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First time developing Black & White Film at home: Fail.


maxip

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Hey guys! 

I just developed my first film at home. 

 

Tri X 400 at 1600. Shot on my M6 with a 35 Summicron and Yellow Filter. This is my go to setup.

Today I tried do develop my first role at home with the following recipe: 

 

-18:30 in Rodinal 1+50 at 19°C/68°F

-Agitate 30 seconds initially, then 2 inversions every 2 minutes

-Rinse/stop with 19°C/68°F water for 1 minute

-Adox Adofix 1+9 fixer for 4.5 minutes

-1 min wash


-Adox Adoflo 35 seconds with distilled water

-hang to dry

 

Bye the way, I know Rodinal is probably the most inappropriate developer one can use for pushing tri x at 1600.

 

Here ist the outcome. Strange streaks all over the negatives.. So much grain and a strange tone curve. 

 

img_828770qll.jpg

 

bildschirmfoto2016-0158osm.png

 

Any ideas what caused this problem? :(

Edited by maxip
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I suspect that the film was submerged in the developer solution only part of the time. Is your tank of an appropriate size to hold exactly one 35mm film?

 

It is a Paterson Universal tank and it holds up to 2 35mm film or one plan film. 

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I would agitate more. My standard is 2 or 3 inversions every 1 minute. The agitation cycle take 5-7 seconds. I want a complete movement of the solution. I don’t know how Paterson tanks work, but don’t use any twirling schemes. Put the lid on and invert the tank by 180 degrees. Twirling will promote eddies around the sprockets and will show up as uneven development.

 

Also, make sure you are using enough solution. Test with water and the lid off.

 

Also, some other unsolicitated suggestions that have nothing to do with your developing difficulties:

 

  - Use HC 110 with Tri-X. Rodinal produces coarse grain. Not generally thought to be ideal.

 

  - Don’t expose Tri-X at 1600. You are, in fact, under exposing by 3 stops, virtually guaranteeing negatives with very poor shadow detail that are difficult to print (and maybe scan). Tri-X’s best exposure index is about 200-250, which produces beautiful, rich negatives.

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There is so much that seems to have gone wrong that I suspect you have more than one problem, maybe three or four, all overlaying each other.

 

But basically if we are looking at the end of roll (a shot frame is just visible to the right), it doesn't look like you have fixed the film properly. I've tried to find the dilution instructions for that particular fixer and they are ambiguous at best, but it seems you haven't got the dilution or time right. So, using an otherwise discarded un-developed bit of film (say the bit in the bin you've left attached to the cassette after cutting it off, or snip a half inch from a film leader) immerse it in your diluted fix, either 1+4 or 1+9 (but I would use 1+4 for film), and time it until it has fully cleared. You then multiply that time by 2 and that is you fixing time for that dilution of fix. You can do that test in daylight.

 

And while it won't have contributed to the overall problem your washing time seems very, very short at 1 minute. In running water I'd expect it to be at least 20 minutes, but the Ilford method is the most economical and efficient. It is fresh water in the tank and invert ten times and pour out. Fresh water and invert twenty times and pour out. fresh water and invert forty times and pour out. The film is now washed to archival standards.

 

Steve

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The main problem definitely looks like incomplete fixing. If you do not remove the unexposed silver completely, it will turn dark once you open the tank and expose it to light.

 

Here is Adox's own procedure for testing that fixer and detemining the correct time to fix. http://www.adox.de/Photo/support/film-fixing-time/

 

Two important things they say:

1) 1+9 dilution will take longer than 1+4 dilution.

2) Actual fix time should be at least two times the "clearing" time.

 

Given their recommendations - 4.5 minutes is enough using a dilution of 1+4, but using 1+9 dilution, 4.5 minutes was far too little. Diluting chemistry means there is less chemical to do the job, so you must give it more time to work.

 

Temperature is important for fixers - they tend to stop working altogether if they are colder than about 65°F/18.5°C

 

Additionally - an acetic acid STOP BATH helps fixers to work. Rodinal/Adonal is a highly alkaline developer (contains sodium hydroxide), and really needs an acid stop bath between development and fixing, to neutralize its alkalinity - not just a water wash. Otherwise it will "kill" the fixer's ability to work (fixers are acidic).

 

The streaks are due to fixer "pumping" through the film holes during agitation, and delivering more agitation in those places, and thus removing more silver.

 

Another tip-off of fixing failure - in addition to the black stains - is the "solarization/Sabattier Effect", or semi-reversal of the tones, in your actual picture sample. White outlines between the buildings and sky, and in the woman's hair and face.

 

http://www.photoanswers.co.uk/upload/6332/images/Solarization%20effect.jpg

 

Failing to neutralize your Rodinal after development with a stop bath, and not giving enough fixing - the image continued to develop in the light, leading to the partial reversal.

 

Recommendations:

 

USE an acid stop bath to make sure you have "killed" the development rapidly and completely after time is up, and neutralized Rodinal's alkali pH so it won't damage the fixer.

TEST your preferred fixer dilution, and make sure you give enough time. It is hard to overfix film (takes 30 minutes or more, with common fixers).

CHECK your fixer temperature, especially in the cold season. Must be 20-24° C

WAIT at least 1 minute (2 minutes is better yet) after starting fixing, before opening the tank to look at the film

WASH film at the end for at least 15 minutes - or use a washing aid/hypo clearing agent, as directed, to "unlock" the fixer molecules from your film's gelatin.

________

 

Nothing wrong with Tri-X in Rodinal - many great photographers have used it.

 

Its high dilution (1+50) will actually increase shadow detail somewhat, in what is called the compensating effect. Between agitations, the very dilute developer gets used up quickly where there is lots of silver, and the developing pauses until the next agitation. Whereas in the shadows where there is not much silver to react with, the developer stays fresh and works the whole time. So it can work very well for "pushing" underexposed film.

 

However, the high dilution also means there is very little "solvent action." Most developers contain a chemical solvent that eats away at the edges of the silver grains, at the same time that they are developing and growing larger. Giving finer grain. Sulfites are the most common solvent (because they are also a preservative).

 

Rodinal has some Potassium Metabisulfite as a preservative - but at the high dilutions, not enough to have a solvent effect. Thus Rodinal will produce larger grain (and also somewhat higher edge sharpness, since the image is not dissolved in any way). Just a matter of taste which effect(s) you desire.

Edited by adan
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Thank you so much guys. I really appreciate that you take your time for helping me out. 

 

@rpavich - It is turned off. 

 

@250swb &  @adan - Fixing was also my first thought. Next time, I will make the test first and try to fix at at least 20°C. To be safe, is it okay to fix about a minute longer than it should? Or fixing it longer will also cause problems? How much do you agitate the fixer? 

 

@adan Thank you so much for these detailed informations. Really helpful. I didn't know a stop bath is more or less "necessary" when working with Rodinal. Also didn't know anything about "solarization/Sabattier Effect".

 

I'll go for something cheaper than Tri - X next time and keep you updated. 

 

Max

Edited by maxip
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Hi Max, I agree with all recommendations above.

 

At a second step , I also use Acetic Acid ("white vinegar" sold in supermarket and cheap)

dilution 1/10, as said Adan to stop the developer.  :)  

first step in developer (Ilfotech HC110 3.30mns) , I gently turn the spires (Paterson tank) all

along the 3mn30.

third step : fixation time (Ilford fixer) is important too , within 10 minutes in my case in turning gently.

Developer and fixer volumes prepared for 1 liter

 

 

Here is the result

 

Welcome, dear visitor! As registered member you'd see an image here…

Simply register for free here – We are always happy to welcome new members!

 

Leica MP-28 Summicron Asph

Nikon scan 5000

 

Some more photos in "I like film"  thread

http://www.l-camera-forum.com/topic/205842-i-like-filmopen-thread/?p=2962866

http://www.l-camera-forum.com/topic/205842-i-like-filmopen-thread/?p=2963143

 

 

and for pushing TX400 > 800 with dev. D76  :

http://www.l-camera-forum.com/topic/205842-i-like-filmopen-thread/?p=2957872

 

Try again and good luck Max :)

Best

Henry

Edited by Doc Henry
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To be safe, is it okay to fix about a minute longer than it should? Or fixing it longer will also cause problems? How much do you agitate the fixer?

 

Eventually - the fixer can start dissolving the metallic silver image. But as I said, that takes much, much longer than a couple of extra minutes. Don't go out for lunch (or on vacation) leaving your film in the fixer - but really, even 2-3x the "normal" time shouldn't cause any harm.

 

Outside of extremes, the idea of fixing is to "fix to completion." You want ALL the non-image silver-halides removed completely, because if any remain, they will eventually turn brown or black.

 

Depending on the exact brand and chemical composition and age/previous use of the fixer, that can take from 4 (very fresh, so-called "rapid-fix") to 10 minutes. If it takes more than about 5 minutes to "clear" the film visibly, the fixer is worn out.

 

Agitation should be gentle, to avoid those vertical streaks. 1 inversion every 15 seconds, or 2 every 30 seconds, or 4 every minute - it all comes out the same.

__________

 

Digging a little deeper - if you could see the film just before it goes into the fixer, it would be translucent and milky. The black/gray developed images would be clearly visible on the emulsion side, but only faintly visible through the back of the film.

 

The milkiness is the remaining light-sensitive silver halides that were not exposed and developed (and are now wet). The same milky-gray/brown/pink stuff you see when loading the film into the camera, but a bit more transparent. http://www.redorbit.com/media/uploads/2004/10/0_a3c0877d59d925f86a0919e67588be41.jpg

 

As the fixer starts to dissolve those, the milkiness goes away, or "clears." But since we are talking about tiny molecules, the mere fact that you can't see them anymore does not mean they are all gone. Therefore, the standard recommendation to "fix for twice the clearing time," to be sure the last little bits have also been dissolved.

 

(I couldn't find an image of "unfixed" developed film on the web - for the obvious reasons that it is still sensitive to light, and it is (usually) a very temporary condition. I may have to do the world a favor and take a snap of my next roll, in between stop bath and fixing - done carefully, and quickly, it should not actually cause damage!)

Edited by adan
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"WARNING: This stunt was done by a trained professional under controlled conditions! Do not try this at home!" ;)

 

As promised, snapshots of some film, after the stop bath, but before fixing.

 

This is Kodak Tmax 400, which has an extra-strong pink tint from anti-halation dye (which will also wash out eventually). Most films will be more of a cream color.

 

Note the milky semi-opaqueness, which is the light-sensitive silver halides that have not yet been removed by fixing.

 

I was able to get these pictures by giving the film two stop baths and a rinse, to remove any left-over developer, and taking the snaps quickly. Even so, if the film had stayed like this for more than a few minutes in light, it would have "fogged" from the light and darkened.

 

 

Welcome, dear visitor! As registered member you'd see an image here…

Simply register for free here – We are always happy to welcome new members!

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Thank you Andy, for taking this risk! :D

 

I followed your tips and I think it worked quite well. 

 

-Fixer dilution 1+9 but for 6 min at 20°C. 

 

-Washed the film for at least 5 min. 

 

-All prepared for 400ml instead of 300ml. 

 

-1 min permanently inverted, every 30 seconds 2 inversions.

 

-Even without a stop bath. I will try it with white vinegar next time, thank you Henry! 

 

23973605530_edb08e029a_z.jpg

 

More to follow in the I Like Film thread. Thank you all :) 

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Looks very good indeed. White vinegar would be fine - stop bath is acetic acid with an indicator. Look at Ilford's processing instructions (see web site) - I think you should wash for more than 5 minutes for maximum permanence. But this looks like an excellent negative.

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I don't know which bit of the advice you've been following but yes, 5 minutes wash is another recipe for disaster, although it will come home to roost much later. Seriously, the Ilford method hardly takes more than five minutes and is much more efficient than running water.

 

 

Steve

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Andy's illustrations are excellent. As an aside, a counterintuitive cure for removing tenacious antihalation is to fix and wash and then dunk the reel of film back into developer, agitate till it is gone and rewash.

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I don't know which bit of the advice you've been following but yes, 5 minutes wash is another recipe for disaster, although it will come home to roost much later. Seriously, the Ilford method hardly takes more than five minutes and is much more efficient than running water.

 

 

Steve

 

I used the Ilford method.

I should have made that clear. Sorry! 

 

Max.

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I used the Ilford method.

I should have made that clear. Sorry! 

 

Max.

 

Ah good, one bit of good technique you can put a tick next to. It is science lab practice and all worked out by some boffin counting molecules, how many changes of water (with agitation) before you got to billions-to-one contamination levels.

 

 

Steve

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