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  #1  
Old 10th August 2020, 02:53 PM
Terry S Terry S is offline
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Default Home mixed D76 / ID11 died on me. Is my metol dead?

Recently, I've started to return to having a go at mixing my own formulas, using ones widely available and so tried and trusted.

So far I have tried D72 print developer, teaspoon formula, which worked very well and lasted for ages in my Nova slot processor. It only let me down on one brand of paper, with all of Ilford's and other brands papers working fine, including some from the 1980's. (I made a separate post about this so won't say any more.)

I then had a go at mixing another teaspoon formula, of D76 / ID11. The first test film put through it at 1 + 1 was fine and as expected, so I was very happy. BUT, just a few days later I did another test film using more of the made developer at 1 + 1, and it came out VERY, VERY thin. I think I might JUST get a print out if I use grade 5.

I thought about ditching it and making up some more of the same but then read that Phenidone could be used instead of Metol, at 10% i.e. 0.2 gram of P, rather than 2.0 grammes of M. As I had this available, I gave it a go.

So far, I have only put a few drops of both on two separate 35mm film leaders. The Phenidone version went black in a minute or so. The Metol formula did nothing, even after leaving it a while longer.

From this I can only deduce that the Metol version has died on me. I thought it could be the Metol that had died on me somehow, having done a bit of reading about its properties, but then why would it develop one film fine and then not the second one, not long after? And why did the print developer last for over two months and was still okay, when it too had some Metol in it?

Does anyone have any suggestions or has anyone had this happen to them before, especially when mixing ones own from scratch?

ID11 / D76 formula: http://www.afterness.com/kod_d76.html

D72 formula: http://www.afterness.com/kod_d72.html

Terry S
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  #2  
Old 10th August 2020, 05:55 PM
John King John King is offline
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Something has not gone correctly. I have used ID11 and D76 which has been made up and part used leaving a part empty bottle even when it was 8 months old.
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Old 10th August 2020, 07:06 PM
Svend Svend is offline
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Hi Terry,
Sorry to hear about your trouble. As John said, something is not right. There could be a number of things that went awry. If you don't mind, could I ask a few more background questions?

What colour is your metol powder? If brownish I believe it has gone off and oxidized. It should be a pale off-white.

Was there any colour change in your stock solution from first to second film? As above, if it's brownish then it's gone. This would be unusual after a short storage period, as D76 stock lasts quite a long time (more than 6 months for me, in full airtight bottles). How old was your stock?

Are you certain of the proportions that you used? Did you perhaps inadvertently add too little sulphite (being a preservative)?

Is there any sediment or undissolved chemical in the bottom of your bottles? Perhaps incomplete mixing/dissolving occurred.

Do you use dedicated and separate developer and fixer stock sol'n bottles? Perhaps the D76 was put into an old fixer bottle containing a bit of residual.

Did you use the D76 as one-shot diluted or full-strength? If full-strength, then as above, could there have been some residual fixer in the tank from the first roll that weakened the stock?

Please don't think I am suggesting sloppy habits, but I'm merely trying to find out what could be the problem. Metol is quite long-lasting as a powder and I would find it highly unusual that it had died. I have used decades-old (like 1970s and '80s) ID-11 and D76 powder and they have worked perfectly (given that their pouches remained airtight! I have tossed some old powders that had an air leak in the pouch and turned brown).

As an aside, a really great tip that Ian Grant mentioned to me here was to add a pinch of sulphite to the water before adding any other chemicals in order to scavenge the oxygen out of the water and prevent premature oxidation. Makes the stock last much longer apparently. If your water was highly aerated then that could have been a factor.

Speaking of water, how's the water quality out of your tap? Suitable for photo chemical mixing?

Sorry for all the questions. Hope we can find a cause and cure here. :-)
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Old 11th August 2020, 02:26 PM
Lostlabours Lostlabours is online now
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Metol keeps for decades in a closed jar, it shouldn't go off, same with Hydroquinone.

I made up some Ilford ID-3 (D165 - Selectol Soft) this Spring with Metol made in the early 1960's and it works fine.

If the Metol has gone off you'll see a colour when you mix it up. Here's the PQ versions of ID-11

As Svend mentions adding some Sulphite first prevents oxidation.

Ian
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Old 12th August 2020, 01:09 PM
Terry S Terry S is offline
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Thanks for replying in full Svend, and no, there's definitely not too many questions if it helps me to find the solution to my problem.

So, I will now reply to each of your questions, one at a time.

What colour is your metol powder? If brownish I believe it has gone off and oxidized. It should be a pale off-white.
I've checked the metol and yes I would say just off white, as you say.

Was there any colour change in your stock solution from first to second film? As above, if it's brownish then it's gone. How old was your stock?
No, there was no colour change in the stock solution, which was only a few days old, between developing the first film and the second one.

Are you certain of the proportions that you used? Did you perhaps inadvertently add too little sulphite (being a preservative)?
As far as I remember I added exactly the recommended portions of all the various chemicals, including the sulphite.

Is there any sediment or undissolved chemical in the bottom of your bottles? Perhaps incomplete mixing/dissolving occurred.
No, there is no sediment at the bottom of the bottle. Everything was mixed until dissolved.

Do you use dedicated and separate developer and fixer stock sol'n bottles? Perhaps the D76 was put into an old fixer bottle containing a bit of residual.
I always try to use bottles that have had the same solution in before.

Did you use the D76 as one-shot diluted or full-strength? If full-strength, then as above, could there have been some residual fixer in the tank from the first roll that weakened the stock?
I used the developer at 1:1 and EVERYTHING I use during a session is heavily washed at the end in clean water.

...a really great tip... was to add a pinch of sulphite to the water before adding any other chemicals in order to scavenge the oxygen out of the water and prevent premature oxidation.
This is mentioned in all the formulas I've read, so I mix in a good pinch of sulphite first.

Speaking of water, how's the water quality out of your tap? Suitable for photo chemical mixing?
I filter all of the water that comes out of the tap and I've never had any problems before with any other chemical solutions that I've mixed up, apart from a bottle of Rodinal that I've mentioned in another post previously.

Quote:
Originally Posted by Lostlabours View Post
Metol keeps for decades in a closed jar, it shouldn't go off, same with Hydroquinone.

I made up some Ilford ID-3 (D165 - Selectol Soft) this Spring with Metol made in the early 1960's and it works fine.

If the Metol has gone off you'll see a colour when you mix it up.[/URL]

Ian

That is what is confusing me Ian. Everything I've read tells me that this shouldn't happen, but as mentioned in a previous post, a brand new bottle of Rodinal also died on me, when I developed the second film with it as well...!?!

What to do next?

Well I made up a new batch of the formula a couple of days ago, but this time I added a reduced portion (10%) of phenidone instead of the metol. As mentioned, a quick film leader test showed it to be active, whilst the first metol formula did nothing.

Yesterday, to see if I maybe did something wrong initially, although I can't imagine what, I carefully made up a fresh version of the teaspoon formula of D76 / ID11 with metol once more. Everything was carefully measured and a BRAND NEW bottle was used to store it in. I will give it a day or two to settle down and then I will do test developments in both the metol and phenidone versions to see what happens.

It's also worth pointing out once more, I think, is that I made some D72 print developer with the same metol, before making the above, and it was still working fine, 6 weeks later, and just before making the above.

I will report back once I have done some more tests, but many thanks for all of the help so far. It's been very much appreciated.

Terry S

Last edited by Terry S; 12th August 2020 at 01:13 PM.
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Old 12th August 2020, 05:34 PM
Svend Svend is offline
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Gee Terry...this is indeed baffling. Since the D72 that you mixed up also contains HQ, it seems we can't blame that chemical for being dead. Your metol sounds like it's OK too.

How about trying another little experiment? Do you have access to a sensitive scale, capable of measuring to within 0.1g? If so, take your teaspoons and tablespoons - the same that you've been using to mix up your formulas - and measure out each ingredient onto the scale and then compare to the recipe to see if the spoons do indeed give you accurate measurements. You might find they are off by quite a bit. Esp. the metol, as it's only 1/2 tsp so easier to get a false measure on such a small amount. I.e. it could be that D76, having smaller quantities of metol and other stuff than D72, is more prone to such measuring error.

Before I started using the teaspoon method, and being a "prove it to me" kind of fellow, I "calibrated" my spoons to a laboratory scale, and found there was quite a variation. Significant adjustment was needed. Well worth doing! Let us know how it goes if you try this.
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Old 12th August 2020, 08:51 PM
Mike O'Pray Mike O'Pray is offline
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Terry, seeing what Svend wrote I have just done a little experiment. My wife has a set of calibrated plastic spoons for baking purposes and I placed the half teaspoon one into sugar. I then drew a knife edge across the spoon to level the sugar and weighed it. it was exactly 2 grams so it would appear that calibrated spoons are pretty accurate. However when I transferred that known 2gms to an ordinary teaspoon I had great difficulty working out if this was half the ordinary teaspoon. I think that had I had to use an ordinary teaspoon that I use the stir my tea I would probably had underestimated what 2 grms were.

Of course the density of metol powder and sugar may mean that volumes for 2grms are a little bit different but probably not much

So if you are using calibrated half teaspoon measures then I think you will have an accurate measure but "by eye" I would have underestimated the amount

That leaves the question of how much of a safety margin is built in to 2 grams and this I don't know but suffice it to say that my estimate of half a teaspoon by using an ordinary teaspoon would have been wrong by maybe 0. 2- 0.3 grams

Mike
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Old 13th August 2020, 11:22 AM
Terry S Terry S is offline
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Thanks again Svend and Mike.

I do use a set of calibrated stainless steel spoons for my chemical measuring, and they are kept away from another set for use in the kitchen only.

When I get a mo, I'll try measuring all the chemicals in the formula with the spoons and then weigh the chemicals on a sensitive set of scales that I've also got, and see if the amounts differ at all.

What ever happens, I don't understand why the first film would come out fine and then the second one, developed only a day or two later, came out so thin? And of course the same happening to a new bottle of Rodinal?

I'll update when done.

Terry S
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Old 13th August 2020, 12:39 PM
Svend Svend is offline
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Quote:
Originally Posted by Terry S View Post
What ever happens, I don't understand why the first film would come out fine and then the second one, developed only a day or two later, came out so thin? And of course the same happening to a new bottle of Rodinal?

That is indeed puzzling Terry. I'm scratching my head on this one. If you hadn't done the leader test I would say to look at your camera. Is there anything unusual about the films you're using? Odd brand? Ancient stock? Hot storage? Did you use the same film for the first roll and the second? (Just trying to see if there are other variables at work here)

The fact that two stable, reliable developers have had a sudden death fate is very strange. If this were Xtol, well, that's a different story, but Rodinal and D76....very odd.

Let us know how your teaspoon measures compare to the weighed values. That seems the most likely culprit at the moment (in the absence of any other brilliant ideas )
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Old 13th August 2020, 06:26 PM
Mike O'Pray Mike O'Pray is offline
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Quote:
Originally Posted by Terry S View Post
Thanks again Svend and Mike.

I do use a set of calibrated stainless steel spoons for my chemical measuring, and they are kept away from another set for use in the kitchen only.

When I get a mo, I'll try measuring all the chemicals in the formula with the spoons and then weigh the chemicals on a sensitive set of scales that I've also got, and see if the amounts differ at all.

What ever happens, I don't understand why the first film would come out fine and then the second one, developed only a day or two later, came out so thin? And of course the same happening to a new bottle of Rodinal?

I'll update when done.

Terry S
Terry have you kept both films' leaders and if so is there any discernible difference in them using the light bulb test I mentioned or if you don't have a clear bulb then looking through a window to see if the same scene is darker or lighter? If this is the case then it has to be down to the developer for reasons as yet unspecified would seem but if both are equally dark then all I can then think of is camera fault.

So is there any chance that the same developer worked equally well but for whatever no developer reason one film is just thinner than the other due to camera maladjustment/fault ? If it was the same camera then I admit that unless the camera's metering and /or shutter or aperture adjustment has suddenly gone wrong this seems unlikely and yet we are heading close to the cause being unknown "gremlins"

Mike
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