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Trouble washing negatives


Xícara de Café

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Dear darkroom doctors,

I've been having ongoing issues with my negatives not washing properly, ie. having signs of residues or -- and perhaps this is another issue -- having blotchy  regions, especially apparent in uniform regions without much detail.

I've been trying various things. On my last roll of film, which I developed as usual in a Paterson tank, i used a real acidic stop bath (a solution using alcohol vinegar) rather than water and a hypo clearing agent (a fresh solution using sodium sulfite). Most of the roll was good, but on the following uninteresting shot you can see the type of blotching that I'm talking about:

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I developed the neg with Kodak D-76 for the required time (11 min for Ilford Delta 100 @ 20 degrees C), then added the stop bath for 30 seconds, then fixed for 10 minutes with standard Kodak fixer (perhaps too long? i was worried the fixer was getting old). I then washed the neg for 5 minutes under running water with just the spool in the open tank, bathed it for 5 min in the sodium sulfite solution, then washed for a further 5. Further, I gave 40 rotations of the tank (a la a partial Ilford method) in carbon filtered water. Then a minute to soak in a second bath of filtered water with a few drops of dish washing detergent.

Any ideas where I might me going wrong? This is the first time that I've used an acidic stop bath with film and the first time I've used sodium sulfite. The result above is however fairly typical of other poor results that I've had in the past. Perhaps I should wash for longer but our water bills are huge.... I can't yet connect a hose to the tap in my darkroom (a bathroom) but will be doing that in the future so I can use the A. Adams method of forcing the water up from the bottom of the tank, rather than having running water entering from the top. I guess it could be the dish washing detergent, but i don't know.

Any advice here most welcome!

Thank you,

 

 

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Since getting back into the darkroom some years back, I've had no issues using the "Ilford" method of washing film. In summer here tap water is way too hot, so I keep a couple of gallons stored in the house with the film chemistry. I'm on well water, so I also use water filtered through a reverse osmosis filter, so it is essentially mineral free. I use stainless tanks, so I can use the inversion method of agitation that Ilford recommends.

After fixing you go directly to rinse, filling the tank (leaving air space at the top), and do 15 or so gentle inversions as when agitating developer. Then dump the rinse water and repeat with a 2nd fill, doing 20-25 inversions. Then a 3rd fill doing 30 or so inversions. Then empty the tank, and I cover the reel with RO filtered water (use distilled if necessary) with a couple of drops of flo. After 30 seconds or so remove the film and hang to dry. (I also use a rinsed film squeegee immediately.) So this wash cycle takes less than 5 minutes.

I've always understood that shorter wet-times in processing causes less adverse changes in the emulsion, so I also use developers that take 5-10 minutes, citric acid stop for 30 seconds, and rapid fixer that takes 2 minutes. Total processing time under 30 minutes, using well less than a gallon of water, including mixing one-shot developer & stop.

Ilford's chemical testing shows this 3-fill washing achieves archival hypo-free film equivalent to long constant flow washing. This makes sense, as running water wash gradually displaces the hypo solution, while each agitated fill and empty removes the diluted hypo solution when emptying each time. Unlike paper prints, the film base doesn't absorb, so you are really just cleansing the thin emulsion.

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Thanks Tom. I'm starting to think that perhaps it's the detergent  that I'm using that's causing the problem, I'll try and source some of the real stuff. I'll also try using rapid fixer. 

7 hours ago, TomB_tx said:

I use stainless tanks, so I can use the inversion method of agitation that Ilford recommends.

I'm curious about this comment, can a Paterson tank not be used for some reason? I've used the ilford inversion method myself in the past with the funnel insert of the Paterson tank removed. Certainly, given our water bills, the Ilford wash would be ideal. If only I could get it work well! Our water can be dirty which is why I learned to use filtered when doing the Ilford wash and in the final steps of the running water wash.

 

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The Paterson tank will be fine for inversion wash with the top cover snapped on. I didn’t mention it because of people who don’t use the top cap and agitate by rotating the reel, as the plastic caps sometimes split with age.

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I've been using the same method for ever-

Dev for whatever time, 30 seconds stop, fix 5 minutes ish wash running water 20 minutes then 1 minute Tetenal wetting agent. The biggest quality difference to my negs was changing from drying cabinet to a film dryer that dries the film still on the spiral.

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I have a film washing now.

Rodinal 8 minutes, Ilford stop bath less than 1 minute, Ilford rapid fix 2-4 minutes (as long as it takes to wash the lid off the Paterson tank), several quick changes of water before 30 minutes wash through filter, Ilford Fotoflow for a few seconds at the end, then hang up to dry.

seems to work for me.

i don’t see the need for sodium sulfite or hypoclear if you are washing the film in water. Maybe hypoclear if you are very short of water?

you mention dish washing detergent, I would not use any chemicals designed for other uses it might have abrasive things in it.

the only kitchen chemicals I have used are coffee and washing soda - lots of info on the internet if you google developing film in coffee !

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250ml Kindermann stainless tank. Tank, lid and Hewes reel spotlessly clean. 

Rodinal (1+50) mixed with distilled water.

30 second rinse with distilled water, continuous agitation.

Rapid Fixer (1+4) mixed with distilled water, 10 inversions to start, then 5 inversions every 30 seconds. 

Distilled water rinse, 5 inversions. 

Distilled water rinse, 10 inversions. 

Distilled water rinse, 20 inversions. 

Hold ends of film and snap straight several times to remove large droplets. Hang in shower stall to dry. Do not wipe or squeegee!

Total water used less than 1.5 liters of distilled. No tap water. Only chemicals are Rodinal and rapid fixer. My negatives developed this way 40 years ago look (and scan) perfect today.

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To me this does not look like improper washing. Do you ever get soapy or foamy solutions when you pour them out? It could be residual soap residue on the reels and tanks if you are putting the dish soap in while in the same plastic reels and tanks. If you have a foaming action in a small tank, it can cause processing irregularities. One test would be to increase your tank size and developer volume. Make sure that the film is very generously covered in the solutions. You can increase the dilution if you are worried about wasting chemicals. D76 can do up to 1 to 3 I believe. Also, make sure that you agitate generously but not roughly. Do your inversions methodically and consistently. Better to agitate a bit too much than not enough. You will add contrast and decrease development time slightly, but you will make sure things are well mixed. Don't shake it like a cocktail though, or you will generate a lot of foam and air bubbles.

Another thing you could try is a pre wash. Just soak the film in water with some agitation before you start to remove the anti-halation layers and to make the diffusion of the developer into the film a bit less sudden. 

Ditch the dish soap and buy a bottle of photo flo. Mine is half full and I have had it for 15 years. As long as you do not use it for prints, it lasts forever. I use about 1.5mL per 500ml of water. Dish detergents can have fragrances and colors that are made with oils and other contaminants. Photo Flo is clean and designed for the purpose. It might be unfortunate that it is expensive, but it lasts forever. I personally prefer Photo Flo to Ilfotol. I would have assumed they were the same, but Ilfotol irritates my nose, and photo flo is more or less odorless. Not sure how they differ. Photo Flo seems to work better for me in general.

If you are using standard kodak fixer (sodium thiosulfate), 10 minutes if fine. If you are using rapid fixer, Doug is right that you should not do longer than 5 minutes and keep an eye on the clearing time. I use a two bath fixer and a fixer tester. When batch A fails the test, I recycle it, mix up a fresh liter and make that B, and take the existing B and shift it to batch A. That way you are always fixing with fresh fixer. It does not really add any more work. Just pour out A halfway through the fixing and pour in B.

As for washing, your method sounds good to me. I always use a modified Ilford method (basically just a few more changes of water and some soaking time while I do other things), and it has worked very well for me over the years. I have twenty years of negatives and no fixing problems so far... Prints made at a school darkroom, however, are a totally different story. Film is pretty easy to effectively wash if you are not sloppy. Fiber prints are not so easy...

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Thanks very much everyone. I've just ordered a litre of Ilfotol. I couldn't find Photo Flo here. While I use a non-coloured and non-perfumed type of detergent, it could well be the cause of the problem. I have a 2-reel (35mm) Paterson tank. Usually i economise if I'm developing 1 neg by adding 300ml of developer and doing a gentle "twiddle" style agitation. Then for stop and fix I use 600ml of each and do inversions/rotations with the cap on to agitate. With both developer and fixer: continuous agitation for first 30sec then a 5sec agitation every following 30sec. My 5sec agitation with fixer (or when developing 2 negs with the cap on) involves two fluid inversions simultaneously rotating the tank. That was how i remember reading Adam's method in "the negative".

I don't think there's any residual detergent on my tank and reels (no foaming, except after the last detergent step), but i'll give them a good soak and dry before using it again. Will also try Stuart's suggestion of increasing the developer volume to 600ml to see if that helps.

All the best!

Edited by Xícara de Café
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Air bubbles sticking to the film during part of the development - I have to ask, but one (unusual) cause is adding wetting agent / detergent to the developer. It's not needed and causes foaming. BTW, if anyone wishes to purposely demonstrate the air bubbles effect, dilute the concentrated dev with soda water...

Less likely, though possible, is drying marks through not using wetting agent in the final rinse water. Chemical residues due to inadequate washing (rather than no washing) would normally take longer to appear and would show on other frames, too, as well as the film edges where the manufacturer's ID is printed.

Although the OP didn't see the marks on other frames, was this because the subject matter was more varied than the plain sky shown in the example? Was this frame on the outside or inside of the film reel?

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  • 2 months later...

I know this is a long time after the event but you should consider the possibility that you haven't mixed the chemicals enough before using them, especially the developer. I would also avoid putting 'extra's' into the mixes such as detergent into the developer.

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4 hours ago, 250swb said:

I know this is a long time after the event but you should consider the possibility that you haven't mixed the chemicals enough before using them, especially the developer. I would also avoid putting 'extra's' into the mixes such as detergent into the developer.

Indeed - I’m no sure from the above description if the detergent / wetting agent is being applied in the developing tank, but I suggest doing it separately in a plastic container or similar, after removing the films from the reels. I use a plastic tub, and just roll the film backwards and forwards through it by hand in a see-sawing ‘U’ shape.

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  • 1 month later...
  • 4 weeks later...

Thanks 250swb and EoinC. I am using an Ilford wetting agent now, but it never occurred to me to apply it to the film separately from the reel and in a different vessel. Will try this. I don't think the problems I've experienced have had anything to do with gentle agitation. It's something that has dried on the surface of the negative,  I believe.  All the best,

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On 12/18/2019 at 5:29 PM, tobey bilek said:

Uneven negs come from lack of proper agitation.  Quit the “gentile”  so many talk about.

Lots of fix agitation is a important if not more than developer.  

Those marks on the OP could be bubbles early in the dev process, which then dislodged...? Or maybe exhausted or under-agitated at beginning of fix...?

Always do a pre-wet with plain water (at 20C) and lots of agitation before the dev. Guarantees the entire area of emulsion is wet and dev will not have bubble related problems. 

5 gentle inversions and a tap-tap on the counter top at the beginning and on every minute thereafter for the dev - be consistent 

Fresh water with aggressive agitation for the stop (acid not necessary)

Fix with aggressive agitation for the first 30s (v.important). Correct fix time is then simply double the clearing time - irrespective of how tired or dilute it may be (though anything more than 2 mins should be sensibly replaced - assuming Rapid Fix)

Wash the Ilford way with 1 drop of (Fairy) washing up liquid at the end

(No issues with this method over many, many hundreds of rolls processed)

Good agitation is key - and do it the same way every time...

(Hope this helps)

Edited by PCPix
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I’ve not long started developing my own black and white film and having done a couple of rolls by simply flushing with water from the tap switched to the Ilford method. I usually add an additional wash just because and the results are definitely better. 
 

Easier to do as well as it means the water use is more controlled. 

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  • 3 months later...

I wash the film after fixing with water for 30 seconds, and then treat it with Kodak hypo eliminater as per instructions.  I then wash with tap water for the recommended time and flow.  I finish the wash cycle by washing the film in two conseutive washes of 90 minutes each duration with distilled water.  I use no wahing aid such as Kodak Photo flow.  I also do not touch the negatives to remove water drops.  Since the distilled water removes all minerals left over from the tap water wash cycle, there are no water marks.  So, after the final distilled water wash, the negative is pure as the driven snow and is not contminated with a wetting agent, which will leave residue that can cause Newton rings or marks/blothes, and is not touched with a squeegee or other device to remove water drops!

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  • 5 weeks later...

Kinderman or Nikkor type 500cc tank Hewes or Nikkor reels

I prewet 30 sec, the film develop per film, I use TMax developer, has always given me good shadow detail, decent grain. 

Stop bath Sprint indicator 

Sprint Fix 4 minutes, agitation 5 inversions per minute.

Wash 1 water change

Sprint indicator Fixer Remover 3 minutes

10 water changes each change 30 seconds. Uses about 4 liters of water 6000cc for the whole process

30 seconds or so in Kodak Photoflo 2 drips from cap in 500cc

Squeegee 

This works for me

 

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