something incorrectly.

I don't think so. I've had developer with Metol at KOH 20% by weight sitting on the bench for 8 months and it's fresh as the day it was mixed.

A quick view of that paper indicates it's talking about oxidation of the Metol. In the developer is 6% DEHA whose primary purpose is an oxygen scavenger in high pressure boiler systems. (That's the only reason it's affordable.) I don't think there's much oxygen left in the aqueous system with that present.

My naive understnding of the way superaditive developers work is that the Metol reduces the silver halide and the second developer (DEHA) reduces the oxidized Metol (I don't know what its oxidation product is, I'm afraid) back to Metol. So I would expect the Metol to be safe until all the DEHA is oxidized first. At 6% by weight the DEHA is about 0.67M, and oxygen saturated water has an oxygen concentration of 2.4x10-4M, about 3000 times lower. I think the Metol is safe.

That's my back of the envelope analysis.

>When I have used metol the developer has instantly turned deep red when I'm mixing it in, so I must be doing something incorrectly.

Did you add it before or after the DEHA?

 

[alecrmyers]

@Qebs

I did some experiments with Ilford multigrade this morning. This is what I came up with:

Results look pretty good to me. How badly do you want to know how I did it?

 

[analogwisdom]

I don't think so. I've had developer with Metol at KOH 20% by weight sitting on the bench for 8 months and it's fresh as the day it was mixed.

A quick view of that paper indicates it's talking about oxidation of the Metol. In the developer is 6% DEHA whose primary purpose is an oxygen scavenger in high pressure boiler systems. (That's the only reason it's affordable.) I don't think there's much oxygen left in the aqueous system with that present.

My naive understnding of the way superaditive developers work is that the Metol reduces the silver halide and the second developer (DEHA) reduces the oxidized Metol (I don't know what its oxidation product is, I'm afraid) back to Metol. So I would expect the Metol to be safe until all the DEHA is oxidized first. At 6% by weight the DEHA is about 0.67M, and oxygen saturated water has an oxygen concentration of 2.4x10-4M, about 3000 times lower. I think the Metol is safe.

That's my back of the envelope analysis.

>When I have used metol the developer has instantly turned deep red when I'm mixing it in, so I must be doing something incorrectly.

Did you add it before or after the DEHA?

I actually haven't made a DEHA developer with metol added yet. The oxidation(?) happened in my TBHQ-based one. I added the metol last. Perhaps I didn't have enough sulfite.

 

[analogwisdom]

@Qebs

I did some experiments with Ilford multigrade this morning. This is what I came up with:

View attachment 416884

Results look pretty good to me. How badly do you want to know how I did it?

Wow, great dmax. The contrast is great too.

 

[alecrmyers]

Wow, great dmax. The contrast is great too.

The contrast is great if that's the look you're going for, but it would be nice to be able to dial it down a bit. I'm not sure if that's a developer or a transfer agent issue. I suspect the former. It might just be the negative material, too. Perhaps worth trying a yellow filter to reduce contrast; it is multigrade, after all.

 

[alecrmyers]

I actually haven't made a DEHA developer with metol added yet. The oxidation(?) happened in my TBHQ-based one. I added the metol last. Perhaps I didn't have enough sulfite.

The staining (because of oxidation) issue is one reason why I wasn't unhappy to move away from hydroquinone//thiosulphate/sulfite systems. I wonder with your yellow/brown print earlier how much of the tone is due to residual developer.

 

[Qebs]

Hey Alec, I for one, would really love to know how you did it to compare with my attempt that's about to start.
Thanks so much

 

[alecrmyers]

Hey Alec, I for one, would really love to know how you did it to compare with my attempt that's about to start.
Thanks so much

It's basically exactly the changes to what you were doing that I suggested a few posts ago. I just used my "regular" silica paper and "regular" developer, that I've been using with the x-ray film. It works really well on Multigrade paper too.

 

[Qebs]

It's basically exactly the changes to what you were doing that I suggested a few posts ago. I just used my "regular" silica paper and "regular" developer, that I've been using with the x-ray film. It works really well on Multigrade paper too.

Thanks Alec!


Did you mean this developer?

25g base (2.5% CMC and 10% w/w NaOH)
sodium carboxymethylcellulose (CMC)

2.5g uracil pyrimidine-2,4(1H,3H)-dione
1.0g diethylhydroxylamine (DEHA)
0.5g aminoethylethanolamine (AEEA)
0.1g metol ( 4-methylamino)phenol sulphate )

 

[alecrmyers]

I'm not going to list the ingredients for you.

Start with what you wrote here:
Developer:
43 grams of H20
2.8 grams of NaOH
1.75 grams of CMC
5.2 grams of Uracil
1.2 grams of AEEA
2.2 grams of DEHA
0.1 grams of Metol

And try these adjustments:

off the top of my head:

Your developer should likely be 15-20% by weight of -ium hydroxide.
CMC is at your discretion
Uracil looks about right, a little high maybe but not crazy
AEEA try half that
DEHA looks low but I suppose will depend on your negative material, so if you get a well developed negative then I wouldn’t mess with it too much

 

[Qebs]

Wonderful, I'll go with your original advice.
Thanks so much for your support Alec.
I really appreciate it
Have a lovely weekend

 

[alecrmyers]

Wonderful, I'll go with your original advice.
Thanks so much for your support Alec.
I really appreciate it
Have a lovely weekend

OK, good luck - let's see the results.

 

[Qebs]

Hey,
Here is what I did:

• 39.1 g distilled water
• 7.22 g NaOH
• 1.8 g sodium CMC
• 5.0 g uracil pyrimidine-2,4(1H,3H)-dione
• 2.2 g diethylhydroxylamine (DEHA)
• 1.0 g aminoethylethanolamine (AEEA)
• 0.10 g Metol sulphate

The new image is on the right, with the big finger print

Now there is more of an evident yellow cast.
It still has this muddy cast that drops the exposure a fair amount.

I had the cast at times with Ilford paper but eventually got it more under control.
This yellow cast is interesting though, no idea why they both have it to a degree. Maybe I have a contamination issue.
NaOH % with Total Developer before was 4.9%
After adjustments, I got to 12.3% (I missed the 15% mark as I accidentally compared with the developer's base mass.
Anyone have any ideas what I should try next?

Keep increasing NaOH, maybe 18%?
I keep wondering if it's not enough DEHA or Metol as it's the pooling that gets a good development result. This is where time elapses before I can manage to put the sandwich through the laminator machine.

What is a reasonable amount to increase the DEHA?

 

[analogwisdom]

Hey,
Here is what I did:

• 39.1 g distilled water
• 7.22 g NaOH
• 1.8 g sodium CMC
• 5.0 g uracil pyrimidine-2,4(1H,3H)-dione
• 2.2 g diethylhydroxylamine (DEHA)
• 1.0 g aminoethylethanolamine (AEEA)
• 0.10 g Metol sulphate

The new image is on the right, with the big finger print

Now there is more of an evident yellow cast.
It still has this muddy cast that drops the exposure a fair amount.

I had the cast at times with Ilford paper but eventually got it more under control.
This yellow cast is interesting though, no idea why they both have it to a degree. Maybe I have a contamination issue.
NaOH % with Total Developer before was 4.9%
After adjustments, I got to 12.3% (I missed the 15% mark as I accidentally compared with the developer's base mass.
Anyone have any ideas what I should try next?

Keep increasing NaOH, maybe 18%?
I keep wondering if it's not enough DEHA or Metol as it's the pooling that gets a good development result. This is where time elapses before I can manage to put the sandwich through the laminator machine.

What is a reasonable amount to increase the DEHA?

View attachment 416939

I would try doubling the metol.

 

[alecrmyers]

Use a slower speed on the laminator or thicker rails.

If the negative is well developed then the DEHA and metol are good. For experimentation, skip the metol entirely and add a stop of exposure. It’s one fewer variable to worry about.

The yellow cast is probably not “contamination” unless you are making up your solutions with seawater.

 

[analogwisdom]

Use a slower speed on the laminator or thicker rails.

If the negative is well developed then the DEHA and metol are good. For experimentation, skip the metol entirely and add a stop of exposure. It’s one fewer variable to worry about.

The yellow cast is probably not “contamination” unless you are making up your solutions with seawater.

Do you think it's possible his developer is too viscous? Where it's more white on the puddle made me think this might be a possibility. The thin layer might be too viscous to allow proper diffusion of the silver-uracil complex?

I hope I'm not too far off base. I really am trying to learn fundamentally how this process works.

edit: thicker rails or slower speed might achieve the same thing (I see where you suggested that now)

 

[alecrmyers]

Do you think it's possible his developer is too viscous? Where it's more white on the puddle made me think this might be a possibility. The thin layer might be too viscous to allow proper diffusion of the silver-uracil complex?

I hope I'm not too far off base. I really am trying to learn fundamentally how this process works.

edit: thicker rails or slower speed might achieve the same thing (I see where you suggested that now)

I can speak only from my experience, which suggests that viscosity isn't important, except for practical convenience: too loose and the developer runs all over the place; too thick and it doesn't wipe up easily. 2.5-4% CMC seems to work well for me without any obvious differences to the results within that range.

My processor runs at 7mm per second. Rolling speed makes a big difference to print density, for me.

Rail thickness did too, until I gave up using them.

This morning I've tried thirteen variations on a new developer. Yesterday and thursday it was eight different ways to get the silica to stick to the paper. Understanding is great, but it comes through doing. The knowledge is out there but the universe is going to make you fight for it.

 

[analogwisdom]

I can speak only from my experience, which suggests that viscosity isn't important, except for practical convenience: too loose and the developer runs all over the place; too thick and it doesn't wipe up easily. 2.5-4% CMC seems to work well for me without any obvious differences to the results within that range.

My processor runs at 7mm per second. Rolling speed makes a big difference to print density, for me.

Rail thickness did too, until I gave up using them.

This morning I've tried thirteen variations on a new developer. Yesterday and thursday it was eight different ways to get the silica to stick to the paper. Understanding is great, but it comes through doing. The knowledge is out there but the universe is going to make you fight for it.

View attachment 416969

you're right. I think #3 on top looks best.

I spent all day working on the best technique for coating with the bar. I think I'm starting to get the hang of it. The laminator machine came just about an hour ago, and I was in a hurry so I shoved a quick 8x10 through.

this is with a photo paper negative. the developer I used was unlabeled, but I believe it was TBHQ + metol. I shot the paper at around ISO 10. One step forward, two steps back. Back at it again tomorrow. Going to cut the sheets I coated down to 4x5 and try X-ray film.

 

[analogwisdom]

Here's the "negative". Some interesting(?) partial solarization.

 

[Qebs]

Thanks AnalogWisdom and Alec for your inputs.
This laminator I have runs at about 10-15 mm per second.

Okay, I will try later this week more metol and no metol.
Alec, may I ask, when you don't use rails, how do you keep developer from laminating out the sides of the sandwich?

Do you just use more developer and have to clean up more?
Keep up the hard work AnalogWisdom.
It will totally pay off in the future.
I for one, am confident this is process I want to do for many years. There are so many artist reasons to love this process.
And I really love the immediacy but also truthful mechanical representation moments that I can share with a portrait subject/client. I can't thank you all Alec enough!
I'm going to try double and triple rails and for experimentation no rails.
Have a good rest of your weekend everyone.

 

[analogwisdom]

Here's a result with the same paper and a developer with only TBHQ.