Xtol shelf life? Particles floating on bottom of bottles..

Discussion in 'B&W: Film, Paper, Chemistry' started by Ihmemies, Mar 2, 2010.

  1. Ihmemies

    Ihmemies Member

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    I store my xtol in plastic soda bottles. Once I developed a roll of Neopan 1600 with about 5 month old xtol. It came out severely underdeveloped, and when looking at the bottle I saw some kind of white, fungus-like particles floating on bottom of the bottle. I dumped rest of it and nearly thought of stopping using xtol completely.

    I still had a extra 5l set of xtol though to get rid of, so one day I mixed it. Now it's maybe 2-3 months old, and I have two unopened, full 1,5 liter soda bottles of xtol left.

    I thought of developing a few rolls today, and when examining the bottle I saw these same kind of particles floating on bottom. I'm very hesitant to try to develop anything with that kind of looking stuff again, so....

    What I am doing wrong? Kodak promises at least six months of storage life, but I've never gotten it myself. Do the soda bottles suck? How much storage temperature affects it? It has been around 20-26C depending on time of year. I must be doing something wrong since other people have so good experiences with xtol.

    When turning the bottle around now it's naturally full of that stuff... took a photo:
    [​IMG]
     
    Last edited by a moderator: Mar 2, 2010
  2. Fred Aspen

    Fred Aspen Member

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    I had the same trouble with Xtol until I mixed with distilled water (my water is about 40 gr. of hardness!) and stored in glass containers. Plastic containers do 'breathe,' as it were, and eventually air oxidizes the developer.
     
  3. Ihmemies

    Ihmemies Member

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    So basically tap water is not ok, neither are plastic bottles. Great :tongue:

    Might as well use dd-x & rodinal while considering if I should ever buy these kind of developers you need to mix yourself again... Hauling distilled water from god knows how far away, buying glass bottles, removing the excess air or replacing it with some gas is just not my cup of tea.
     
  4. fotch

    fotch Member

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    Not trying to be a SA but, how far is civilization from you? You had to haul the bottles your using now so hauling glass would be a one time event.

    If you fill to the brim and use a Saran wrop cover before screwing on the cap, you should not need to use Nitrogen. Kodak I believes makes their chemicals to use tap water but the quality of that can vary.

    Do you have the problem with any other powder to mix formula's like D76 or ID11? You can also try running the Xtol thru a coffee filter prior to use. This may be a good idea for any product anyway.

    Good luck.
     
  5. Ihmemies

    Ihmemies Member

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    I don't mind glass bottles, but if the tap water is not good enough and I needed to haul water, that isn't very funny.

    Maybe I need to try to source glass bottles somewhere and google what a Saran wrop is. What one does with half-full bottles, or should I plan my developing so that I use a bottle till it's empty in one session?

    Xtol is the only powder chemical I've used so far. Would that kind of looking xtol work if I ran it through a coffee filter? (I don't drink coffee but buying those isn't a problem :smile:
     
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  6. hrst

    hrst Member

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    If it doesn't work anymore, using a coffee filter won't recover it. It just removes the crud.

    Ihmemies, "Saran wrap" is Elmu-kelmu in Finnish :wink:. The purpose here is to make the lousy cap tight.

    This is very surprising and XTOL mixed in same tap water (in the same city as Ihmemies) and stored in the same kind of PET bottles has always been fine for 6 months for me. 2-3 months sounds unbelievable. There shouldn't be so much iron here, either.
     
  7. Fred Aspen

    Fred Aspen Member

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    Xtol mixed with my tap water expired in 2-3 months, regularly. I did go to glass but the problem wasn't truly solved until I bought the distilled H2O. Now it meets Kodak spec.
     
  8. Laurent

    Laurent Subscriber

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    I mix X-Tol with demineralized (??? not exactly distilled, hope this is the right word) and have no issue, except the white thingies that float on the glass bottles from time to time...

    I'm not sure it takes me more than 2/3 months to fully use a 5 litres batch though
     
  9. Namir

    Namir Member

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    somehow looks like my xtol... (maybe I have slighlty less particles). I do use demineralized water and glass bottles. recently bought them new, produced in cleanroom, (-> medicine bottles). Have had the same probs with D-76 and Calbe A49. (Maybe the problem is me...) This time I noticed this fallout only some days after mixing it... So I proceeded as I did with Calbe A49 and D76: Simply ignoring the particles- And in my case it still works well (6 weeks after mixing it). As a precaution I make a check with a small piece of film every time I develop af film
    In my case the reason could be, that I do not mix it according Kodaks recommondations, I mix it slightly "stronger", (625/530), and in winter it is not really warm in our flat, but never below 17°, so actually this should be no problem.
    I am going to watch if it will have any discernable effect on the results, today's negatives look good.
     
  10. Ronald Moravec

    Ronald Moravec Member

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    Xtol needs to mixed with water up to the recommended hot temp, around 90 deg F. Don`t do the room temp stuff.

    Don`t store colder that 68 F/20 C. or you can get precepitation.

    decent glass bottles with well sealing caps are an investment every darkroom needs. Sometimes plastic works, sometimes not. Some plastic have an air impermiable membrane. All this is hard to tell by looking.

    Soda bottles need to be cleaned completely, not rinsed out.

    The exp date is important on Xtol. If the bag is past date, toss it. Even if it all goes into solution and looks good, the shelf life after mixing will be a week or so. It was a bad experience that Kodak resolved by dating the bags. My bag was before they were dated. They replaced the Xtol, buy my photos are gone forever.

    I now mix D76 a liter or two at a time. Always fresh, always works, cheap as dirt. T Max 100 and 400 are beautiful in D76. TMY-2 is shockingly good.
     
  11. Namir

    Namir Member

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    I just checked it out... it looks uglier than several weeks ago... D76 from last year still looks fine...
    I suppose anything that falls out actually is supposed to be solved... I will see, how the negatives print... and try to mix it with warmer destilled water the next time. Or change my developer...
    20°:
    3° below 20 in my case actually should not be that serious. (some people mix it double strength without any problems... If 20° would be the critical temperature, they would have to store it significantly warmer than 20° to have no fallouts...)
     
  12. Jedidiah Smith

    Jedidiah Smith Member

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    When I used Xtol and D76 in Alaska, I always mixed with tap water - and got the same white particles (the crud / floaters) that you get! :D I never thought back then to mix with any kind of "special" water. Hehe...guess I was too young to think about things like that at the time.
    But - it always worked. So, I don't think the particles are really your problem. It's probably the soda bottles. At the time I used dark brown plastic jugs from B&H, and they worked pretty well - kept for at least 4 months, but I always wanted glass.
    I'd say try some glass bottles and "special water" if you want maximum longevity! I know you want Xtol specifically, and I don't blame you because it's fabulous stuff, but you could try some HC-110 syrup if you shoot very little and just need a developer around all the time. That stuff's supposed to last forever! :D

    Jed
     
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  13. Ihmemies

    Ihmemies Member

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    I recall I used 30C water when mixing xtol. The xtol was fresh, dated 2011 or so. Kodak gives instructions like this:

    I'll try glass bottles next time, and maybe even try to get deionized water. My friend hrst said he could probably get the water from some lab at the university.
     
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  15. Simplicius

    Simplicius Member

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    3 observations as an xtol user who gets 6 months from it no problems.
    1: I use a filter jug and never have the particle issue, it's cheaper than buying water
    2: I use screw top wine bottles (seem to have an endless natural supply of them!) with saran wrap and the they are fine... not brown but still dark.
    3: I started getting better longeivity when I stored the chemicals in the hot press , this applies especially to winter as it's probably the most temperature consistent place in the house and also when I go to develop the base temperature is always around 18C so it doesn't take much time to get everything up to 20C.
     
  16. hrst

    hrst Member

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    I've done some storage testing with XTOL and one of the tests involved storing in refrigerator at 4C. This test didn't show any precipitation, but showed a great extension in shelf life. A test sample of 300 mL at the bottom of a 1 L bottle with air showed the same low level of oxidation than a 300 mL bottle without any air in room temp (23C). OTOH, the corresponding sample (300 mL in 1 L bottle with air) stored at room temperature showed a high level of oxidation.

    Other samples at room temp had butane and they showed oxidation between the extremes.

    The method of evaluation was visual inspection of yellowness, and developed test strips on film, scanned and measured for density in scanning software.

    The result of the test was that if air cannot be squeezed out completely, putting it in a refrigerator can be surprisingly good way to slow down oxidation and increase shelf-life. After all, most chemical reactions slow down in cold.

    There was no problems of precipitation. However, XTOL for this test was more dilute to speed up the expiration. Testing period was about 4 weeks IIRC.

    If something would precipitate so easily in lower than 20C, say, at 10C, which I don't really believe, it would probably dissolve back when taken to 20C or over for processing.
     
  17. Maris

    Maris Member

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    My 1 litre bottle of Xtol is still working consistently after 7 years and hundreds of films. All it gets is a replenishment of 90ml of fresh Xtol for each film and an occasional trip through a coffee filter to take out the white particles and other debris.

    I believe the white particles are calcium ascorbate but whatever they are I have never noticed any effect on developer performance.
     
  18. H. James Wolf

    H. James Wolf Member

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    As Maris said, replenished Xtol seems to last almost forever, even in the old hard rubber Kodak floating lid tanks. I have been using it well over 10 years both as replenished and one-shot and have never had it expire. That said, I mix it with distilled water and store it in brown glass bottles. I use the same mixing and storage for all developers, including D23, and have not had a problem with chemistry expiring.
     
  19. cmo

    cmo Member

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    My first experience with Xtol was ugly - I used tap water, and at that time I lived in a city where a lot of iron particles were in the tap water. There were little spots all over the negatives. Next time I bought 'demineralized' water in a 5 liter plastic canister, put the whole canister into a bucket filled with warm water until the content of the canister had the right temperature. Then I poured in the contents of the A and B bags, screwed the cap on the canister and started shaking it for a while. Then I allowed it to stand until the next morning, shaked it again, then filled it into glass bottles and added some butane gas (heavier than air, prevents oxidization). Now my Xtol now works fine for 6-8 months. I use it as a one-shot developer 1:1 or 1:2. There is a thread about using bag-in-box containers in this forum. In the meanwhile I heard from several people that they store their Xtol in these dirt-cheap containers, it lasts for a very long time.

    http://www.apug.org/forums/forum43/73184-bag-box-chemistry-storage.html
     
  20. ath

    ath Member

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    I think this is fungus. I had it in my stock XTOL solution, even when mixed with demineralized water. When I changed the stirring stick from wood to plastic they were gone.
    Currently I'm using XTOL I mixed last April. Latest after a year I dump it.
     
  21. Ihmemies

    Ihmemies Member

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    Really.. could that be the cause? I used a wooden stick too to mix the xtol in open bucket. Well, I think weirder things can happen :D
     
  22. fotch

    fotch Member

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    Wood is porous and would retain some of the chemicals mixed so probably should be discarded after use. Wooded tongs are usually color coded and at least would stay in the same type of chemical with use.

    I have several and all are plastic except one is stainless steel.
     
  23. markbarendt

    markbarendt Subscriber

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    I'm with Maris too.

    I mix my Xtol with distilled water from the grocery, I keep the stock solution in a wine box and working solution in an old 1.75 liter Margarita mix bottle, filter the working solution once in a while with coffee filters, and replenish at 70ml.

    No problems.
     
  24. StMichel

    StMichel Member

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    Very interesting indeed.

    I mixed five liters of XTOL a month ago, and as I had read from hrst's experiments earlier, I decided to leave one liter to the lab and put the rest to refrigerator to wait for use. I just don't shoot enough film to use five liters of developer diluted 1+1 in six months. I just checked the ones in the fridge, and they have same kind of fluffy goo as in Ihmemies's photo. I'm going tonight to the lab, I'll check the remaining developer there for the flakes, if I remember.

    I also mixed the developer with local (Espoo) tap water, so it's more than likely that the flakes are some kind of organic products. Mold, fungus, or something. It is quite clear to me that oxidation, or storage in soda bottles, have nothing to do with this stuff.

    I actually doubt that the flakey stuff hasn't got that much to do with your storage life problem, but it just happens to occur the same time. (Though, it also could be that the flake-causing-organic-creatures are consuming some vital developer component.) I will get back with my results when I have developed something in the refrigerated XTOL.
     
  25. clayne

    clayne Member

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    Not true.

    Also not true. Or at least, not at anything 10-20C.

    Anyways, I think this guy's issue is one of non-distilled water and containers which allow an ample exposure to light. One can buy 2gal of distilled water at any supermarket for around 2-3$. It's not that much an issue to worry about. Surely one can "haul" a gallon in each arm, or are we that lazy these days?
     
  26. Anon Ymous

    Anon Ymous Member

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    I've mixed Xtol with deionised water and got a very fine precipitate at the bottles. It doesn't cause me much concern though, I can always filter it. My batch wasn't exposed to light either, so that doesn't seem to be a cause. BTW, real distilled water requires a great amount of energy and 2-3$ for 2 US gals is a bit suspicious.