Removing powdery stuffs from the emulsion side

Yes, I pulled another 'one' after a while! The emulsion side has lots of white and somewhat powdery stuffs throughout the roll. I'm guessing it is due to either of the followings (or combination of both):

(1) Instead of using non-powdered gloves I used a powdered one after washing both sides. Seems I didn't wash it enough. Could this be due to the powder thingy? I know I should've used non-powdered (Nitrile) gloves regardless!

(2) I use Tetenal Superfix Odourless (Art. Nr. 103067), which had some chrystal forming near the mouth. Reading some threads, I get the idea that they form due to colder weather and that they're not a problem. I only made a working solution of 500 ml (1+4 => 100 ml Fixer + 400 D. Water) yesterday and this is the 2nd roll with this fresh mix. Should I filter it? I don't see anything floating, or being at the bottom.

FYI:
- it is a 35mm Rollei RPX 400 (@ box speed),
- developed with SPUR HRX (recently opened bottle) - 1+9 (25ml + 225 ml).
- I used distilled water (DW) in everything except 3/4 water washes with our tap water (a total of 6 mins) - followed by 2 DW washes (3-4 mins) and wetting agent (with DW) thereafter.
- I don't think it is the tap water though as such thing never appeared on my films before.
- the temperature was between 21-19, starting at 20 deg Celsius as per standard

Will a rewash with water and then DW wetting agent scheme solve the problem? Anything else?

Bests,

Ashfaque

It could be the tap water. Take some of the film (not an important frame) that has the powder and rinse with a dilute acid solution. If it removes the powder it probably was calcium carbonate in the water. If you are using PhotoFlo you only need a few drops/liter of distilled water.

http://www.jeffreyglasser.com/

jeffreyg said:

It could be the tap water. Take some of the film (not an important frame) that has the powder and rinse with a dilute acid solution. If it removes the powder it probably was calcium carbonate in the water. If you are using PhotoFlo you only need a few drops/liter of distilled water.

http://www.jeffreyglasser.com/

Click to expand...

Thanks for the tip, Jeffrey. I use Tetenal Mirasol 2000 Antistatic (Art. No. 101080) @ 1+400 as wetting agent. Can I use Fotospeed SB50 (it has an indicator)? Please let me know the dilution I should use for this. I generally use it as a 1+19 dilution (15ml + 285ml) for stop bath.

Bests,
Ashfaque

It sounds to me like your tap water couldn't possibly leave deposits on the film. Your distilled water rinse with wetting agent is usually all that's needed even with rather hard water. FWIW, I use moderately hard tap water for everything except the final rinse in DW and wetting agent; never a problem like you're describing.

So, on to other possibilities: A little crystallization around the mouth of the fixer bottle is unavoidable, just clean it off before you pour and/or filter your fix. However, if your fixer concentrate is old and has started to sulfur-out (form insoluble sulfur particulates), then this ca (and often does) end up on the film. It sticks to the emulsion side and is often very difficult or impossible to remove in the subsequent wash step. Check your filter concentrate by shaking up the bottle and then pouring it into a clear vessel. Check for small suspended particulates. If they are present, you need to discard your fixer and buy new. Also, filtering a solution when there is doubt will never hurt! If you're overusing your fixer and/or using the same fix for film and paper (you shouldn't) unwanted precipitates can form. Normally, keeping track of throughput and not exceeding capacity will prevent this. Getting too-old stock solution from your dealer is another issue and one that is often overlooked.

I have a tendency to fill my trays though a filter funnel equipped with an additional paper filter. This ensures sludge-free solutions for processing. You may be able to filter your solutions before pouring them into the tank if you think this may help.

Another thing to look at is your film drying environment. Dust control is really important. If you're sure that the deposits on your film is something other than dust, then disregard this. Otherwise, make sure you're hanging your film in a clean environment to dry.

Powdered gloves... hmmm... As far as I know, powdered gloves are only powdered on the inside to help them slip on to (sweaty) hands easier. I don't think that the small amount of powder on the inside of the glove should cause a problem unless you put the gloves on inside-out an handled wet film immediately. Any residue should rinse off easily (you do rinse your gloved hands well before handling wet film, don't you?). Heck, I often use powdered gloves or even give a shake or two of talcum powder into my nitrile gloves to help them slip on easier; never a problem. FWIW, if you use powdered gloves, put them on dry and then wash the outsides just like you'd wash your hands. That should take care of any dust/powder problems.

As for rewashing: you might try getting the film well soaked with DW and wetting agent and then very, very carefully try to manually remove the deposits by gently brushing with your fingers. Particulates stuck in the emulsion are often difficult to remove without some emulsion damage however.

Finally, check all your solutions for dust/particulates and replace or filter them as needed.

Hope this helps,

Doremus

Thanks for the detailed advice, Doremus.

I just checked the fixer concentrate as per your instructions, by pouring in a freshly washed clear graduate. The fixer is absolutely clean, nothing is floating, neither anything at the bottom.

I'll buy some coffee filters just to make things less susceptible. It'll give me the opportunity to try some press coffee too.

Another possibility: The film roll was developed almost a year later. Forgot to mention it. All this time it stayed in the fridge (not in freezer even though it should've). Kodak also suggest that the exposee films should be processed within 6 months. Could this be the culprit.

Interestingly, I did another wash before getting feedbacks from you two though. I left the roll soaking in DW for about 40 mins (inside Jobo 1510), followed by wetting agent step outside the Jobo with a seesaw movement (about 1:30 mins). But I didn't attempt to clean the bits, even though I wanted too. Was too afraid.

Good news is that some of the nasty stuffs are gone, especially inside the roll. The further away from the core of the reel, the worse it is. But overall it is better than before.

So, whlist I was at it, I cleaned all the inerds of the tank. Used some cotton buds to reach and clean some narrow areas. Pulled out some blackish stuffs, it was somewhat sticky. My guess is it came from the previous fixer working solutions as I overused it by about 80-90%.

I'll do another DW wash and wetting thingy now and try to remove the rest manually (if I can summon up my courage).

Sorry for the long reply. I hope it'll be useful for me and others for further advice and future reference.

Bests,
Ashfaque

Your problem is particulates of some kind on the film; nothing whatsoever to do with refrigeration, etc. BTW I wouldn't freeze exposed film or even keep it in the refrigerator because of the possibility of condensation forming. Better to just store it in a cool, dry place (room temp. is okay).

If there was "blackish stuff" in one of your tanks, then that may be your culprit. Clean things, use fresh chemistry, don't overuse chemicals, do a final rinse in DW with wetting agent, dry your film in a dust-free place and you should have no more problems.

Best,

Doremus

Thanks again, Doremus.

I am quite the newb, and the gentleman above practically gave you all the advice you could need, but, if I may add my .001:

-I found that, especially for the processing tank, the hands are very good at removing any minute dust/ small particles that may be on it. Just make sure your hands are clean and dry.This won't help much if you have stuff "caked" on it. I have also completely dropped the wetting agent from the final rinse, as it had accumulated residue on the small crevices(especially on the reels, the last place you want sticky stuff to form!). I have extremely soft water, for the record.

-Dust/etc, if provenient from the drying stage, seems to come off much much easier, than dust/particles introduced at the processing stage, which seem to "dig" into the emulsion harder, making removing it a very hard task. I had many problems with unwanted grit on my negs early on, but I have successfully solved all of them, resulting in the points I made above. They may or may not solve your probs.

Hi Micheal,

I was/am careful on both counts. Thanks for your reminder though.

P1: Jobo specifically mentions in the instruction sheet not to use wetting agent step inside the Jobo tank/reel. I made the mistake only and iirc, Matt pointed it out me. Thanks Matt.

P2: I always take a hot shower beforehand. Consequently there are less dust particles floating around. The door is always shut whilst rolls are drying. Draft wind is not a problem either as the area is pretty long. When I started out, dust was a big issue. It was mainly due to the dampness of the lower ceiling o the bathroom (have a storeroom on top). But since a new paint job, it is no longer a concern.

Bests,
Ashfaque

Have you been able to resolve the problem? Does rewashing or refixing the film help?

I have encountered something similar / the same this weekend, developing 9x RPX-400 in RPX-D. The emulsion of the DRYED film feels a bit sticky and seems to have white powder (extremely fine, finer than flour) embedded as a kind of drying spots. I gave all the films a final bath in distilled water & surfactant, and I am sure my process & lab is clean enough / water soft enough for not having caused this. All the film has been fresh, procured directly from Maco between September 2016 and January 2017, exposed in December / January 2016. RPX-D has been freshly bought / opened, the Fixer has been open a while (4-6 months), smells a little but it is clear and has behaved perfectly normal in a clearing test and fixing HP5+.

I am not sure about what could have caused this, but maybe the following has contributed:

1.) I have done a rotation development, I am not sure whether RPX-D is suitable for rotation development?
2.) I have used Ilford Rapid Fixer 1+9 for 5 minutes, which is approximately 2,5 times the clearing time. Maybe, this film need a stronger fixer?
3.) 7 of the 9 films were slightly fogged by X-Ray (three times at various airports) and overdevelopment, maybe this had an effect? BTW: Despite of the fogging/overdevelopment, the tonal range & contrast of the pictures is just fine.

I have passed two of the films between my fingers to "facilitate drying", and the powder is in a shape of lagoons of the water spots although the emulsion itself is unharmed. The powder became visible immediately inside the emulsion - the water was clean, so I hang the other films directly and they have a fewer spots.

I have developed another 3 RPX-400 in RPX-D manually (one x-rayed, two fresh). For one I have used the acid stop bath (more spots), the other two were bathed in water only instead of a proper stop. These last two look a little better than the others, yet the emulsion is a bit sticky, too, and there also seems to be the white powder - but thinner. I have furthermore developed 5x HP5+ in Microphen 1+1 which turned out just perfect - nothing strange at all.

I have not tried to print these negatives yet, so I don´t know if this affects during printing.

Any ideas anybody?

Following up and sharing:

I have tried refixing & rewashing which does not really solve the problem.

Furthermore, I have commented on this issue with Wolfgang Moersch. He had a look at the negatives and suggested hardening the emulsion - a sticky emulsion after proper drying is a strong indicator for a dehardened emulsion. In his experience, a fine silvery fog sometimes remains in a softened emulsion. Tested on an unexposed frame, it did the trick. The powdery stuff disappeared and so did most of the stains in the area of the film which had been in contact with the reel.

Lesson learnt: RPX-400 in combination with RPX-D will get the "Hardening Fixer" treatment.