Got flakes in my XTOL
Old 01-21-2012   #1
Ljós
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Got flakes in my XTOL

Hi all,

I am a happy HC-110 Dil. B. user (with Ilford HP5, also with TMY2), but heard many good things about XTOL, too. Now that I got a sizeable amount of rolls shot under similar light to develop I bought a gallon pack of XTOL and figured I'd give it a try and compare with HC-110-developed negatives.

I used distilled water and followed the instructions (heating the water, but not too hot etc.) to the letter, but from the getgo I could see "flakes" (see the crappy cellphone picture to get an idea http://www.flickr.com/photos/summaro...in/photostream ) in my full strength solution. I googled around and found reports of this happening with XTOL, but not so much info here on RFF.

The first two films are done (HP5 with XTOL 1+1 in a Jobo1520 (485ml capacity)), the next two are hanging to dry. So far everything looks good, I am going to make prints this weekend.

My question: how big a deal is this? Tips for possibly improving the mixing stage? Should I bother to filter the full-strength solution?
I am not so much worried about the discussed-to-death "sudden-death" of XTOL, because a) it has been sufficiently (for me) pointed out that this was mainly a problem with the now discontinued 1l packs of XTOL and b) because I shoot and develop film at a quite regular pace of at least 10-12 rolls a month, so if I were to switch to XTOL I'd burn through a pack in less than three months.

What I am worried about is spots on the negatives/uneven development etc... I will look at the coming rolls with eagle eyes, but maybe someone here has general experience with this scenario.

Any firsthand experience with this phenomenon would be very valuable!

Thanks in advance for chiming in!
Greetings, Ljós
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Old 01-21-2012   #2
Photon42
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I'm not an XTOL expert and certainly no chemical one as well, but XTOL is my most used developer. The mixing takes some time, however, I have never seen flakes yet in any of my set-ups. My hunch is that flakes stem from improper mixing and/or contamination in the bottle or even from the bottle (in case some weird generic plastic bottle was used). Given the price of the developer, you may want to redo the solution - that is want I would do. But then, if the outcome is good, you get away with that. Maybe also a question of how many flakes you have. I think in the latter case I'd either try to dissolve the flakes or filter them. They could stick on the film surface giving undesirable effects.

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Old 01-21-2012   #3
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Thanks Ivo,

yeah, stuff sticking to my film is what I am trying to avoid. I am having trouble uploading a picture right now, even though it is only 64kb and no wider than 600pixels.

I am quite certain it has nothing to do with contamination of the bottle - I used a new 5l canister of distilled water. But maybe I should have mixed for a longer time...

What kind of temperature do you folks recommend?

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Ljós
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Old 01-21-2012   #4
sojournerphoto
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It's most likely that you didn't completely dissolve part A before adding part B. Also, if you add the powder to the water too quickly then it clumps and be hard to dissolve. I tend to mix xtol in about 3 to 4 litres of water and give it a really good shake in the (sealed!) container whilst adding A in small amounts and then again adding B in small amounts at a time. Sometimes there's a bit of residue, that often disappears after a couple of weeks anyway, but I've never noticed any problems.

Shelf life actually appears quite good in practice, though I did have one batch that just failed. However, I think it may have been contaminated with fixer in a 'putting chemicals in the wrong jug accident!'

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Old 01-21-2012   #5
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Mike,

adding Part A (and at the second stage Part B) in smaller increments sounds like a good idea, I will try that next time. If I remember correctly I added the powder A (and later B) more or less in one go, expecting it to dissolve easily in the warmed water. I did shake vigorously with resealed cap, but stopped at some point when I saw I didn't get rid of the "flakes".

I guess the prints/enlargements will show whether I caught some spots, but so far the negatives look good. Of course I now need to dial in my development, at first attempt I got more density/contrast than I would have gone for with my HC-110 routine. But should print well, we'll see.

Thanks all so far!
Ljós
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Old 01-21-2012   #6
haempe
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Similar experience here.
Let Part A time to dissolve complete before adding Part B.
I usually wait a hour or two before adding Part B.
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Old 01-21-2012   #7
Tim Gray
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So I've had this happen. The first time I noticed, I was about halfway though using the batch. It was several months old, so I just dumped it and mixed a new batch in new bottles. I was very careful mixing the new batch. I always use distilled water. Anyway, the new batch was good. Three weeks later, I noticed it again. Assuming now that it was contamination from the new bottles, and that it wasn't an issue from mixing (since it developed a good deal of time after mixing) I just went ahead and used it. I have a funnel with a metal screen in the tip so I just pour my XTOL through that when mixing it up 1:1. I've not had any problems with it, and no increase of crap on my negatives. It happened again in the latest batch I just mixed up too, so 3 batches in a row.

Here's a thread about it on APUG. I forget exactly what they said - I'm going to read it now.

http://www.apug.org/forums/forum37/7...m-bottles.html
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Old 01-21-2012   #8
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Tim,

thanks for chiming in and the link to APUG.

"Xtol needs to mixed with water up to the recommended hot temp, around 90 deg F. Don`t do the room temp stuff."
http://www.apug.org/forums/viewpost.php?p=955318

My take is to use a higher temperature next time (I was within Kodak spec but a few degrees lower than the stated max. temp. And I am getting the feeling that a few degrees more than 85 deg. F./30 degrees Celsius won't hurt.)
That, and take more time to dissolve Part A.

I am going to keep using the stock I mixed though, unless my printing session later reveals some shocking flaws :-)

Greetings!
Ljós
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Old 01-22-2012   #9
bigeye
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I've never had a problem with flakes at room temp. The last bit of Part B can be a bit of pain to finish dissolving, but I've never seen anything like that. I use tap water.

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Old 01-22-2012   #10
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Yes, when adding the powder to water, I've noticed it wanting to flake up. I just keep stirring, stirring, and stirring. I'll use the stirring stick to break up these flakes. Eventually I get them all. There may be a few very, very tiny flakes, but I've never had problems. Then I pour in part B and proceed in the same manner as with A.

Usually by the time I'm finished, I don't see any flakes. I use a strainer-funnel to fill the brown glass jugs I store the concentrate in, and if there are some very minute flakes, the funnel usually catches them.

I've been doing this since beginning developing film on my own, which was about in 2006. I've yet to had a problem with this, and have routinely had XTOL last for a year before all of it has been used up.
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Old 01-22-2012   #11
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I agree that the most likely source of problems here is not dissolving part A before adding part B. Was the water distilled or deionised? In water with ions I would say it is possible that the flakes were precipitated chelated divalent cations. Xtol contains several chelators, intended to remove any calcium, magnesium, divalent iron etc ions and these occasionally precipitate when they have done their job. In distilled or adequately deionised water, however, this is unlikely to be the case.

We all know that Xtol requires more careful handling than other film developers, so the following will aid in preventing angst:
  • Do not mix Xtol at over 85F/30C. There are some temperature-sensitive components in the developer that are critical to its activity. You will probably be fine most of the time, but you occasionally might not. To dissolve part A, stir and keep stirring, carefully, to avoid dissolving bubbles into the solution.
  • If you strain the mixed Xtol stock developer, make sure that the strainer is made of something non-reactive. The Paterson filter contains a metal mesh, but it seems to be a very high grade stainless steel, which is non reactive. Any reactive metal will add ions that can cause the Xtol to oxidise and it won't develop the film properly.
  • Use good water, and store your mixed Xtol in airtight bottles with as little air in them as you can. Store them in the dark.
If the photos are important to you, the process to make them appear reliably should be too.

Marty
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Old 01-22-2012   #12
Tim Gray
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I just want to stress that I have no problems getting everything dissolved properly in distilled water. And that when I pour the mixed developer into bottles, it is clear. The flakes come later for me, in storage. Which is dark by the way.
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Old 01-22-2012   #13
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Quote:
Originally Posted by Tim Gray View Post
I just want to stress that I have no problems getting everything dissolved properly in distilled water. And that when I pour the mixed developer into bottles, it is clear. The flakes come later for me, in storage. Which is dark by the way.
This is curious; I have no idea what this might be, neither have I ever seen it. I will ponder.

Marty
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Old 01-22-2012   #14
Ljós
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Marty,

thanks for your detailed input!

Quote:
Originally Posted by Freakscene View Post
I agree that the most likely source of problems here is not dissolving part A before adding part B. Was the water distilled or deionised? [...]
It was distilled and demineralised water. (On the label it says it was demineralised according to German standard VDE 5010.)
I will heed the advice to give more time for part A to completely dissolve next time.

In the meantime I have enlarged some negatives, und they look just fine. I developed three tanks so far, all six films (HP5plus) were (on purpose) more or less underexposed because of dire light situations - exposed as if it were between about 640 and 1600. Therefore I went for XTOL 1+1 for 16minutes for the two rolls that were underexposed most, 14 minutes and 12 minutes respectively for the rolls were the light was better. Agitation was the Ilford scheme I am used to (after initial agitation four inversions every minute). All in all from what I can see so far, and the filtration I needed (30 yellow), I can reduce developing time. Probably 10 to 11 minutes in 1+1 for "normal" exposure at 400, we'll see.

Tonality and grain structure look good so far, but I will have to enlarge more negatives from different rolls in different light to form an opinion.
First impression:
Overall I think I see a tad more speed than with HC-110 dil. B, that would certainly be welcome.

Greetings!
Ljós
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Old 01-25-2012   #15
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Glad to hear that they look fine.

VDE 5010 deionised water will not make flakes appear in Xtol stock from precipitation of cations captured by the chelating agents.

I'm still thinking, but can't be sure what might cause Tim's problem. No-one has ever explained Xtol's development behaviour to me fully, so it's entirely possible that other unexplained behaviours might emerge.

Marty
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Old 01-25-2012   #16
Michiel Fokkema
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I noticed getting flakes when i stored the made up Xtol colder then romo temperture.
Might be crystallization. If I warmed up the flaky Xtol again the flakes disappeared after some time.
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Old 01-25-2012   #17
Tim Gray
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Quote:
Originally Posted by Michiel Fokkema View Post
I noticed getting flakes when i stored the made up Xtol colder then romo temperture.
Might be crystallization. If I warmed up the flaky Xtol again the flakes disappeared after some time.
That could be what happens to me. Not sure. But it can get pretty cold in my apartment.
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Old 01-25-2012   #18
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Same experience here, taking the bottle from the storage place, where its cool (8 celsius) I notice some flakes. Taking it inside and making my solution its getting to room temp (20 celsius); no flakes absolutely cristal clear.
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Old 01-25-2012   #19
Ljós
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Thanks to you all for your contributions!

In the meantime I have developed some more rolls with the "flaky" XTOL and everything is looking very good. Also the prints do not show any "defects" in the negatives that I could see.

Dialling in the developing now, I used 12 minutes in 1+1, the time usually recommended for "straight" development of HP5plus (EI 400, normal contrast) for films that needed some extra development (EI 800-1000), and that seemed to have been enough. I am printing with Focomat Ic with condensor (but modified head: Dunco Multigrade via Kienzle adapter.)

If I may add another question: 100ml stock of XTOL are recommended for every 135 film. Using a Jobo 1520 with 485ml capacity, XTOL 1+2 would fall short a bit of this rule, giving only about 80ml stock. Now, knowing from my years spent with Rodinal I know that there is always a safety factor built in in these manufacturer's recommendations, so I should be fine.

But: has any of you experience with going 1+2 in a about 500ml tank, and/or: just how visible are differences between 1+1 and 1+2? The largest I routinely print is 18x24 centimeters.

Liking the XTOL experience so far, whether I stay with it or not it is good to know there is an alternative to HC-110 for me. I have tried Ilford DD-X with HP5 before and know it is great, but also too expensive for the volumes I shoot. Looks like XTOL will give me many of the advantages DD-X has over HC-110 at a much cheaper price.

Greetings,
Ljós

Last edited by Ljós : 01-25-2012 at 06:52. Reason: typo
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Old 01-25-2012   #20
Michiel Fokkema
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I'v compared Xtol to DD-X and couldn;t find a difference.
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Old 01-25-2012   #21
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Quote:
Originally Posted by Ljós View Post
If I may add another question: 100ml stock of XTOL are recommended for every 135 film. Using a Jobo 1520 with 485ml capacity, XTOL 1+2 would fall short a bit of this rule, giving only about 80ml stock. Now, knowing from my years spent with Rodinal I know that there is always a safety factor built in in these manufacturer's recommendations, so I should be fine.
I'm guessing that bit doesn't have much of a safety factor built in. Remember, Kodak stopped recommending dilutions higher than 1+1 because so many people were having issues with them, most likely because there wasn't enough active developer.

Then again, maybe you'll be ok. Personally, I'd drop down to one roll per tank or get a bigger tank. Also, personally, if I was experimenting with higher dilutions than 1+1, I'd go right to 1+3 and skip 1+2. I'm not sure if 1+2 provides enough of a benefit over 1+1 to bother with it.
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Old 01-25-2012   #22
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Quote:
Originally Posted by Ljós View Post
If I may add another question: 100ml stock of XTOL are recommended for every 135 film. Using a Jobo 1520 with 485ml capacity, XTOL 1+2 would fall short a bit of this rule, giving only about 80ml stock. Now, knowing from my years spent with Rodinal I know that there is always a safety factor built in in these manufacturer's recommendations, so I should be fine. But: has any of you experience with going 1+2 in a about 500ml tank
It depends on what film you use. I mix my Xtol in deionised water with very neutral pH and I can reliably develop four rolls of Neopan 400 or Tri-X in a litre of Xtol 1+3 (about 62.5 mL/roll) but it doesn't work with TMZ, Delta 3200, Acros or TMX. Kodak originally said to use a minimum of 80mL / roll but revised it up after users reported problems and the Kodak lab was easily able to replicate the same problem with TMX.

Quote:
Originally Posted by Ljós View Post
and/or: just how visible are differences between 1+1 and 1+2? The largest I routinely print is 18x24 centimeters.
I mostly use Xtol diluted 1+3 to get a more manageable development time. I like times of around 10-12 minutes if I can get them, to improve consistency. I doubt you'll see much difference in an 18x24 cm print.

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Precipitation!
Old 01-25-2012   #23
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Precipitation!

The flakes could be because of precipitation in cold temperatures. The reason I wouldn't see that is that my Xtol stock is stored at 20C.

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