Ilford Wash Procedue

Discussion in 'Darkroom Developing and Printing' started by Steven Woody, Jun 16, 2007.

  1. Steven Woody

    Steven Woody Guest

    by searching the net, i've got know that the Ilford introduced a
    invised wahs procedure which use three tanks of fresh water with
    agitation rather than using all the time running water.

    i think i like the method because it save water and don't ask for any
    washing gear. but it seems the method is designed for non-hardening
    fixer. so i want to ask:

    1, does the method still valid if what i used is a fixer such as
    Kodak F-6a. should i modify the procedure?

    2, if i switch to use non-harding fixer, such as Ilford's rapid
    fixer, will it bring any harm on those legendary films such as kodak
    Tri-X ?

    another question is, if i also want to use washaid in the overall
    process, how do i modify the Ilford's procedure?

    thanks in advance.

    -
    woody
     
    Steven Woody, Jun 16, 2007
    #1
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  2. Wash aids, as you called them were invented after someone found that
    washing film in salt (ocean) water worked a lot better than washing
    them in regular water. Probably someone on a ship. :)

    I've used various ones since the 1960's with all sorts of film and
    fixers.

    I think the bottle I currently have was made by Tetnal. Kodak makes (made?)
    one called "Hypo Clearing Agent". There are lots of them around and they
    all basicly work the same way.

    Rinse the film for 1 minute, soak in chemical for a minute, was for 5
    minutes. I think that was for "archival" processing, for "regular",
    it was 30sec rinse, 30sec soak, 1 minute wash.

    The new low water methods are not much different. Instead of constant flowing
    water, they are fill and drain, fill and drain. This makes it more reliable
    than guessuing the flow rate of the running water.

    Geoff.
     
    Geoffrey S. Mendelson, Jun 16, 2007
    #2
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  3. Geoffrey S. Mendelson spake thus:
    Yes; U.S. Navy, WWII. (Right, Richard?)
    The simplest, if you can get it, is plain old sodium sulfite. Cheap &
    easy to use. That's what most HCA is, anyhow.


    --
    Any system of knowledge that is capable of listing films in order
    of use of the word "****" is incapable of writing a good summary
    and analysis of the Philippine-American War. And vice-versa.
    This is an inviolable rule.

    - Matthew White, referring to Wikipedia on his WikiWatch site
    (http://users.erols.com/mwhite28/wikiwoo.htm)
     
    David Nebenzahl, Jun 16, 2007
    #3
  4. Both Kodak and Ilford have instructions for washing
    using successive baths of water. This is quite useful when
    there is no running water and is conservative of the water.
    Kodak uses about 6 baths of constant time, Ilford uses fewer
    baths with the time in each bath starting out short and
    becomming longer. The total time for either is about the
    same but the Ilford method probably uses less water while
    the Kodak system is easier to keep track of. The overall
    time is about the same as it would be for a running water
    wash.
    The use of a sulfite wash aid like Kodak Hypo Clearing
    Agent reduces the wash time for film by about 6 times. The
    normal wash time for untreated film in running water is
    about 30 minutes. After a two minute treatment in KHCA the
    required time is only 5 minutes.
    Kodak HCA and the current Ilford product are probably
    identical or nearly so. Kodak has published a technical
    paper on KHCA and there is some additional information in
    the patent. While the solution is mostly Sodium Sulfite
    Kodak has added Sodium Bisulfite as a buffer and two
    sequestering agents: EDTA Tetra-sodium salt, and Sodium
    Citrate. The solution is buffered to neutral pH. At this
    value the hardening produced by white alum hardening fixing
    baths is not destroyed but the mordanting effect of the alum
    for thiosulfate is. Also, at neutral pH the electric charges
    in the gelatin are such as to repel the thiosulfate ions
    rather than to attract them as it does when acid. The
    Sulfite acts as an ion exchange agent displacing the
    thiosulfate ions and fixer reaction products which may not
    wash out without it. This compensates to some degree for
    partially exhausted fixing baths. The purpose of the
    sequestering agents is to prevent the deposition of Calcium
    and Magnesium salts from hard water on the film and to
    prevent sludging from carried over alum.
    The research leading to KHCA was an extension of work
    done to discover why sea water was more efficient than fresh
    for washing photographic material. While this fact was known
    before 1900 the reasons remained something of a mystery
    until the middle 1950's. Sea water washing was extensively
    used, especially by the Navy aboard ship, during WW-2. A
    fresh water rinse is necessary after the use of sea water
    because the halides remaining in the emulsion will quickly
    destroy the image. However, little water is needed for this
    rinse so the method is very conservative of fresh water. The
    use of a sulfite wash aid like KHCA is even more effective
    than sea water and much more effective than the old trick of
    treating film or paper with a mild alkaline bath.
    Check the Kodak and Ilford sites for specific
    instructions about the sequential bath washing but for the
    Kodak method the time is about 5 minutes in each bath with
    constant agitation in each. If KHCA is used I suggest at
    least two shorter baths to a total time of about 5 minutes.
    This same system will work for paper. RC paper washes out
    very quickly without a wash aid so probably two or three
    short baths with a total time of around 5 minutes will do.
    Fiber should be treated in KHCA and washed for the total
    times recommended using about 5 minute baths.
    The sucessive bath method is fully as effective as
    running water washing.
     
    Richard Knoppow, Jun 16, 2007
    #4
  5. Steven Woody

    dan.c.quinn Guest

    I use the Ilford sequence in a relaxed manner. The 5-10-20 inversion
    sequence is done a few inversions at each fill up and at least those
    number of inversions are completed prior to the next fill-up. Some
    still time is allowed while I clean-up around the darkroom. Photo
    Flo rinses of film and eight blade film squeegee are last.

    Films have been pre-hardened for many years. IMO, do without
    hardener. A fresh fix of sodium thiosulfate alone will do the job.
    Try a good half ounce, 16 grams, of the anhydrous in 500ml
    of water. Allow 10 minutes with more of less continuous
    agitation. Easy fresh fix each film or films. Dan
     
    dan.c.quinn, Jun 17, 2007
    #5
  6. Hardener is not necessary for many films. Also, the
    shorter fixing times required by "rapid" fixers probably
    don't give the hardener enough time to work anyway.
    If a sulfite wash aid is used there is no difference
    between wash time for hardening or non-hardening fixing
    baths. Its not the "hardness" of the emulsion but the
    mordanting effect of the common White Alum hardener which
    causes the increase in washing time plus the acid condition
    needed for the hardener to work. The pH adjustment made by a
    Sulfite wash aid affects both of these factors as I
    mentioned in my last post. Ideally, the pH of the emulsion
    should be about neutral. At neutral pH the hardening is
    preserved (sometimes it _is_ desirable) and the emulsion is
    raised above its isoelectric point where the thiosulfate is
    no longer attracted to the emulsion by charge.
    A non-hardening or "plain" fixing bath should have some
    Sodium sulfite in it to act as a preservative for the
    thiosulfate and also to counteract staining from any carried
    over developer. In an acid fixing bath the developer is
    immediately inactivated but it will remain active for a time
    even in a neutral fixer and especially in an alkaline fixing
    bath. Film or paper to be fixed in a non-acid bath should be
    very well rinsed after developing. Again, there is an
    advantage to the use of an acid fixing bath because it
    allows the use of an acid stop bath instead of a plain water
    rinse. The acid stop bath immediately stops development
    without any chance of staining from diluted developing
    agents as is possible in a plain water stop bath.
    For a plain fixing bath about 5 grams/liter of Sodium
    Sulfite is enough. The much larger amount, typically 15
    grams/liter, found in acid fixers is because the Sulfite
    must also preserve the thiosulfate from being decomposed by
    the acid. It is the reaction between the sulfite and acid
    which results in the odor of Sulfur dioxide which is common
    for fixers and which many people find very irritating.
    Non-acid, non-hardening fixing baths are perfectly
    satisfactory provided that an adequate rinse is given
    between developer and fixer, an actual short wash rather
    than just a few seconds in a tray of water.
    Even though a neutral fixing bath will result in
    significantly shorter wash times than an acid hardening
    fixing bath the use of a wash aid will further shorten the
    wash because of the specific ion exchange property of
    Sulfite for thiosulfate and some fixer reaction products.
     
    Richard Knoppow, Jun 17, 2007
    #6
  7. Steven Woody

    Steven Woody Guest

    thanks for replies from all you folks! but i still get below
    questions not so clear:

    1, you folks tend to think hardening fixer is not neccessary for
    films because most of modern films are already pre-hardened. is it
    true for traditional Kodak 400TX roll films? and, is it true for RC
    and FB papers?

    2, i still got bottles of Kodak F-5 which is a kind of hardening
    fixer, and i still want to use it. below are a fill-and-drain style
    of prededure i designed after study your replies and Ilford's method,
    would you give opinions about if it is okay?

    step 1, fix using Kodak F-5
    step 2, rinse using clear water, 30 secs.
    step 3, washaid ( Ilford washaid or Kodak's Hypo-Clearing Agent ), 1
    to 2 minutes
    step 4, drain and fill tank with clean water, invert it 5 times
    step 5, drain and fill tank with clearn water, invert it 10 times
    step 6, drain and fill tank with clean water, invert it 20 times.
    step 7, Kodak phot-flo, 30 secs.

    some notes about above precedue,

    a, step 4 to step 6 are directly copied from ILford's method which
    assumes that fixer is non-hardening and no washaid was used.
    b, the time for step 3 is directly copied from Kodak's publish for
    some films including 400TX.
    c, if i use non-hardening fixer, step 1 and step 3 can be skipped, am
    i right?

    3, Richard, after searched Kodak's site, i've not yet found publishes
    about what you menthioned the wash method Kodak introduced which, you
    said, is similar to Ilford's method. would you please give me an URL?
    thanks.

    5, about the one-shot plain fixer, would anyone please give me an
    exact formular? i like to try it some times later.

    thanks in advance.

    -
    woody
     
    Steven Woody, Jun 17, 2007
    #7
  8. Steven Woody

    Digitaltruth Guest

    1, you folks tend to think hardening fixer is not neccessary for
    Unless a material or process specifically recommends use of a
    hardener, you should avoid using one. Kodak Tri-X 400 does not require
    a hardener.
     
    Digitaltruth, Jun 17, 2007
    #8
  9. Steven Woody

    Steven Woody Guest

    thanks a lot. i still looking for replies on the others questions.
     
    Steven Woody, Jun 17, 2007
    #9
  10. What would be the negative effects of using a hardener for a film that
    does not recommend the use of hardener? I'm asking because I mixed a
    fixer with hardener for EFKE KB25 and I'd like to use the same fixer
    for Tri-X 400 (135mm) that I'm going to develop next, but of course if
    it's going to cause problems I'll have to make another fixer for
    Tri-X.
     
    Toni Nikkanen, Jun 17, 2007
    #10
  11. Steven Woody

    John Boy Guest

    Rinse the film quickly, do the anti-hypo thing, then hang the reel on a
    t-stick and stick it in the toilet. Flush six times with one minute
    between flushes. Done.

    I'll bet the archive fanatics are rolling over in their soup now.
     
    John Boy, Jun 17, 2007
    #11
  12. Steven Woody

    dan.c.quinn Guest

    One-shot plain fix. There are two versions of plain fixer, plain
    and
    very plain. Plain has a little sulfite added while very plain is
    nothing but
    sodium or ammonium thiosulfate.
    The 16 gram or half ounce plus suggestion I made is a good starting
    point. I intend to use that on a first roll of Acros 120 and expect
    good results.
    May take 10-12 minutes with off and on agitation. It will be used
    fresh so
    I don't bother with the sulfite. Also no stop of any sort; one-shot
    fixer.
    If you've a usual sort of rapid concentrate on hand try 20ml. All
    solution
    volumes are 500ml, one roll of film. After fixing it's down the drain.
    One-shots can be prepared ahead in some quantity and amount each.
    This evening I've four small prints to make. I'll prepare a print fix
    ready for
    a four way dilution. No used or ageing fix hanging around. Dan
     
    dan.c.quinn, Jun 17, 2007
    #12
  13. Hardening fixers became standard practice in the
    early 1930s because emulsions were soft enough to have
    problems with frilling and other damage during washing. Note
    that the hardener works only when the film is wet.
    Essentially, it reduces the amount of swelling. Methods of
    improving the resistance of emulsions to mechanical damage
    were made continuously from the 1930s (if not before) until
    nearly the present. Up to about 1940 the standard processing
    temperature was 65F, improvements in emulsion hardness
    allowed that to be increased to the familiar 68 f about that
    time. Some current B&W emulsions are hardened like color
    film to withstand 100F processing. Among these films are the
    Kodak T-Max series.
    This hardening is partially due to the addition of
    plastics to the emulsion. Even though research has been
    carried out for a century to find a substitute for animal
    gelatin for emulsions nothing has been found which works
    nearly as well but other substances have been found which
    can be added to it for improving, for instance, mechanical
    properties.
    Not all films and papers will withstand high
    temperature processing or are resistant to damage when wet.
    Hardeners in the fixing bath really do not do any
    damage and can be used routinely. However, the fact that the
    fixing bath must be acid for the hardener to work, and the
    properties of the usual White Alum (to distinguish it from
    Chrome Alum, a non-related chemical also used as a hardener)
    result in the gelatin binding Thiosulfate ions and some
    fixer reaction products.
    Gelatin is amphoretic, that is, it is neither acid or
    alkaline but has properties of both. Gelatin takes on the pH
    of the last bath it was in. However, it has a sort of
    preferred pH called the isoelectric point. This is the pH
    where the gelatin molecules have no net elecrical charge.
    For most photographic gelatin the isoelectric point is very
    slightly on the acid side of neutral. At the isoelectic
    point the swelling of the gelatin is minimum.
    When an acid hardening fixing bath is used the residual
    Alum binds thiosulfate and fixer reaction complexes in a
    fasion known as mordanting. This is the way dyes are bound
    in fabrics to keep them from bleading. The mordanting effect
    takes place only in a window of pH on the acid side of
    neutral. At neutral or alkaline pH the mordanting is no
    longer effective. If the emulsion is made more than slightly
    alkaline the hardening effect of the alum is lost. The
    gelatin pH is also important in binding thiosulfate and
    complexes due to electric charges in the atomic structure of
    the gelatin. Everyone knows that opposite charges attract
    and similar charges repel. The electric charge in gelatin is
    related to its pH. As stated above at the isoelectric point
    the charges are balanced so there is no net charge. On the
    acid side the charges are so as to attract the thiosulfate
    ions and some complexes. If the gelatin is made slightly
    more alkaline than its isoelectric point the charges will be
    such as to repel so washing out is accellerated. The charge
    effect takes place even if a hardener is not used.
    It has long been known that treating an emulsion in a
    weak alkaline bath accellerates washing. It does so by
    breaking the mordanting of alum hardener (when it is used)
    and adjusting the pH of the gelatin to the alkaline side of
    the isoelectric point. However, the gelatin needs only to be
    made neutral to obtain both of these advantages and,
    further, will have minimum swelling at that point.
    The use of Sodium Sulfite and other Sulfites as wash
    aids was discovered at Kodak Reserach Labs in the mid 1950's
    as the result of research into sea-water washing. Sea water
    will wash out Hypo in about half the time of fresh water but
    itself must be washed out with fresh water. Sea water
    accellerates washing more than a simple aklaline solution
    such as a 2% solution of Sodium carbonate or Borax so they
    decided something else beyond simple pH change was occoring.
    This was discovered to be an ion exchange effect. Some ions
    will actively displace others. Kodak discovered that
    sulfites have a very strong ion exchange action for
    thiosulfates and thiosulfate-silver complexes. The basic
    wash aid was a 2% solution of Sodium sulfite. However, it
    was also found that by neutralizing the solution the gelatin
    was brought close to its point of minimum swelling.
    According to Kodak this results in the shortest diffusion
    path for the unwanted ions to reach the surface and be
    washed away. Also at neutral pH the hardening effect of
    white alum is preserved but its mordanting effect is broken.
    So, there is good reason to buffer the solution.
    Because the fixing properties of hypo are not affected
    by pH it is possible to make a neutral or alkaline fixing
    bath. Either results in faster washing than an acid fixing
    bath whether hardening or not. However, a neutral or
    alkaline fixer will still result in longer washing than if a
    sulfite wash aid is used because of the ion exchange
    property of the sulfite.
    Since treatment in a sulfite wash aid will give the
    shortest wash times regardless of the type of fixing bath
    used it is, in general, a good practice to use it.
    Acid fixing baths do have one virtue, they allow the
    use of an acid stop bath which stops developing action
    instantly and even if there is developer carried over to the
    fixing bath it is inactive. While many have perfectly good
    results using a neutral or alkaline fixing bath and a water
    rinse stop this still has a slight risk of increased
    development and staining. The last is probaby more a risk of
    the water stop than of the fixing bath since any fixing bath
    should contain some sulfite to preserve the hypo and that is
    usually sufficient to prevent staining from developer
    reaction products.
    In short (I seem to be running very long today) there is
    NO damage done by using a hardening fixing bath. The longer
    wash times can be eliminated by the use of a sulfite wash
    aid. There may also be no advantage to the use of a
    hardening fixing bath especially for already well hardened
    films and most modern papers.
    If one looks at the recommendations for fixing time
    given in old books one finds times like 15 or 20 minutes
    recommended. These long times were partially due to the
    assumption that partially exhausted fixer would be used but
    also it was to give the hardener a long enough period to
    work. Where relatively short fixing times are used a
    hardening fixing bath probably does not do much hardening
    anyway.
    Of this slightly but it should be mentioned: The
    capacity of a single fixing bath, whether Sodium or Ammonium
    thiosulfate is quite limited. The use of two successive
    baths is strongly recommended. It is important to the
    permanence of a negative or print that _all_ the unused
    halide in the emulsion be washed out. The purpose of the
    fixing bath is to convert the insoluble halides to a soluble
    form. Some of this comes out in the fixing bath and some in
    washing. The conversion is a step-wise process the halides
    becoming progressively more soluble. Incompletely converted
    complexes will not wash out and remain in the emulsion where
    they will eventually destroy the image. The ability of the
    fixer to complete the conversion depends on the number of
    free thiosulfate ions available. It takes about three
    thiosulfate ions to convert one molecule of silver halide.
    Once the complexing occurs the thiosulfate ions are no
    longer available. By using two baths the bulk of the
    conversion is done in the first bath leaving the second one
    relatively free of dissolved silver and in condition to
    complete the conversion of any halide left over from the
    fist bath.
    Since a sulfite wash aid will also eliminate the binding
    of some insoluble complexes it gives further assurance of
    complete fixing.
    A further note: Compete fixing is more important to
    image life than complete washing. It was discovered about
    1960 (simutaneously at Kodak and Fuji) that a very small
    residue of thiosufate remaining in the emulsion protected
    the image from oxidation from air-borne peroxides. While
    this is hard to quantify it is taken into account in the
    wash times recommended by Kodak when its wash aid is used.
    The heroic overnight soaks, etc, suggested in some older
    books in not necessary and should be avoided. These long
    washes actually reduce image life plus they can damage the
    emulsion and, in the case of fiber paper, the support.
     
    Richard Knoppow, Jun 18, 2007
    #13
  14. FWIW -- my paper washing experience.

    Most of my work is on DW fibre. I fix with rapid fix
    (Arista/Ammonium Thiosulfate). Fix for 1 minute, holding
    water bath for a few hours, second fix bath, Farmer's
    (sometimes), Selenium, Rinse and hypo clear. I wash in a tray
    with warm water, a water change every 1-10 minutes. I test
    for washing with Kodak's HT-2 residual fixer test and
    wash until there is _no_ stain on a test print.

    With Kodak brand KHCA the prints wash out in 20 minutes or so,
    ~5-10 changes.

    With Perma Wash it takes 1 hour+, ~10-20 changes, and
    there is still a very faint stain.

    I am rather surprised by this, but it has been the
    case on two bottles of the stuff.

    I notice most www'ers use Perma Wash only for film,
    without much reason stated.

    Anyone else with similar/different results?
     
    Nicholas O. Lindan, Jun 18, 2007
    #14
  15. Steven Woody

    Steven Woody Guest

    hi, dan

    did you mean 16 gram sodium thiosulfate in 500ml for one roll of 120
    film? how did you calculate that? i like to know any reasoning.
    and, for one sheet of 8x10 paper, what's the amount for sodium
    thiosulfate and water?

    on the other hand, you said 10-12 minutes of fixing time, you know,
    Kodak F-5 suggests 9 minutes. again, why you think the one shot fixer
    need 10-12 minutes?

    thanks.

    -
    woody
     
    Steven Woody, Jun 18, 2007
    #15
  16. Steven Woody

    Steven Woody Guest


    Hi, Richard

    thanks for your inputs, it's very in-depth coverage of the subject.
    up to my understanding, you points are mainly:

    1, hardening fixing makes no damage in any way;
    2, hardening fixing makes no advantage on most modern films and
    papers;
    3, hardening fixing will take longer time to wash unless wash aid is
    used;
    4, acid is necessary for two reasons: (a) it is necessary when using
    hardening fixer because the hardener has to be work in acid solution.
    (b) it allow using of acid stop bath
    5, wash aid is useful not only because it can shorten fixing time but
    also i give further assurance of compete fixing.

    to me, because i most likely process no more than 3 rolls one moth, so
    i still look for one shot solution of fixing. because it is for one
    shot usage, i think the formula should as simple as possible and the
    amount of each ingredient should be as less as possible.

    after study your inputs, i think i can decide,

    1, use no hardening fixer because this will elminate at least one
    ingredient --- alum.
    2, use wash aid
    3, because there will be no hardener in the formula, so i tend to
    remove acid too. but, you said the acid solution allow using of acid
    stop bath which is important in preventing incresed development from
    happening, so i want to ask you, if i decide tol use acid stop bath,
    what do i do to still use non-acid fixer? will it work if i insert 5
    seconds of wather rinse after stop bath and before fix bath?
    5, because i dont store the fixer, so i think i can further remove the
    sodium sulfite. now only one thing left in the formula, that is sodium
    thiosulfate only.

    is the above okay? if so, how many sodium thiosulfate do i need for
    fixing one roll of 120 film in 600 ml solution? and, how many the
    same thing do i need for fixing a sheet of 8x10 paper in 900ml
    solution?

    thanks in advacne.

    -
    woody
     
    Steven Woody, Jun 18, 2007
    #16
  17. The MSDS for Permawash claims a trade secret for its principle
    ingredient. It does contain Ammonium sulfite. By memory, this is one
    of the salts mentioned in the Kodak patent. It is the anion rather
    than the cation which is important and the patent lists several
    sulfite salts.
    I don't know why Permawash should be innefective but its
    interesting to read your experience with it. The ingredients of KHCA
    are pretty well known. The formula in the patent is not quite the same
    as the MSDS mainly in that it does not have sodium citrate, a
    sequestering agent. The patent formula lists only EDTA tetra-sodium
    salt but the commercial product also has sodium citrate. The purpose
    of the sequestering agents is to preclude the deposition of mineral
    salts from hard water or a sludge of aluminum salt from alum hardener
    on the emulsion. Otherwise KHCA is a neutral solution of Sodium
    sulfite and Sodium bisulfite. The amount of the bisulfate might have
    to be adjusted to account for the sequestering agents although they
    are present in relatively small amounts.
    I will post the patent number later for those interested. I am
    away from home at the moment and do not have access to my references.
     
    Richard Knoppow, Jun 18, 2007
    #17
  18. Better than filing for a patent. But the 'trade secret' doesn't
    have to be anything but a secret. It doesn't have to work - could
    be table salt or wetting agent.
    Which tells you (or is supposed to tell you) just how to make
    KHCA. The purpose of patents is to reveal what would otherwise
    be trade secrets (a purpose I agree with), not 'protect the inventor'
    (a purpose that makes no sense at all). "My invention is protected
    by a patent!" - yeah, right...
    It appears to contain 1/2 the amount of sulfites, with Ammonium
    Sulfite instead of Sodium Metabisulfite.
     
    Nicholas O. Lindan, Jun 18, 2007
    #18
  19. Richard Knoppow wrote (in part):

    Must be a typo. Sodium bisulfate would make the solution quite acidic, IIRC.
    Is that not the active ingredient in toilet bowl cleaners?
     
    Jean-David Beyer, Jun 18, 2007
    #19
  20. Steven Woody

    Steven Woody Guest

    hei richard, please help :)
     
    Steven Woody, Jun 18, 2007
    #20
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