Selenium fixer stain problem

[Doremus Scudder]

Completed some more tests. So far the issue seems wash dependent.
I made two new test strips. Both using the two fix bath process and toned in selenium 1:9 for 5 minutes.

This time instead of doing a quick rinse I washed one strip for 20 minutes and another for 5 minutes in water, 10 minutes in hypo clear solution, and 5 minutes again in water.

The strip that had the 20 minute water wash stained. But, it was barely visible in the white areas of the paper. The strip that went through the hypo clear shows no stain with perfect whites. I had a third party validate this too because I'm maybe going a bit mad at this point.

As previous commenters pointed out, I'm assuming this means the hypo wash is clearing out the residual silver compounds that is bonding with the selenium.

I ordered myself some Formulary TF-4 fixer like I used to use. I'm pretty sure I was using this stuff back when I was only selenium toning prints and I never had staining issues. I'm going to retest once I have it. I'm hoping that simply switching to a different fixer will help.

As I posted above, if you're using an acid fixer, like Rapid Fixer 1+4, you need to wash thoroughly before toning to avoid stains. You've just confirmed that.

Transferring directly from a neutral or alkaline fix to the toner works without a wash, but do avoid the "short rinse" in either scenario.

A wash aid, like Hypo Clearing Agent accelerates the wash, a good idea if you want to optimize wash time. Try the Ilford 5 minute wash - 10 minutes wash aid - and 5 minute final wash (Ilford says five minutes, but I think a bit longer is better). Information is here: https://www.ilfordphoto.com/ilford-optimum-permanance-wash-sequence-fb-papers/

With TF-4 you should be able to transfer prints directly to the toner from the fixer; no intermediate wash or "short rinse." The rinse will actually cause uneven toning; better to wash fully or not at all. As I posted above, Ilford Rapid Fixer at 1+9 is neutral enough to do this with; I do it all the time.

Note that selenium staining is a good test for residual silver in the emulsion, i.e., inadequate fixing. I've always been a bit skeptical about the Ilford 60-second fix method really doing the job in such a short time. I'm sure it works on Ilford papers with a thorough drain after the stop bath and continuous agitation in the fix, but with other papers or more carried over stop or maybe even including the drain time from the fixer in the fixing time, you may be underfixing. I'd do a film-clearing test on your fixer to check its activity as well. Hopefully, you have a baseline clearing time from a previous test in fresh fixer to compare to. If not, and your testing conventional film, any clearing time longer than 45 seconds or so indicates weak fixer. One problem with acidic fixer concentrates is that they go bad with time. If you've got a hold of some long-stored stock, the fixer could be not doing its job. Usually in that case, there are signs of sulfuring-out of the fixer; a precipitate or flakes floating in the concentrate. Look for those.

That's about all I can think of to help at this point. Hope things work out for your toning.

Doremus

 

[john_s]

Reducing acid in your processes will have a lot to do with the solution. As an experiment, try an alkaline bath after fixing. Sulphite (wash aid) possibly enough, but as an experiment, I'd try carbonate, not concentrated. I don't know how long at would take to neutralize acid in the paper, but as an experiment, I'd try 5 minutes. Then straight into the toner.

Incidentally, any conditions that cause staining with Selenium toner are probably degrading the toner also, by producing deposit.

 

[cirwin2010]

I got my bottle of TF-4 fixer today and ran my test. No stain. Well this is a relief that I can go back to my normal workflow. The last few prints I made took forever due to the amount of washing and hypo baths.

Wish I knew that before I bought 5 liters of the Ilford Rapid fixer. I typically use the stuff for processing my film anyways, but that is so much... Maybe when my new print washer arrives the Ilford Rapid fixer will be easier to use.

 

[Bill Burk]

I’ve struggled with the same exact issue but am stubborn about the chemistry.

I use Dektol 1:2, Kodak Indicator Stop 1/10 ounce to 32 ounces. And Kodak Rapid Fixer 1:7

I used to do one fix bath thinking because it’s fresh I can get away with a single bath.

Lately switched to two bath because of so many fix and selenium toning issues. The third print and later are definitely holding something bad with a single fix bath. With a two bath regime I believe the first bath gets all the complex halides and the second bath stays pretty clean.

I still plan to wash a full cycle prior to toning. But I’m not in love with Selenium toning any more.

 

[Doremus Scudder]

I got my bottle of TF-4 fixer today and ran my test. No stain. Well this is a relief that I can go back to my normal workflow. The last few prints I made took forever due to the amount of washing and hypo baths.

Wish I knew that before I bought 5 liters of the Ilford Rapid fixer. I typically use the stuff for processing my film anyways, but that is so much... Maybe when my new print washer arrives the Ilford Rapid fixer will be easier to use.

If you use a two-bath fixing regime, you can still use the Ilford Rapid Fixer for bath 1, so you can use it up. You can also use it for film and save the TF-4 for paper.

Doremus

 

[john_s]

You can make the Ilford fixer less acid by adding a little sodium hydroxide, or better if available ammonia solution ("ammonium hydroxide") which is what I do. I used to use C-41 fixer which is not far from neutral, but in this part of the world it's harder to obtain at a reasonable price. So I decided that I might as well support Ilford, hence the pH adjustment.

 

[koraks]

You can make the Ilford fixer less acid by adding a little sodium hydroxide, or better if available ammonia solution ("ammonium hydroxide") which is what I do.

Yeah, that'll work. How do you control pH; go by smell - keep adding some until the fixer starts to reek of ammonia (and maybe then back off a little by adding some acetic acid)?

 

[john_s]

Yeah, that'll work. How do you control pH; go by smell - keep adding some until the fixer starts to reek of ammonia (and maybe then back off a little by adding some acetic acid)?

I use pH indicator papers. No need to go fully alkaline, just 6-point-something.

 

[koraks]

Papers are great, yeah. I agree it doesn't have to be alkaline, or very exact even. When making fixer from ammonium thiosulfate crystals, I used to acidify to just below 7 by smell. It should work quite well the other direction as well; hence the question.