Disappointing results (i.e. nothing happened !)

[slm]

Hello Everyone, I just tried mixing (first time mixing anything from raw chemicals) the D-85 found on unblinkingeye.com. I followed the formula in the order shown, mixing each chemical in until fully dissolved. I also substituted the Paraformaldehyde for acetone.
Nothing happened ! I left a test strip in the developer for 20mins, and nothing. I tried Ilford Multi FB paper (wasn't expecting it to work from what I read, but tried anyways) and Forte Poly warm tone FB (supposed to be lithable). I then left the test strips out (of the tray that is), with any developer left in it, over night. There has been a change in paper color (Forte is copper looking). Any ideas where I went wrong, and if I can add to or save the batch ?

thanks
steven


D-85 Two Solution Lith Developer

Solution A
Water at 125° F 500 ml
Sodium sulphite 36.5 g
Boric acid crystals 9.4 g
Hydroquinone 28 g
Potassium bromide 2 g
Water to make 1 litre

Solution B

Water at 90 ° F 500 ml
Sodium bisulphite 11 g
Sodium sulphite 1 g
Paraformaldehyde 37.5 g
Water to make 1 litre

Mix solutions with good ventilation. Mix 4 parts A + 1 part B for use.
You may substitute 82.5 millilitres of acetone for the paraformaldehyde.

 

[psvensson]

The formula seems to be missing an alkali! Very strange. I checked unblinkingeye and digitaltruth, and they have the same formula. Try adding 10g sodium hydroxide or 30g sodium carbonate.

 

[Gerald Koch]

The paraformaldehyde reacts with the sodium sulfite to generate sodium hydroxide and the formaldehyde sulfur dioxide addition product.

Na2SO3 + H2O + HCHO --> 2NaOH + HCHO.SO2

 

[psvensson]

... but if you're using acetone instead of formaldehyde, does the same thing happen?

Edit: Indeed, it seems it should.

 

[Gerald Koch]

Yes. It is the carbonyl (-CO-) group in both acetone and formaldehyde which reacts.

 

[psvensson]

It's great to have real chemists on the board! I'd still add some alkali to the mix to see what happens. When I've tried Ilford papers in my homemade lith developers, it's not that they don't develop, they pretty much turn grey-black all over, immediately. See the Dr. Jekyll formulas in the paper developer formulas section.

 

[Photo Engineer]

Yes. It is the carbonyl (-CO-) group in both acetone and formaldehyde which reacts.

While I agree with this statement, I question the rate at which it proceeds and the yield that it gives.

If either rate or yield is off, you don't get the amount of base that you are entitled to.

My question is this... Was part "B" cloudy? This is a characteristic of the reaction when the paraformaldehyde reaction does not take place or is slow or is incomplete. In that case, there was not enough base formed. If acetone was used, remaining acetone odor is the clue that things didn't work as expected.

This is a neat way to get base, but I wouldn't do it myself for any reason other than avoiding handling sodium hydroxide. But then you are substituting formalin. Nice tradeoff.

PE

 

[Gerald Koch]

The portraitist G. Paul Bishop used the following for all his negatives. Here the acetone serves only to create an alkaline solution by reacting with the sulfite.

Water .................................. 28 oz
Acetone ................................ 1 oz
Sodium sulfite (anhy) .................. 30 gr
Metol .................................. 20 gr

http://www.gpaulbishop.com

 

[slm]

While I agree with this statement, I question the rate at which it proceeds and the yield that it gives.

If either rate or yield is off, you don't get the amount of base that you are entitled to.

My question is this... Was part "B" cloudy? This is a characteristic of the reaction when the paraformaldehyde reaction does not take place or is slow or is incomplete. In that case, there was not enough base formed. If acetone was used, remaining acetone odor is the clue that things didn't work as expected.

This is a neat way to get base, but I wouldn't do it myself for any reason other than avoiding handling sodium hydroxide. But then you are substituting formalin. Nice tradeoff.

PE

Hi, yes part B is cloudy, and still has a strong acetone odor. Working solution is clearer, maybe just a tint of cloudiness, and has a much less pronouced acetone odor.
Can I fix this, or is it just no good ? Also, was considering trying Ansco 81, but I can't find dilutions to use with paper developing.

Many thanks for all the replies !
Steven

 

[Gerald Koch]

The reaction between acetone or formaldehyde does not go to completion but is in equilibrium. The intent is to reduce the amount of sulfite ion in solution to a low level to encourage infectious development. As sulfite is used up more is released from the addition product. In other words the adduct is a reservoir for sulfite ion.

 

[Donald Qualls]

From my reading on this, I understand lith printing requires a HUGE amount of exposure -- that is, many minutes for paper that would require a minute or less for development in Dektol; it then takes a relatively long time for the image to begin to appear in the lith developer. Is it possible your paper either simply didn't get enough light for the lith developer to bring up an image, or wasn't left in the developer long enough (like fifteen minutes, if I recall correctly)?

 

[Photo Engineer]

Hi, yes part B is cloudy, and still has a strong acetone odor. Working solution is clearer, maybe just a tint of cloudiness, and has a much less pronouced acetone odor.
Can I fix this, or is it just no good ? Also, was considering trying Ansco 81, but I can't find dilutions to use with paper developing.

Many thanks for all the replies !
Steven

Steven, residual acetone odor indicates that the formation of the sulfite adduct was incomplete. Less alkali was formed than desired, but by how much is hard to determine. Also, acetone reacts itself with alkali, forming polymeric compounds IIRC, and can further tie up the alkali.

To my way of thinking, this is a very qualitative way of making a developer and I would not use it myself personally. By all means, try other lith developers, and Donald has a very good point above about exposure.

PE

 

[psvensson]

Looking at the formula, I would guess that acetone is in excess in B, so that it can absorb the sulfite in A when the solutions are mixed together. So it would make sense that even as designed, part B would have an acetone smell.

 

[Photo Engineer]

Looking at the formula, I would guess that acetone is in excess in B, so that it can absorb the sulfite in A when the solutions are mixed together. So it would make sense that even as designed, part B would have an acetone smell.

Quite possibly true (I didn't do a molar calculation), but the excess acetone, if present, would begin reacting with the sodium hydroxide in an aldol condensation creating polymers and reducing the amount of acetone available for producing further base thereby possibly reducing the alkalinity. The point is that this is a qualitative method for generating base in situ.

It can be used, but I wouldn't.

It is so much easier to add X grams of NaOH. One ingredient instead of 2 and having to hope that things turn out for the best. The relative concentration of NaOH and the rate of appearance in soltuion would depend on room temperature as well.

PE

 

[dancqu]

Hello Everyone, I just tried mixing ...
D-85 Two Solution Lith Developer

Solution A
Water at 125° F 500 ml
Sodium sulphite 36.5 g
Boric acid crystals 9.4 g
Hydroquinone 28 g
Potassium bromide 2 g
Water to make 1 litre

Solution B

Water at 90 ° F 500 ml
Sodium bisulphite 11 g
Sodium sulphite 1 g
Paraformaldehyde 37.5 g
Water to make 1 litre
QUOTE]

By way of contrast, Wall's Normal Hydroquinone:

Solution A;
Sodium Sulfite 100 grams
Hydroquinone 20 grams
H2O to make 1 liter

Solution B;
Sodium Carbonate 110 grams
H2O to make 1 liter

I've substituted 110 grams of S. CO3 for the 120
grams of P. CO3 in the original formula.

Mix 1:1 and dilute for paper ???
That they don't say. Well, lith is for film is it not?

Those three chemicals will produce lith prints. I concocted
a Wall's similar developer which worked well. If you give Wall's
Normal Hydroquinone a try use it one-shot. I would brew up
a 1/20 batch and test. Only enough sulfite should be used
to preserve the hydroquinone. I think the HQ to CO3
ratio in the ballpark. You may wish to tweak. Dan

 

[slm]

Thanks everyone for the info.

I did add 2 stops more exposure than what was required for development in a normal developer, but it was not in the order of minutes, and the test strip was left in the developer for ~20mins.

Not sure how I will proceed yet, but I'll probably try another formula.

 

[dancqu]

Not sure how I will proceed yet, but I'll
probably try another formula.

Your first Home Brew, D-85. That's jumping in the deep end.
I suspect you committed a lot of chemistry; a live and
learn experience.

I'm a little amused at the fixes suggested for Kodak's D-85.
AFAIK, that formula has been producing a sold dependable lith
developer for 60, 70, maybe 80 years. I did not take note but
in the 50s when doing process camera work and half-tone
production D-85 may have been there.

D-85 is just one of many lith developers. I'm very sure it's
intended use was and is publishing and newspaper plants. One
of many developers intended for that purpose. I can just about
guarantee that EVERY lith formula you look at is intended for
film and LOTS of it.

Your advantage in compounding your own chemistry is one of
batch size. I've a .01 gram Acculab scale. I weigh no amounts
less than 1 gram. Where smaller amounts are called for, stock
or concentrates are used. Perhaps only a few drops of this or
that from a bottle is all that is needed.

Give a one gram HQ Ansco 81 a try. Leave out the citric acid
and the bromide. The citric I think is a many years ago Calgon;
the bromide, to counter the high activity of the developer
and for the films of days gone by.

Tweak the carbonate level and see what happens. If the
developer turns any more than a little yellow while developing,
up the sulfite a bit. I've a very well lighted Graded paper
darkroom. No problem watching the action. Dan

 

[Photo Engineer]

I would like to point out that the last use by EK of Paraformaldehyde was in the E1 stabilizer bath. The results were so variable that it was never used again or recommended in any product.

PE