Developing really, really old (but kept frozen) Plus-X and Tri-X

PhilBurton · Jun 16, 2020

So "life happened" and I never did process all the Plus-X and Tri-X that i exposed on a cross-country trip in the late 1970s. About 65 rolls in all. I was quite surprised when I counted up all the rolls recently. If I could have built a darkroom in this house, I would have done it years ago but ....

Fortunately the film has been kept frozen all this time but my "chief operating officer" wants the freezer space back. I used to do all my own B&W, which I bulk-loaded. I still have my Nikor tank with 2 35 mm reels, changing bag, thermometers, beakers, drying clips, etc. So I need some good advice on how to process this film. I remember the basic steps, which 40 years ago were:

Developer
Stop Bath (Kodak Indicator)
Fix 1
Fix 2
wash
Photo Flo
Dry overnight

My big uncertainty is the choice of developer and time/temp. Years ago, I used to use 1:15 Edwal FG-7, but that's no longer available, and I'm not sure if that would even be the best choice. I would prefer one-shot use developer, because I want to keep the workflow simple. I'm just trying to get negatives with decent tonal range.

I also still have my old Watson (or Lloyds - can't remember which) bulk-loader because once I get all this backlog of film processed, I want to start shooting Tri-X or maybe some Ilford equivalent again.

Thanks for helping out an "old timer" here.

Bill Burk · Jun 16, 2020

D-76 1:1 develop for a certain amount of time, start with spec sheets But probably 11 minutes for Plus-X and 13 minutes for Tri-X. Rinse or stop for about a minute and then Fix for twice the time it takes to clear. Use fresh fix this isn’t like a print you can toss in the trash. Wash at least 20 minutes but listen to the experts. Then in some filtered water add some wetting agent like Photo-Flo. I use about 1:100 in a tray and glide the film through like a see-saw and hang to dry without touching it. Let the water drip off naturally

Michael Teresko · Jun 16, 2020

I went through this with a bunch of rolls i shot in the late 70s and early 80s. Expect a lot of base fog and grain. I tried several developers (Rodinol, caffenol, HC-110, pyrocat-hd). Rodinal semi-stand developing works great if you don't mind a lot of grain. It's convenient because time and temp are not super critical. If I were doing it again, I would try Xtol, which is a great developer for most any film, plus it results in much finer grain than Rodinal, and it has a relatively low toxicity. Dilute the stock 1:1 or 1:2 and use it as a one shot developer. D-76 is probably a good choice also. I prefer to just use 2-3 exchanges of tap water at developing temp (usually 20C) instead of a stop bath, and fix with TF-4 (available from Photographers Formulary), which washes out very quickly. I then do a final rinse with distilled water with a couple of drops of PhotoFlo or an equivalent. Let hang and drip dry.

This shot was from the early 80s and developed in 2018. It's TriX developed in caffenol for 75 minutes with a couple of inversions every 30 minutes

Fort Ontario by Michael Teresko, on Flickr

jimjm · Jun 16, 2020

Like Bill said, I'd use D-76 1:1 as a one-shot developer. Mix up a few gallons of stock solution and that should handle most of your backlog. Maybe 10-20% extended developing time over the normal recommendation.
I can't see that you'd need a second fixing bath, a hypo-clear bath for 2 or 3 mins before your final wash is a good idea. Start with fresh fixer (fix for at least 2x the clearing time) and you can re-use it until your clearing time gets longer than 5 mins. Then dump it and start with a fresh batch.
Final wash of at least 10 mins and then a 30-sec immersion in Photo-flo before hanging to dry.
I just processed a 30-year old roll of HP5 that I recently shot, using the above process and I got good results.This film was not refrigerated. Certainly some base fog was present, but the negatives were very easy to print in the darkroom, just needed extended print times.
Good Luck!

Raghu Kuvempunagar · Jun 16, 2020

If you don't mind sacrificing one or two rolls from the bunch, you can do a bit of experimentation with small strips of film, evaluate the results and take an informed decision on how to develop the rest of the rolls.

Randy Stewart · Jun 16, 2020

I'll "third" the advice of Bill and imjm above, except as to Photo-flo. The Kodak dilution from stock to use solution is 1:200, and many including me find that 1:400 works as well or better. Truly a situation where "less is more". Using Photo-flo in higher concentration leads to delayed drying and if much to concentrated, some scumming on your film. Take care to adjust your process to a fixed developing temperature and vary your time a bit as you go if you need to improve your contrast. Frankly, developing 65 rolls of 35mm, 2 rolls at a time, would drive me nuts.

Sirius Glass · Jun 16, 2020

I have had great results with XTOL and replenished XTOL for Tri-X 400. It has time and temperature for Plus-X.

PhilBurton · Jun 16, 2020

Randy Stewart said:
I'll "third" the advice of Bill and imjm above, except as to Photo-flo. The Kodak dilution from stock to use solution is 1:200, and many including me find that 1:400 works as well or better. Truly a situation where "less is more". Using Photo-flo in higher concentration leads to delayed drying and if much to concentrated, some scumming on your film. Take care to adjust your process to a fixed developing temperature and vary your time a bit as you go if you need to improve your contrast. Frankly, developing 65 rolls of 35mm, 2 rolls at a time, would drive me nuts.

Agreed, but (1) I'm motivated, and (2) my "chief operating officer" will be pleased. If I do two rolls every other day, that's two months, which IS a lot. But that way, I'll be sure that if I mix up any stock solutions, it will still be fresh when I finish my backlog. Of course, then I'm probably going to be tempted to drag out my old Nikon F2's again. All I need is fresh batteries for the light meters, but that's a separate topic.

PhilBurton · Jun 16, 2020

Sirius Glass said:
I have had great results with XTOL and replenished XTOL for Tri-X 400. It has time and temperature for Plus-X.

View attachment 248502

First of all, thank you all for these suggestions.

In my OP, I mentioned using two fixer baths. I remember reading (in Popular Photography?) that Fixer1 is already partially used, and Fixer 2 is fresh. Once Fixer 1 gets to a certain point, you get rid of it, Fixer 2 becomes Fixer 1, and you start a new Fixer 2. Is that considered a "best practice" or just something a long-ago writer wrote to fill up some column-inches?

I do remember HC-110 but not Xtol. This chart is extremely useful to me. Allow me to explain. On this cross-country trip, I did general photography with Kodachrome (in one F2 body) and black and white (in the second F2 body). The B&W is mostly railroads. I am a railroad hobbyist, a/k/a railways enthusiast, a/k/a un passionné de chemins de fer.

The railroads in the US today are quite different than they were back then, and I distinctly remember photographing some lines (The Milwaukee Road) that were subsequently abandoned and torn up. Detail in rail photos is important. So acutance is important, but so is shadow detail. So I have to do some thinking and research here. Again, I want to thank everyone who responded.

Michael Teresko · Jun 16, 2020

PhilBurton said:
First of all, thank you all for these suggestions.

In my OP, I mentioned using two fixer baths. I remember reading (in Popular Photography?) that Fixer1 is already partially used, and Fixer 2 is fresh. Once Fixer 1 gets to a certain point, you get rid of it, Fixer 2 becomes Fixer 1, and you start a new Fixer 2. Is that considered a "best practice" or just something a long-ago writer wrote to fill up some column-inches?

I've never used more than one fixing bath, and have negatives that are pushing 50 years old that look fine. Seems unnecessary to me...

Alice Quarterman · Jun 16, 2020

Ilford describes two bath fixing as ‘extremely efficient’. I’m not sure if it’s considered best practice but it will make your supply of fixer last longer.

Patrick Robert James · Jun 16, 2020

Rodinal is a great low fog developer for old film. That would be my recommendation based on experience with older film. Not sure what to tell you though because in all the years I've been doing photography, I've never heard anyone try to develop a 40+ year old frozen latent image. I could give you some guesses, but they would just be guesses. I don't like to guess giving people advice.

Good luck. Hope you post the images here too. Really interested to see how it works out for you.

MattKing · Jun 16, 2020

Alice Quarterman said:
Ilford describes two bath fixing as ‘extremely efficient’. I’m not sure if it’s considered best practice but it will make your supply of fixer last longer.

Efficiency might be a really good idea if you need to develop 65 rolls.
I'll post my link here for what I do with one bottle of fixer in my space constrained area - if you use two bottles, it should work even better: https://www.photrio.com/forum/resou...ixing-procedure-for-black-white-negatives.75/
If I had a 65 roll backlog, I would get out my larger tanks and extra reels!
If you were nearby, I would lend you some!

Bud Hamblen · Jun 16, 2020

Kodak developing times for Plus-X have changed over the years. In 1959, Kodak recommended for Plus-X a time of 8 minutes at 68F with D-76 (1:1) and intermittent agitation, but in 2002 the recommendation was for 7 minutes. Why and when the change occurred, I know not. Tri-X times also have changed, but I can't lay my hands on old Tri-X data sheets right now.

MattKing · Jun 16, 2020

I have a few sources for recommended development for a few versions of Plus-X with a variety of develop-before dates. Can you identify what versions of the films you have (the names and badging are clues) and what their dates are?

grainyvision · Jun 17, 2020

No idea on the Tri-X, but I received some similar vintage Plus-X that I believe had either been kept cold or frozen since purchase, expiration is 1960s. There is a slight bit of fogging, but it's usable at box speed for my batch (1/2 stop over exposed would probably be better to lower visible grain). I use a custom developer mostly, but in testing I used D-76 1+1 with the time listed on massive dev chart. The emulsion is a lot softer than modern films so be careful in handling and make sure to not use any hot water for rinsing and such.. but otherwise processed great with no problems. I have no idea on how well the latent image would hold up over such a long time though

edit: I believe I used 8.5m in D-76 1+1, adjusted slightly for a room temp of 72F

edit2: I also use TF-4 fixer. The emulsion is soft after final rinsing, but not so soft that I felt a hardener was needed. After drying it seems fairly sturdy

DREW WILEY · Jun 17, 2020

Old film risks emulsion frilling, so keep both your dev and wash temps standard at 20C (68F), and not excessively warm, and use a somewhat weak stop bath (around 1/2% acetic).

PhilBurton · Jun 17, 2020

DREW WILEY said:
Old film risks emulsion frilling, so keep both your dev and wash temps standard at 20C (68F), and not excessively warm, and use a somewhat weak stop bath (around 1/2% acetic).

This advice really, really appreciated. Those photos from 1976 are scenes that simply don't exist any more.
What is the out of the bottle % of acetic acid? I assume that I will need to dilute the stop bath.

grainyvision · Jun 17, 2020

PhilBurton said:
This advice really, really appreciated. Those photos from 1976 are scenes that simply don't exist any more.
What is the out of the bottle % of acetic acid? I assume that I will need to dilute the stop bath.

Alternatively don't use stop bath and instead use a water rinse. Otherwise though if you insist, you could just dilute standard household vinegar (3% acetic acid) 1+4 or so

DREW WILEY · Jun 17, 2020

Actual glacial acetic acid is pure, and a 1/2 or 1/4 percent solution of that would be appropriate. But most photographers buy safer 28% instead, then dilute that down. If you use the tinted 28% Indicator Stop Bath, simply dilute it down to a rather pale yellowish urine color. It's cheap enough that way to use one-shot, but changes color to purple anyway when exhausted. I routinely use TF4 Archival Fix; and in your case the advantage of it would be shorter fixing and rinse times. It should be used one-shot. Long soaks are the enemy with old film, along with thermal shock from solution being too hot or too cold, or too different in temp in between.

Developing really, really old (but kept frozen) Plus-X and Tri-X

PhilBurton

Bill Burk

Michael Teresko

jimjm

Raghu Kuvempunagar

Randy Stewart

Sirius Glass

PhilBurton

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Alice Quarterman

Patrick Robert James

MattKing

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Bud Hamblen

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DREW WILEY

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Developing really, really old (but kept frozen) Plus-X and Tri-X

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