Fixer Failure - Any Ideas Why??

[Pioneer]

I had a bit of a problem with my fixer the other day.

I have been using Arista Premium Odorless Fixer, both dry packs that I mix, and Liquid. Nothing special about it but it has been pretty reliable so I have seen no particular reason to change.

A week ago I mixed up another one gallon batch from a package of dry fixer following the directions as usual. However, this time something had to have been different somewhere.

All the films I have developed with this batch have been under-fixed, coming out of the wash with a milky grey appearance. I have since re-fixed them using some other fixer I have so the film is fine.

My question has to do with this fresh batch of fixer. Does anyone have any suggestions on what I should do to troubleshoot what happened. I have done this numerous time before this with no problem until now.

Any brilliant ideas??

 

[Stephanie Brim]

How old was the bag of dry fix? How much time do you give the film in the fix? Were you using the same film as you used that worked in this fix before?

 

[Pioneer]

How old was the bag of dry fix? How much time do you give the film in the fix? Were you using the same film as you used that worked in this fix before?

Not certain of age since there are no expiration dates on the package. I purchased three bags of this about a month ago, one of the reasons I am asking since I have plenty more to use up.

I have always had good success fixing at 5 minutes but I went all the way to 12 minutes to test it with no visible change.

Yes. I have used this fixer with several different films but in this case I was developing and fixing Arista Premium 400 (Tri-X under any other guise.)

I am going to dump this out into a large bowl tomorrow to see if the mix has somehow precipitated out of solution (not sure why it would but it won't hurt to check.)

Another difference I have noted. I typically use my developer as one shot and dump the used developer into a bowl in the sink. I also use my fixer as on shot and dump the used fixer into the same bowl. Some of my films (Arista Premium is one) have a color dye that turns the water green, blue or purple. Dumping the fixer usually changes the color or even clears it. But this last couple times I noticed that when I dump the fixer into the bowl it turns the solution a muddy brown color.

 

[Stephanie Brim]

I use Arista EDU Ultra. I prewet before developing to get rid of the blue dye since I'm using the older emulsion. Do you?

I have basically defected from all fixers that are not TF-4 and all developers that are not Rodinal or HC-110, so I don't know how to give any more advice as to what it could be.

 

[Pioneer]

I sent an e-mail to Freestyle so we'll see what they come up with.

I use a LOT of Arista EDU Ultra, mostly 400 but quite a bit of 100 as well. You certainly cannot beat the price. I usually don't bother pre-wetting anymore. I did some back to back tests a little over a year ago with some Arista EDU 400 and could see absolutely no difference in the negatives between pre-wetting and no pre-wetting.

I also use a lot of Rodinal, some Arista Premium and, more recently, HC-110. My favorite is certainly Rodinal but I do like the HC 110 as well. Based on my small amount of use to this point it looks like HC110 and Rodinal are a lot alike.

I have been looking at the Legacy Pro ECO Pro fixer and I may start using that as it seems to be a little more environmentally friendly.

Why have you decided on TF-4 fixers?

 

[Stephanie Brim]

It has always worked for me. It is NOT a hardening fixer, though, so you have to keep in mind that any negatives with very soft emulsion, like Efke, should be handled with more care. I've used it with HP5/FP4 and Foma 100/400 with no issues, though, and I just like it. The stock lasts quite a while in cool, but not cold, storage conditions as well. I mixed up from stock that's 3 years old.

 

[Rick A]

It sounds as though the fixer might be bad, not the film. I dont have experience with AristaPremium fixer, but regularly use Formulary TF-4, which I love, and Eco-Pro fixer. I used to use TF-4 exclusivly with film and Eco with paper for odor reasons, but I am switching to just the Eco-Pro for everything. I like it because it works well with Pyro developers plus no odor for paper fixing in trays. TF-4 has a slight amonia smell that is ok to deal with in a daylight tank, but I find offensive used for extended periods in trays. Both are rapid acting and require short wash times.
If you need to harden emulsions, switch to a Pyro developer such as Pyrocat-HD or similar.

 

[bdial]

You should start with the basics, is there any chance you over-diluted the mixture? Did you fix for enough time for that fixer?
What procedures are you using otherwise, for example are you using a stop bath, either water or acid? How much agitation in the stop and fixer?
How about temperature of the fix? Colder than 68?

If you're good on those, try mixing a batch using distilled and test that.

 

[Peltigera]

Any factory produced item will occasionally not be to spec. It could be something as simple as one of the hopper containing the chemicals in the factory was extremely low and a few mis-mixed packets missed the QA system. Happens occasionally in the best run factories.

 

[removed account4]

how about doing a clip test with unused freshly mixed fix.
time the amount of time it takes to CLEAR a clip of film
and double that time for your full film fix time.
use 2 baths, and split the fix time between 2 baths ..

i only use sprint fixer, never had trouble with it, and it is liquid stock
and easy to mix ... lasts forever and fixes fast ...
( and if you can't buy it locally, it can be purchased off their website )

 

[Pioneer]

Fixer Testing

Mixing was done with a one gallon water jug. Water heated to 85 degrees F. Once mixing was complete and the powder was dissolved I decanted the solution into a 5 liter container that had contained the same fixer solution.

Fixing was initially done at 5 minutes, which was traditionally good. I have been using this same fixer, sometimes mixed from dry, sometimes purchased in liquid form, for the last two years with no problem.

I am usually pretty careful with my solution temps when developing but I am not quite as careful with the fixer temps. My water temp could be dropping below 68 degrees by the time I get to that step so I'll pay a bit more attention in the future. However, to be completely honest, I have not noticed any problem before this, and the Kodak fixer certainly did not seem to be adversely affected.

I have done a bit of testing since I discovered the problem. After coming to the conclusion that the fixer was not working properly I upped the fixing time from 5 minutes to 7 minutes and then to 12 minutes. I could see absolutely no change in the appearance of the film.

I contacted Freestyle and they will replace the dry fix. I have another bag that I will mix again and try. That bag was manufactured in February 2012. I didn't hold onto the other bag but since they were purchased at the same time then it may have been from the same batch...or not. Before I do this mix I will do a full rinse of the 5 liter container on the assumption that there may be something causing contamination. Not sure what that would be but better safe than sorry.

I do like the idea of doing a clip test, I hadn't thought of trying that yet. If I can't get this fixer to clear an unexposed strip of film in a reasonable bit of time then I have to assume it is a bad batch.

I did have 12 ounces of some Kodak Rapid Fixer that I bought quite some time ago so I was able to recover and re-run the film. It doesn't appear that anything has been lost. But this also has booted me out of my complacency and I am going to take a look at some other fixers as well. I think I'll order up that some of that Eco-Pro fixer and give it a try. But I also ordered up another gallon of that Kodak Rapid Fixer to have on hand. Certainly not odor free, but it did work.

Thanks everyone, I appreciate your ideas and suggestions.

Dan

 

[Mark Crabtree]

Freestyle is very good about following up on issues with their products. I contacted them last year with a question about one of their branded chemicals. They didn't really know the answer so followed up with the company who manufactured the product and called me back a day later with a detailed answer.

 

[Pioneer]

Just thought that I would close the loop on this.

First, the fixer. I tried the clip test and, after 20 minutes, the film had not yet cleared. I decided that the fixer was bad although I am still not completely certain why.

I then dumped the fixer, rinsed the 5 liter container, and mixed up the 2nd bag using the exact same process I had used in the past. I used new mix to fix some 35mm film and everything worked just like it always had before. The film cleared at 2 minutes and by adding another 3 minutes I feel that everything is back to normal. The only possible answers have to be either some unknown contaminant in the 5 liter container (unlikely), a bad batch of powder from the manufacturer (again unlikely, but possible) and finally, an unknown screw up on the operator's (me) part (certainly the most likely possibility and the one that I have to go with at this point.)

Finally, from Freestyle's perspective, Marvin worked with me by e-mail to help eliminate potential issues and finally called me personally on the phone to issue the credit to my card for the fixer. I know that no company can be perfect but Freestyle has consistently provided me with excellent customer service and I recommend them highly.

Thanks to all your suggestions, and thank you Freestyle. I am off and developing once again.

 

[Dennis S]

If all companies were as good as Freestyle the world would be a better place...;o)

 

[Rudeofus]

have you ever thought of using fixer one-shot?
Just to boil it all down to a minumum of variables.

Unlike developers, you can't (or at least shouldn't if you want lasting results) use diluted fixer, which means using fixer single shot is a somewhat costly proposition, and certainly not necessary IMHO. One thing that is recommended frequently, though, is two stage fixing, and it gives you the extra benefit that the likelihood of both fixers gone bad is much much less than that of one fixer bath.

 

[Rudeofus]

Rudeofus: lemme ask you this question. What does it cost more, losing precious pics or using the fixer one-shot?

Alessandro, lemme ask you this question: what costs more, a quick clip clearing test before fixing or tossing out perfectly good fixer after each film roll?

The nice thing about the clip test is, not only does it tell you whether the fixer works, it even tells you how long it takes. It will also catch fixer mixed from defective powder or concentrate.

 

[Doremus Scudder]

Alright boys, no fighting in the back seat!

There is no reason you can't have your cake and eat it too in this case.

I always use fixer one-shot, or better said, one batch, when I develop film. My strategy is to simply not mix more fixer from concentrate than I need for a particular amount of film.

On occasion, when I'm just developing a couple of sheets, I'll toss a tiny bit of still-active fixer. Usually, though, my fixer amount is tailored to the amount of film.

In order to have enough solution for smaller amounts, I simply mix a weaker dilution. Rapid fixers work fine for film in the so-called "print" dilution (1+9 for Ilford products) and higher. For just a few sheets I mix rapid fixers 1+19.

The trick is to first be sure of the minimum amount of fixer concentrate needed. Ilford and Kodak both provide this information, usually in ml for fixing a 36-exposure roll or 8x10 sheet. Lets say I'm processing four sheets of 4x5, which equals 1 8x10. I then measure out 25ml of fixer concentrate (the amount needed for four 4x5 sheets) and, since I'm using 5x7 trays, I dilute it 1+19 to make 500ml of dilute fixer solution.

Since my fixer is much weaker than the recommended dilution, a longer fixing time is required. The good old clip test comes to the rescue. I do a quick clearing test and then triple the clearing time to arrive at my fixing time. (I think tripling the time is better than the usual doubling for a couple of reasons: first, the fixer exhausts during fixing, and the fixing time is always increasing. Second, film can easily be fixed longer without adverse affects and I like the safety factor.)

Once I have my fixing time (which is usually 6 minutes or so at this dilution), I process and toss all the chemicals except for the Kodak Indicator Stop Bath, which I save and reuse (I do toss citric acid stops, however, since they don't last).

I have similar schemes for greater volumes of film: 50ml of concentrate mixed 1+9 for up to 8 films, 100ml concentrate mixed 1+9 and used two-bath for 18 to 36 sheets (with a fresh second bath after sheet 18), and 200ml concentrate mixed 1+4 for batches above 36 sheets, also used two-bath.

Once you have figured out your schemes and tested for adequate fixing (residual silver tests) with them, then it's really easy to deal with, no fixer gets wasted (in fact, with the two-bath schemes, it is actually more economical) and no mixed fix sits around going bad in a bottle.

Best,

Doremus

www.DoremusScudder.com

 

[ozphoto]

Whilst mixing fresh fixer every time, may be a good idea, would it have helped in this particular situation? The entire 5L mix appears to have been "off" (for want of a better description ), so even though I may have mixed it fresh - I would have got the same result, unless I'd performed the clip test first.

And yes, I'm in the "re-use my fixer" camp and perform a clip test prior to processing my films - anything longer than 3 mins, gets disposed of and a new batch mixed.

 

[Doremus Scudder]

Whilst mixing fresh fixer every time, may be a good idea, would it have helped in this particular situation? The entire 5L mix appears to have been "off" (for want of a better description ), so even though I may have mixed it fresh - I would have got the same result, unless I'd performed the clip test first.

And yes, I'm in the "re-use my fixer" camp and perform a clip test prior to processing my films - anything longer than 3 mins, gets disposed of and a new batch mixed.

Of course, you are correct, Nanette. I was getting a bit off-topic there, distracted by the discussion about whether to use fixer one-shot or not. Just wanted to point out that it works just fine without waste.

As to the OP's problem. If indeed he has a batch of fixer that won't fix, the only thing to do is get some more. Freestyle seems willing to replace it if it is defective and he has already re-fixed the negatives in question. A clip test of the fresh fix would have indeed turned up the problem, but this seems extremely rare. I only clip test fresh fix if I'm using a weird dilution and need to determine fixing time, never just to see if the fixer is working or not...

Best,

Doremus

www.DoremusScudder.com

 

[ozphoto]

Of course, you are correct, Nanette. I was getting a bit off-topic there, distracted by the discussion about whether to use fixer one-shot or not. Just wanted to point out that it works just fine without waste.

As to the OP's problem. If indeed he has a batch of fixer that won't fix, the only thing to do is get some more. Freestyle seems willing to replace it if it is defective and he has already re-fixed the negatives in question. A clip test of the fresh fix would have indeed turned up the problem, but this seems extremely rare. I only clip test fresh fix if I'm using a weird dilution and need to determine fixing time, never just to see if the fixer is working or not...

Best,

Doremus

www.DoremusScudder.com

I've often wondered about using one-shot myself, but the workflow I currently have is giving me good results. Having said that though, I am tinkering with the idea of the 2-bath solution. (Certainly wasn't my intent to knock your method on the head Doremus - was trying to point out to others, that in this actual instance, a one-shot method would have failed as well, and that the suggestion of a clip test for fixer, is an excellent way to determine its viability. )

I must admit that the next time I'm in the darkroom, it will be a fresh mix for all the films I'm processing, simply because I'm away for long periods of time, and the used fixer might not stand the test of time quite as well as I'd like. (Does that count as one-shot?)

 

[Rudeofus]

In order to have enough solution for smaller amounts, I simply mix a weaker dilution. Rapid fixers work fine for film in the so-called "print" dilution (1+9 for Ilford products) and higher. For just a few sheets I mix rapid fixers 1+19.

This is exactly the technique I warned against and I will give you the reason why:

1. Fixing is a competition between AgBr/AgI and the complex of Silver with the fixer, usually Thiosulfate.
2. The balance between these two is governed by the solubility product of AgBr/AgI and the complex stability constants of the various Silver Thiosulfate complexes.
3. Note that all soluble Silver complexes contain several molecules of the fixer, which means the concentration of fixer goes in with an exponent of 2-5.
4. A low concentration of fixer will therefore shift the balance strongly towards AgBr/AgI and those Silver complexes, which contain only one or two molecules of Thiosulfate. Note, that these are insoluble, i.e. they will remain in your film. And they are not archival!
5. This means you will end up with retained silver ions, regardless of how long you fix and what your clip test tells you.

And this is the reason why I advise against one-shot fixing: it becomes expensive, people start diluting their fixer, and archival stability goes out the door. Using two bath fixing with full strength fixer as described by Haist (and many others) is cost effective and avoids exactly these problems.

 

[Pioneer]

Good stuff here. Thanks. Most of my developing work is pretty basic and I don't usually stray to far from the directions unless I am doing N+1 or N-1 developing. I always dilute according to the directions on the bottle or package and don't dilute beyond that point.

Interestingly I have done clip tests in the past, whenever I experimented with a new fixer. But I never thought to use it whenever I started a new batch of a fixer I regularly use. In my case doing a clip test before starting a new batch of fixer would have caught my problem before I had film in the tank. It is a pretty quick and simple process so I think I'll incorporate it in the future when I mix a new batch of dry, or start a new bottle of liquid.

You learn something new everyday!

I use 3 different fixers. When I started with each fixer I did clip tests to establish a fix time for my use. Once those clip tests had been done I have not re-done them. Each fixer is mixed at the time of developing except the dry powder fixer. That one is mixed and makes one gallon which is then used without any dilution. None of the fixers I use are terribly expensive so I have always disposed them after I used them fresh and have not tried to re-use any of them. Once I had established a clear time and then multiplied that by 2.5 I felt comfortable and never considered that my fix may not have been archival.

I have never tried a two bath fix so I will have to research that to see if that helps. I do have one question about it though. In my case, if I had been doing two bath fixing, and one bath was not working, I may have been fooled into believing that my fixing procedure was working correctly when it really wasn't. If I were fixing 4x5 or 8x10 in a tray then I may see the results and catch the problem. But in a daylight tank, you wouldn't know if your fixer was working until you had washed and removed the film for drying. Am I wrong here or is there something I'm missing?

 

[Rudeofus]

I have never tried a two bath fix so I will have to research that to see if that helps. I do have one question about it though. In my case, if I had been doing two bath fixing, and one bath was not working, I may have been fooled into believing that my fixing procedure was working correctly when it really wasn't.

Two bath fixing is an economical way of fixing many films/prints with a limited amount of fixer yet achieving archival results. You basically start with two fixer bathes, and always fix first in bath 1, then in bath 2. After a few rolls of film or sheets of paper you discard bath 1, use bath 2 as the new bath 1 and mix a new bath 2.

But think of this: most studies on archival fixing were done when acidic fixers based on Sodium Thiosulfate were on vogue. These fixers were slow and weak, and difficult to wash out compared to modern rapid fixers! Using two bath fixing with modern rapid fixers is most likely overkill, but could serve as backup and insurance against over-used, over-aged or otherwise ineffective fixer. It is more economical, more effective, and less prone to failure than using one fixer bath single shot.

If I were fixing 4x5 or 8x10 in a tray then I may see the results and catch the problem. But in a daylight tank, you wouldn't know if your fixer was working until you had washed and removed the film for drying.

That's why clip tests are recommended. Note there are also simple test procedures for retained silver, so if you are uncertain about past film rolls, you can still find out whether you need to refix them before bad things happen.

 

[Pioneer]

Thanks Rudeofus. I'll check on the test procedures for retained silver and incorporate that into my process.

I have been photographing and developing for awhile but it seems there is always something else to learn, or to be reminded about. This has been the case here and this has been a great little thread for me. I really appreciate everyone's time and their help.

 

[Pat Erson]

"That's why clip tests are recommended"
Allright but do you have to prewet your clip in plain water before you dip it into the fixer or can you use a dry clip?
I've heard that to get an accurate result you have to use a "wet" clip...

"This is exactly the technique I warned against"
I fully agree. The ONE time I had problems with neg fixing was when a "pro" (he did Helmut Newton's darkroom work in the 80's...) advised me to fix my negs in a 1+9 solution (instead of the usual 1+4).

He said he got "nicer negs", me I got brown-stained unfixed negs...