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09-08-2021, 01:22 AM   #1
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ID-11: Degradation Indication?

Hello all,

Can anyone tell me, please, what the subjective effect of degraded ID-11 is, and whether it degrades suddenly without warning or there's a gradual breakdown? I've been using a 5 litre batch I made up around January this year and which I'd stored in brim-full Bailey's Irish Cream bottles (black-dark opaque glass), sealed with clingfilm, prior to decanting into 500ml dark brown medicine bottles for ready use. I'm aware that perhaps six-months in sealed conditions with airtight bottles is about the theoretical limit for storage.

All has been well until maybe a few weeks ago, and all might be well now, but the last roll of TMax 400 I developed seems a bit 'noisier' than previous rolls. I'm trying to establish whether this is down to the lens on the Minolta SR-1V (Rokkor 55mm 51.7 MC, about f4 because of poor light and high shutter speed needed) I used, or the developer. The last roll of TMax 400 I shot was with my Pentax K1000 and a 50mm f2 PK SMC lens, and it wasn't as noisy.

Development times and temps were identical, as was the method of copying the negs.

All advice appreciated!
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09-08-2021, 08:42 AM   #2
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I don't see why the characteristics of the developer would change dramatically when crossing a certain threshold of storage time. The developer can though go bad quickly if it is contaminated. The fixer will destroy the developer, even only tiny amounts. Don't know if that could have caused the 'noise' that you see. Switching lenses should not have any effect on noise but since you also switched cameras it is possible that they are exposing differently. Underexposure will give you noisy and washed out negatives. You should be able to tell by looking at the negatives. If the negatives from the two cameras differ significantly then that indicates a problem.
09-08-2021, 08:47 AM - 1 Like   #3
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Hi Russell,
I have used ID-11 stored in full sealed bottles up to 8 to 10 months, and maybe longer, without issues. It lasts longer than Ilford says in their literature. What I always do as a matter of routine practice in such a case where the developer (or fixer) is getting near the end of it's ideal lifespan, is a clip test. If you're not familiar with this, it is basically using the leader from your roll that you clipped off before loading your reel to test developer activity. It works like this: dispense a small amount of your stock solution into a little dish, and in full daylight drop your bit of film into the developer; swish it around every now and then to "agitate" and wait to see what happens. If the developer is still good and active it should turn fully black in about 4 to 5 minutes, or less. If it takes a lot longer, the developer is done. This whole thing takes almost no time at all, and you can use that 5 minutes to get other prep done for the developing session. Make it a habit, and you will always be confident that your chemicals are good and you won't ruin a film that you worked so hard to shoot. There's a clip test for fixers too, which you can do a web search on -- works almost the same way, but in reverse -- the film gets clear. Highly recommended practice for both!

As for "noise", what you really mean is film grain. There are several causes for grain increase, so it's hard to advise what caused yours. It's possible that if your temps of all solutions was variable, then reticulation may have happened from temperature shock. Reticulation can have the appearance of film grain. Are you careful to keep all temps consistent, say within 1 deg. C? That is, developer>stop>fixer>rinse water? You really want to keep these all the same.

Hope this helps. Any more questions, ask away...

EDIT: to answer your initial question, I am not aware of stale ID-11 causing a grain increase. You will see reduced contrast and overall thin negs (assuming that the film was properly exposed). Also, ID-11 does not suffer a sudden death like, say, X-tol. It is more of a gradual degradation of activity.

Last edited by Viking42; 09-08-2021 at 09:02 AM.
09-08-2021, 11:45 AM   #4
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Gylfimag and Viking42... Many thanks for the replies; appreciated. Both negs ( shot on Minolta and K1000) appear similar, if a little yellowy-brown, when placed over newsprint - my quick density test to see how the newsprint appears through the dark pats of the neg - but yes: exposures from each camera quite different. The Minolta pic was taken on a dull, grey day and the K1000 in sunshine with some clouds. I appreciate that I'm not comparing like-with-like here!

My temps were consistent each time and fixer, stop and rinse never deviated more than one degree c from 20C. I've used a clip-test for fixer but never for developer, and that's a useful thing to know: thanks for that. I've about 700ml if ID-11 to use up before I mix another batch! Thanks also for the ID-11 degradation info. Yes, I've heard that Xtol can go 'just like that'.

I believe that TMax 400 can degrade fixer rather quickly too. Attached are two pics. The steam train was shot on the Minolta at f4 1/500 sec and the the diesel train shot on the K1000 about f11 1/250. I copy the negs with a Canon EOS 5D and an Elicar slide duplicator from the 1980s, face down on a fluorescent light box.




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09-08-2021, 01:11 PM   #5
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Good to hear that you're on top of the temperature control. Very important, that.

As gylfimag mentioned, underexposure does cause increased grain. If you suspect one camera is underexposing consistently, you might do a side my side meter test first to see if they agree on the same scenes. If yes, then the shutters or lenses may have some variation. Next step is to put the same film in each camera and shoot a couple of the same scenes with each using the exact same shutter/aperture combination, then develop in the same tank. If the negs show different densities then one camera is off.

Re. fixing Tmax films, sorry to ask what may seem an obvious question, but were you aware that they require longer fixing times than traditional grain films like TriX or FP4? About 50% longer if I recall. Ilford's Delta films are likewise. Again, apologies if I'm stating the obvious...
09-08-2021, 02:15 PM   #6
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I develop for 10 mins and 15 seconds and I fix for maybe seven minutes. I wash for longer too; a combination of maybe five minutes running water followed by the 'Ilford' 5 then 10 then 20 agitations way. When I first developed a TMax 400 film the negs were very yellowy-brown indeed as I didn't appreciate the extended fix! Am I correct in thinking that you can't over-fix? I should maybe increase the fix time for TMax. I've developed Delta 400 before at maybe six minutes without any issues. I just use Ilford rapid fixer.

Exposure... My Minolta hasn't a meter, and I was using my old Weston Master III which compares favourably with my Pentax MX 'reference'. as well as the K1000 match-needle. That said, I haven't tried comparing in all lights. Trouble with the Weston Master being that I have to go to the nearest aperture / shutter setting if between, and I tend to go over-exposed rather than under by maybe half a stop. I like the idea of comparing films side-by-side, so I'll do that at some point.
09-09-2021, 06:14 AM   #7
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Hi Russell,

It is possible to overfix, but it would take a lot longer than 7 minutes. Your times seem about right, assuming fixer is fresh and fully active. Rule of thumb for your fixer clip test is to leave your film in the fixer for twice as long as the clip test takes to clear. So your clip test tells you a lot, esp. for older batches that you've run a few films through already.

I'm not sure what would cause your negs to come out yellow-brown. Sounds like this is only with Tmax(?). I've never had that happen before. How's the water quality in your area? You mentioned this happened with your last film, which was done in aged ID-11...how's the colour of the developer? Is it starting to turn darker brown? That's another sign the brew is starting to kip -- ID-11 oxidizes to brownish colour.

09-09-2021, 08:15 AM   #8
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Hi Viking42,

Thanks for the reply, and the over-fixing info. My fixer had done maybe sixteen assorted films, of which three were TMax 400, the rest being Kentmere 100 and HP5+, and a couple of Rollei Retro 400s. I didn't do a clip-test, but I just made up a new batch (damn the expense...). I use unfiltered tap-water and it is reasonably soft, as we don't get scaling-up of kettles, etc... and I use a container of recently boiled water for the final rinse and the rinse-aid. I have, in the past, just used tap-water for the final rinse and not noticed any difference. Kodak TMax 400 is the only film I've developed that results in yellowy-brown negs. I don't know if boiling the water beforehand and letting it cool removes many of the impurities but I kid myself it does.

My ID-11 is clear with no discolouration, and the only untoward thing I've seen is a very, very minor build-up of white crud around the threads of the brown bottles into which I decant my developer for ready use. But this doesn't reflect on the efficacy of the developer that I can see.

I think in the future I'll make more use of clip-tests for both developer and fixer.
09-09-2021, 08:37 AM   #9
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Looks like your film count is within the recommended capacity of 24 films. Here is the Rapid fixer tech sheet:
https://www.ilfordphoto.com/amfile/file/download/file/1833/product/711/

You mention using a stop bath, so you're not carrying over any developer to the fixer, which is good. You might try fixing that film again in the fresh brew and see if it clears the brown stain away....can't hurt to try it.

Best of luck with this. Post back here if you find out any cause for the graininess and brown staining. And yes, do the clip tests!
09-09-2021, 09:45 AM   #10
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Another quick question: it looks like you're using ID-11 in a one-shot diluted manner, rather than developing in the stock solution....so what dilution are you using? From your dev. times it sounds like 1+1, but I just wanted to confirm. Reason for the question is that 1+3 can often result in underdeveloped negs, as the small amount of stock in the tank exhausts rather quickly. I used 1+3 for a while for economy reasons, but found my negs lacked contrast and punch...no guts, all grey and blah. Going to 1+1 solved that and I get great results.
09-09-2021, 01:06 PM   #11
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Thanks for the advice, Viking42. I'll put a strip of film in the tank and re-fix, see what happens. The yellowing can't be a developer issue in any case as I developed my last-but-one TMax 400 in Rodinal (1+50) and it, too, had a yellowy tint to the negs. I've done a couple of TMax 400s in Rodinal and I don't dislike it.

Yes, I use 1+1 when I do ID-11. When I used to buy the powder in 1 litre quantities I'd do 1+1 on 35mm and 1+3 on 120 roll film to eke it out a bit. But buying the stuff in quantities sufficient to make 5 litres is way cheaper, so I just use 1+1 for all fims now. I've never tried stock solution, but I have tried D-76 1+1 and, apart from some minor variations in dev times for a couple of films, it's identical - and easier to mix.

I've tried with and without stop-bath - rinsing under continuous running water for two mins - but I went back to stop-bath. I didn't notice any difference in the finished negs, but decided stop-bath was more consistent and not subject to the upstairs bath being run affecting the water tap temperature at the kitchen sink where I work!
09-09-2021, 01:57 PM   #12
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Hope the refixing works. Let me know the outcome of that. If you're still stumped as to cause of yellowed negs, I can ask on a film users group that I belong to. I'm really curious now...

Yeah, Tmax in Rodinal is a great combo. I ran a bunch of rolls of 400 in it at 1+50 and really liked it. Pretty punchy tones, and very sharp! I may go back to it after trying it in D76 for the last few rolls.
09-09-2021, 07:22 PM   #13
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Just an aside: I don't know if this was ever confirmed, but there was a rumor going around in the early 1970s that the sulfite in D-76 (and therefore in ID-11) reacted (very) slowly with I think it was the hydroquinone. The product would presumably be a weaker developer than hydroquinone itself. This is chemically plausible but it must happen at either a very slow rate (months) or be very storage temperature dependent. Keep ID-11 stock cool and in a full bottle and it definitely will keep for many months.
09-10-2021, 05:38 AM   #14
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QuoteOriginally posted by Sholom Quote
Just an aside: I don't know if this was ever confirmed, but there was a rumor going around in the early 1970s that the sulfite in D-76 (and therefore in ID-11) reacted (very) slowly with I think it was the hydroquinone. The product would presumably be a weaker developer than hydroquinone itself. This is chemically plausible but it must happen at either a very slow rate (months) or be very storage temperature dependent. Keep ID-11 stock cool and in a full bottle and it definitely will keep for many months.

There seems to be some truth to that, but it's actually the reverse of getting weaker - it appears that ID11/D76 get more active as they oxidize over time. There is a lot of anecdotal evidence, and maybe empirical too, to back this up. I belong to a UK-based film users forum, and the chem gurus there all say this is true. Apparently in less than full bottles the stock solution oxidizes and causes the HQ to gain activity. Counterintuitive, I know, but there it is. A web search will bring up lots of threads in the fora on this topic. Kept in full bottles this doesn't happen, so keep 'em topped up folks :-)
09-10-2021, 11:00 AM   #15
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Thanks each. I understand ID-11 degrades from the minute it is mixed! I keep my four 1-litre Bailey's bottles brim-full and sealed, and the remaining one litre goes into my sealed-stoppered brown medicine bottles: all are stored around 18 Celsius. The 500ml bottles may be partially full at times but certainly not for months on end. Not with 1+1 anyway!

Haven't had to resort to marbles in the bottles yet but I did buy some of those inert 'baking beans' with a view to doing so, should the need arise.
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