Amidol/Propylene Glycol and Azo: Initial results

[gainer]

That sounds a bit like what I just tried since my last post only a heck of a lot different, but I used isoascorbic acid instead of hydroquinone and TEA as acivator and no sulfite. It gives warm tones on Arista VC FB paper, but I'm not yet satisfied with the gradations. It may just be a Iittle too soft working. I'll play with it some more.

 

[Tom Hoskinson]

Sounds interesting Pat. Maybe if you added a little carbonate or metaborate to give it a "kick?"

 

[gainer]

My sentiments precisely. I didn't like the carbonate results, but I started over with a mixture of 10 g PAP + 100 g isoascorbic acid in 250 ml of propylene glycol + 250 ml of TEA. Most of it dissolved at about 150 F. Probably a gram of something was left in the pitcher. Used 60 ml of this + 1 tbs borax + 1 tsp of lye in a liter of water. The alkali is not much different from metaborate. This gave nice gradations and a surprisingly warm tone, but too much fog, so I added a pinch of bromide. I like this pretty well, but it really should have another pinch of bromide to keep the edges white.

It doesn't sound very scientific, but after I get it working I can make up a science to go with it, like everybody else. I can weigh my spoonfulls and pinches and have everybody weighing it to the milligram. Of course, I'm just poking fun.

 

[Tom Hoskinson]

Good stuff, Pat! Looks like you are homing in on it.

I ran across another aminophenol formula in Dignan's September 1973 newsletter. This one (The Pain Killer Developer) is from Walter C. Snyder and utilizes 10 500mg Acetaminophen (Tylenol or generic equivalent) tablets. This formula is said to give Rodinal - like results.

Water (100 F) --------------------------------400ml
Acetaminophen ------------------------------ 10 500mg tablets, crushed

On dissolution of the crushed tablets, a white precipitate will form. Do not filter at this time. Cool solution to 70 F and slowly add the following, stirring thoroughly.

Sodium Bisulfite ------------------------------ 30 grams
Sodium Hydroxide (Lye) ----------------------- 25 grams
Potassium Bromide ---------------------------- 6 grams
Edwal Orthazite* ------------------------------- 30ml
Water to -------------------------------------- 500 ml

* I would leave the Orthazite out and add Benzotriazole to the working developer until I like the results.

Filter the solution twice though clean wads of sterile cotton and store in 2 oz amber glass bottles.

To use, dilute the stock solution 1:6 with water. Snyder recommends a developing time of 18 to 20 minutes at 72 F with Kodak Plus X.

Generic Acetaminophen 500mg tablets/caplets are about 2 cents apiece.

 

[juan]

In my Google search for PAP, I noted that Tylenol showed up as a similar chemical. I thought it was nuts to think it could be a developer, so I avoided the embarrassment of suggesting such a fool thing here. Looks like it's not so foolish after all.
juan

 

[gainer]

Now who's on that slippery slope?

From what I have read, including "Theory of the Photographic Process", there are more things in nature that develop film than do not.

 

[sanking]

Now who's on that slippery slope?

From what I have read, including "Theory of the Photographic Process", there are more things in nature that develop film than do not.

Yes, even human urine can reportedely be used to develop film. Anchell and Troop write that pyrocatechin is a constituent of human urine, and continue with this wonderful tongue in cheek statement. "How or why the human body manufacturers pyrocatechin is something we will leave to future generationss of scientists -- or theologians. Perhaps the Creator foresaw a time when developing agents would be in short supply but film would be plentiful?

Sandy

 

[gainer]

I had hoped when I saw that the Tylenol formula gave results like Rodinal that the Tylenol would complete my quest for a grocery store developer. p-aminophenol is synergistic with ascorbic acid, but I haven't had any luck with acetaminophen and ascorbic acid. I should have known that when I saw that the antifog agents outweighed the developing agent.
Maybe I should try hair dye. Some of them contain paraphenylenediamine.

 

[garryl]

Yes, even human urine can reportedely be used to develop film. Anchell and Troop write that pyrocatechin is a constituent of human urine,
Sandy

There was a person on LUG( leica Users Group) that claimed a "Urinol"
formula, with examples of photo done with it, but he never gave up the formula.

 

[Tom Hoskinson]

There was a person on LUG( leica Users Group) that claimed a "Urinol"
formula, with examples of photo done with it, but he never gave up the formula.

I have posted an example of an 8x10 Azo contact print, untoned, developed in Michael Smith's Azo/Amidol formulation. The developer was prepared with my stock concentrate of Amidol in a solution of Propylene Glycol. The concentrate was prepared about 4 weeks before use.

The negative was Efke 100, semi-stand developed in a slosher tray with Pyrocat-HD.

Lens: Barrel mount 305mm Apo Nikkor.
Exposure: 20 seconds at f45 with my Polarfleece Sock Shutter.

 

[sanking]

I have posted an example of an 8x10 Azo contact print, untoned, developed in Michael Smith's Azo/Amidol formulation. The developer was prepared with my stock concentrate of Amidol in a solution of Propylene Glycol. The concentrate was prepared about 4 weeks before use.

The negative was Efke 100, semi-stand developed in a slosher tray with Pyrocat-HD.

Lens: Barrel mount 305mm Apo Nikkor.
Exposure: 20 seconds at f45 with my Polarfleece Sock Shutter.

Tom,

Are you mixing Michael Smith's Amidol formula as a concentrated stock solution and then diluting with water to make the working solution? I have read your previous description of this but am still a bit confused as to exactly how you are mixing the stock and working solutions. I would really appreciate it if you would describe this again as I would like to try this myself as it sounds like a much better way of working than having to mix the developer from scratch every time.

Thanks in advance.


Sandy

 

[Tom Hoskinson]

Tom,

Are you mixing Michael Smith's Amidol formula as a concentrated stock solution and then diluting with water to make the working solution? I have read your previous description of this but am still a bit confused as to exactly how you are mixing the stock and working solutions. I would really appreciate it if you would describe this again as I would like to try this myself as it sounds like a much better way of working than having to mix the developer from scratch every time.

Thanks in advance.


Sandy

Sandy, this formulation has been evolving. Here is my current procedure:

The basic formulation is Michael Smith's Azo contact paper developer formulation, so: 30 grams/liter sodium sulfite, 3 grams/liter citric acid, 2ml 10% KBr/liter. Michael’s Azo formulation calls for 8 grams/liter Amidol.

I have determined that I can dissolve 8 grams of Amidol in 250 ml of Propylene Glycol (PG) at 140 to 160 degrees F. A very small amount of undissolved Amidol debris (typically a fraction of a gram) will be left that will eventually settle to the bottom of the container. This Amidol debris is water-soluble and has not affected the end results with the working developer. I have raised the PG temperature to 250 F and the debris remains insoluble – however, the debris dissolves easily in water at room temperature.

I mix the Amidol stock solution under a vented laboratory hood on a combination hot plate/magnetic stirrer.

MS Amidol Concentrate – Solution A

Propylene Glycol at 160 deg F --------------------------900 ml
Amidol --------------------------------------------------32 grams
Stir until dissolved (some undissolved residue is normal)
Propylene Glycol to -----------------------------------1000 ml

MS Amidol Concentrate – Solution B

Water at 125 deg F -------------------------------------800 ml
Sodium Sulfite ------------------------------------------120 grams
Citric Acid -----------------------------------------------12 grams
10% KBr stock solution ------------------------------------8 ml
Water to ----------------------------------------------1000 ml

For working developer: Mix 1 part A + 1 part B + 2 parts water

 

[Tom Hoskinson]

One additional note. Increasing the amount of PG beyond 30ml PG per gram of Amidol had no apparent affect on the quantity of undissolved residue.

 

[sanking]

Tom,


Is it not possible to mix all of the chemcials in one stock solution? I mean, amidol, bromide, sulfite and citric acid all in the same solution?

Sandy

 

[Tom Hoskinson]

Tom,


Is it not possible to mix all of the chemcials in one stock solution? I mean, amidol, bromide, sulfite and citric acid all in the same solution?

Sandy

Yes, IMO it should be possible to put everything together in a single solution.

I was just taking it one step at a time, to see if an Amidol concentrate was feasible at all.

The obvious next step is to try combining everything into a single solution. I got a bit side tracked in this by investigating the amidol debris residue.

 

[sanking]

Yes, IMO it should be possible to put everything together in a single solution.

I was just taking it one step at a time, to see if an Amidol concentrate was feasible at all.

The obvious next step is to try combining everything into a single solution. I got a bit side tracked in this by investigating the amidol debris residue.

Well, I tried adding all of the chemicals to the glycoal at 250ºF at once, but the result was not satisfactory. Everything appeared to go into solution ok except the sodium sulfite, and it would not go intio solution even after raising the temperature of the solution to over 300ºF.

If it is possible to mix all of the chemicals in one solution the order of mixing would appear to be important.

Sandy

 

[Alex Hawley]

Tom, thank you for doing this research. What would be your recomendation for mixing without having a chemical hood nor a magnetic stirrer?

 

[Tom Hoskinson]

Well, I tried adding all of the chemicals to the glycoal at 250ºF at once, but the result was not satisfactory. Everything appeared to go into solution ok except the sodium sulfite, and it would not go intio solution even after raising the temperature of the solution to over 300ºF.

If it is possible to mix all of the chemicals in one solution the order of mixing would appear to be important.

Sandy

Looking over my notes, I see that back in June I was exploring percentage solutions as part of looking at the MS Amidol formulation.

"...prepared percentage solutions of KBr, sodium sulfite, sodium metabisulfite and citric acid in propylene glycol. KBr dissolves in Propylene Glycol around 230F. Sulfite (and metabisulfite) dissolve around 250F. Citric acid dissolves around 235F..."

I apparently abandoned the effort because I was concerned that the high mixing temperatures might adversely affect the Amidol (based on anecdotal information).

Now, I have experimental data that shows Amidol/PG can indeed survive high mixing temperatures (at least 260 F) with no apparent damage.

I'll head over to the lab and see if any of these percentage solutions still exist (and what the percentage is).

In any case, I can attempt to dissolve the chemicals in the following sequence:

Propylene Glycol at 260 deg F 200 ml
Sodium Sulfite 30 grams
Citric Acid 3 grams
KBr 0.2 grams
Amidol 8 grams

I'll post the results.

 

[Tom Hoskinson]

I tried dissolving 30 grams of sodium sulfite in 200ml of hot PG. Bottom line, sulfite is only slightly soluble in PG. I got maybe half of it or a little less into solution and I ended up at 340 deg. F. The solution started changing color around 320 F - it turned a dirty amber color. I dumped it and tried again.

On the second try, I dissolved 3 grams of Citric acid and 0.2 grams of KBr in 100ml of hot PG (it dissolved around 160 F). I kept heating the solution (with continuous stirring) and when the solution temperature reached 260 F I slowly added 8 grams of sulfite - but only about half of it dissolved. I dumped that, as well.

On my third attempt, I dissolved 3 grams of Citric acid and 0.2 grams of KBr in 100ml of hot (160F) PG, then added another 130ml of PG to the mix and when the solution temperature reached 160 F again, I slowly added 8 grams of Amidol. By the time the solution reached 190 F, most of the Amidol had dissolved. I continued heating and stirring until the solution reached 260 F. At that point a little Amidol debris remained.

I will add the sulfite when I mix the working developer.

 

[Tom Hoskinson]

Tom, thank you for doing this research. What would be your recomendation for mixing without having a chemical hood nor a magnetic stirrer?

Alex, I would probably emulate Pat Gainer and heat the PG with a microwave oven (in a Pyrex beaker or measuring cup). A mixing or stirring paddle should work ok. I would choose a well ventilated, but not breezy place to do the mixing - and high humidity to keep the dust down. Then I would put on a respirator mask and my Nitrile gloves, measure and stir in the Amidol. Once the Amidol is in solution, the inhalation hazard is mostly mitigated. However, you still need to keep the solution away from exposed skin and eyes.

For cleaning trays and utensils use diswashing detergent (that will oxidize the amidol) and plenty of water to dilute, oxidize and get rid of the amidol its oxidation products (which will stain).

 

[Alex Hawley]

Thanks Tom. Sounds like it should work.