EP0605038A1 - Verfahren zum Bleichen und Fixieren von farbphotographischem Material mit niedrigem Silbergehalt - Google Patents

Verfahren zum Bleichen und Fixieren von farbphotographischem Material mit niedrigem Silbergehalt Download PDF

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Publication number
EP0605038A1
EP0605038A1 EP93203591A EP93203591A EP0605038A1 EP 0605038 A1 EP0605038 A1 EP 0605038A1 EP 93203591 A EP93203591 A EP 93203591A EP 93203591 A EP93203591 A EP 93203591A EP 0605038 A1 EP0605038 A1 EP 0605038A1
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Prior art keywords
photographic
silver
fixing
fixer
solution
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EP93203591A
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English (en)
French (fr)
Inventor
Richard Peter C/O Eastman Kodak Comp. Szajewski
John Michael C/O Eastman Kodak Company Buchanan
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Eastman Kodak Co
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Eastman Kodak Co
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Publication of EP0605038A1 publication Critical patent/EP0605038A1/de
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    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
    • G03C7/00—Multicolour photographic processes or agents therefor; Regeneration of such processing agents; Photosensitive materials for multicolour processes
    • G03C7/30—Colour processes using colour-coupling substances; Materials therefor; Preparing or processing such materials
    • G03C7/42—Bleach-fixing or agents therefor ; Desilvering processes

Definitions

  • This invention relates to the processing of color silver halide photographic recording elements. More particularly, it relates to the desilvering of a color silver halide photographic element using a peracid bleach and a sodium thiosulfate fixing agent.
  • the basic image-forming process of color photography comprises the exposure of a silver halide photographic recording material to light, and the chemical processing of the material to reveal a useable image.
  • the chemical processing entails two fundamental steps. The first is the treatment of the exposed silver halide with a color developer wherein some or all of the silver halide is reduced to metallic silver while an organic dye is formed from the oxidized color developer. The second is the removal of the silver metal thus formed and of any residual silver halide by the desilvering steps of 1) bleaching, wherein the developed silver is reduced to silver salts; and 2) fixing, wherein the silver salts are dissolved and removed from the photographic material.
  • the bleaching and fixing steps may be performed sequentially or as a single step.
  • Juxtaposed to the desire for an accelerated process is the desire for, and the need for, photographic elements and process solutions that require lower chemical usage and that generate less polluting chemical waste.
  • Used or spent fixer solutions are desilvered by electrochemical means to recover the semi-precious metal, but these solutions may still contain ingredients that limit their direct discharge into public waste water streams. Further treatment is required for them to conform to standards for environmentally acceptable disposal.
  • higher processing speed can be traded for an indirect advantage in the form of lower processing chemistry usage and lower processing waste per unit of photographic material processed.
  • a process which includes the ecological advantages of both a peracid bleach and a sodium thiosulfate fix is highly desirable; however, such a process has been thought to sacrifice speed in desilvering.
  • Photographic processes utilizing both a persulfate bleach solution, a species of peracid bleach, and a sodium thiosulfate fixer solution are incidentally disclosed as examples in U. S. Patents 4,448,878; 4,481,290; 4,458,010; 4,506,007 and 4,508,816.
  • These publications are directed at bleaching improvements and disclose numerous combinations of different bleaches with various fixers.
  • the sodium thiosulfate fixer solutions incidentally illustrated in these publications, are used at high concentrations and long fixing times so as to ensure adequate fixing.
  • This invention provides a method of desilvering a developed color negative silver halide element, said method comprising bleaching the photographic element with a peracid bleach and subsequently contacting the photographic element with a fixer solution comprising thiosulfate anion and sodium cation;
  • This invention provides a method of desilvering which is fast and environmentally sound. It is based on the discovery that a fixer using sodium thiosulfate actually fixes more efficiently when the bleach which is utilized is an environmentally desirable peracid bleach rather than an iron chelate bleach. Surprisingly, this efficiency increases disproportionately as the silver content of the photographic element is decreased. This unexpected increase in efficiency allows for lower concentrations of sodium thiosulfate in the fixer or shorter fixing times than expected by those skilled in the art. This will make it more desirable for the processing industry to use sodium thiosulfate fixers, which will reduce the amount of ammonium in the processing effluent. Thus, both steps of the desilvering process will be more environmentally benign.
  • the photographic elements of this invention must have a silver content less than 7.0 g/m 2 , and more preferably less than 6.0 g/m 2 . Most preferable are those photographic elements having a silver content of less than 5.5 g/m 2 .
  • the silver content is the sum of the silver employed as silver halide in both sensitized silver halide emulsions and in unsensitized silver halide emulsions as well as the metallic silver deposits incorporated as light filter materials. It will be obvious to those skilled in the art that the amount of silver halide which is utilized in the element must be adequate to form a commercially acceptable image.
  • the silver halide content may be contained in several different emulsions within the photographic element as long as the total amount of silver meets the above parameter. The amount of silver halide in the various emulsions within the single photographic element may differ.
  • the emulsions comprising the photographic element may be comprised of any mixture of silver halides including silver chloride, bromide, chlorobromide, bromoiodide, chloroiodide, and iodide as long as they meet the above silver content parameter.
  • Especially preferred silver halides, for all the emulsions in the element, are silver bromoiodides and iodides.
  • the emulsions of this invention may contain silver halide grains of any type of morphology, such as tabular, cubic, octahedral, and conventional.
  • at least one emulsion contains tabular grains.
  • the tabular grain silver halide emulsions that are useful in the present invention can include (i) high aspect ratio tabular grain emulsions, and (ii) thin intermediate aspect ratio tabular grain silver halide emulsions.
  • High aspect ratio tabular grain emulsions are those which exhibit an average aspect ratio of greater than 8:1.
  • Thin, intermediate aspect ratio emulsions are those in which the tabular grains have an average thickness of less than 0.2 /1 .m and an average aspect ratio ranging from 5:1 to 8:1.
  • Such emulsions are disclosed by Wilgus et al., U. S. Patent 4,434,226; Daubendiek et al., U. S. Patent 4,414,310; Wey, U. S.
  • Patent 4,399,215 Solberg et al., U. S. Patent 4,433,048; Mignot, U. S. Patent 4,386,156; Evans et al., U. S. Patent 4,504,570; Maskasky, U. S. Patent 4,400,463; Wey et al., U. S. Patent 4,414,306, Maskasky, U. S. Patents 4,435,501 and 4,643,966 and Daubendiek et al., U. S. Patents 4,672,027 and 4,693,964.
  • silver bromoiodide grains with a higher molar proportion of iodide in the core than in the periphery of the grain such as those described in GB 1,027,146; JA 54/48,521; U. S. 4,379,837; U. S. 4,444,877; U. S. 4,665,614; U. S. 4,636,461; EP 264,954; and EP-A-0 408 214 and EP-A-0 408 213.
  • the silver halide emulsions can be either monodisperse or polydisperse as precipitated.
  • the grain size distribution of the emulsions can be controlled by techniques of separation and blending of silver halide grains of different types and sizes, including tabular grains, as previously described in the art, for example, in U. S. Patent No. 4,865,964, issued September 12, 1989, entitled "Blended Emulsions Exhibiting Improved Speed-Granularity Relationships".
  • the high aspect ratio tabular grain emulsions and the thin intermediate aspect ratio tabular grain emulsions, as well as other emulsions useful in this invention, can be characterized by a relationship called “tabularity”, (T), which is related to aspect ratio (AR).
  • T tabularity
  • AR aspect ratio
  • This relationship can be defined by the following equations: where “ecd” is the average equivalent circular diameter of the tabular grains, and “t” is the average thickness of the tabular grains, where dimensions are measured in micrometers.
  • Tabular grains are those having two substantially parallel crystal faces, each of which is substantially larger than any other single crystal face of the grain.
  • substantially parallel as used herein is intended to include surfaces that appear parallel on direct or indirect visual inspection at 10,000 X magnification.
  • the grain characteristics described above of the silver halide emulsions of this invention can be readily ascertained by procedures well known to those skilled in the art.
  • the equivalent circular diameter of the grain is defined as the diameter of a circle having an area equal to the projected area of the grain as viewed in a photomicrograph, or an electron micrograph, of an emulsion sample. From shadowed electron micrographs of emulsion samples, it is possible to determine the thickness and the diameter of each grain as well as the tabular nature of the grain. From these measurements, the average thickness, the average ecd, and the tabularity can be calculated.
  • the projected areas of the tabular silver halide grains meeting the tabularity criteria can be summed.
  • the projected areas of the remaining silver halide grains in the photomicrograph can be separately summed. From the two sums, the percentage of the total projected area of the silver halide grains provided by the tabular grains meeting the tabularity criteria can be calculated.
  • Preferred photographic elements include those comprising at least one silver halide emulsion in which greater than 50% of the projected surface area is provided by tabular grains.
  • tabular grain emulsion has a tabularity of from 50 to 25,000;
  • the fixer solution of this invention contains thiosulfate anion and sodium cation.
  • the thiosulfate is present at a concentration from about 0.05 M to about 3.0 M, with 0.3 M to 1.0 M being preferred.
  • the thiosulfate may be supplied by ammonium thiosulfate, sodium thiosulfate, potassium thiosulfate, lithium thiosulfate, magnesium thiosulfate, or calcium thiosulfate, or mixtures of these thiosulfates. Counterions to the thiosulfate may come from the thiosulfate or from other fixer ingredients.
  • a portion of the counterions must be sodium.
  • at least 25 % of the counterions are sodium, with at least 50 % being more preferred.
  • Most preferably, all of the counterions are sodium, and the fixing agent is sodium thiosulfate.
  • the concentration of ammonium in the fixer solution of this invention is less than 1.4 M, and more preferably, less than 0.9 M. If ammonium ion is present, most preferably, the concentration is less than 0.75 M.
  • the ammonium may come from the ammonium thiosulfate or from other fixer ingredients.
  • substantially no ammonium signifies the absence of ammonium intentionally added to the fixer formulation or intentionally added to a solution used to replenish the fixer during processing.
  • Ammonium ion or ammonium species (collectively called "ammonium") which unintentionally occur as impurities, or which are carried into the fixer solution by color photographic recording material, may be present in the fixer.
  • the time of contact of the photographic element with the fixer solution is preferably 15 seconds to 600 seconds. Most preferably, the time of contact is 30 seconds to 240 seconds.
  • the concentration of thiosulfate in the fixer solution can be from about 0.1 molar to as high as solubility in the processing solution allows, but it is preferred that this concentration be as described above.
  • the pH of the fixer solution may range from about 3 to as high as about 12, but it is generally preferred that the pH be between 4 and 10.
  • the fixer solution can optionally contain a source of sulfite or bisulfite ion. If the fixer solution is to be used at a pH below about 7, it is preferred to include a source of sulfite or bisulfite ion in the fixer solution.
  • sodium or potassium sulfite, sodium or potassium bisulfite, or sodium or potassium metabisulfite can be used.
  • concentration of this source of sulfite or bisulfite ion is generally from about 0.01 molar to about 0.5 molar.
  • various buffering agents may be used in the fixer solution, including the above-mentioned sulfite or bisulfite sources, acetate salts, citrates, tartrates, borates, carbonates, phosphates, etc.
  • the fixer solution can contain one or more other compounds known to be fixing agents.
  • Such compounds include thiocyanate salts, thiourea and thiourea derivatives, organic thioethers and thioacids, thione compounds, thiosemicarbazones, organic thiols, amines, and imides. Patent and technical literature references to these and other compounds may be found in Chapter 59 of Comprehensive Coordination Chemistry, Vol. 6, G. Wilkinson, ed., Pergamon, Oxford, 1987.
  • the fixer solution may contain one or more ingredients to effect film hardening and to stabilize the hardening agent in the fixer solution.
  • ingredients include potassium alum, aluminum sulfate, aluminum chloride, boric acid, sodium tetraborate, gluconic acid, tartaric acid, citric acid, acetic acid and sodium acetate, for example.
  • the fixer solution may contain one or more substances which are known to accelerate film fixing. These materials are described in Chapter 15 of The Theory of the Photographic Process, 4th Edition, T. H. James, ed., Macmillan, New York, 1977. Such substances include ammonium salts, such as ammonium chloride (within the content limitations mentioned above), ethylenediamine, and other amines, such as guanidine, which are capable of providing organic ammonium cations that accelerate the fixing process. Other accelerators are thiourea and its derivatives.
  • the fixer solution may also contain compounds for the prevention of precipitation of metal salts of metals that are initially present in or that become introduced into the fixer solution during use.
  • metals include iron, copper, zinc, magnesium, calcium, aluminum, and chromium, among others.
  • Metal sequestering agents, chelating agents, and precipitation control agents may be used to control these metals.
  • metal control agents examples include polycarboxylic acids such as citric acid and tartaric acid; aminocarboxylic acids such as nitrilotriaacetic acid, ethylenedinitrilotetraacetic acid (EDTA), and diethylenetriaminepentaacetic acid; organophosphonic acids such as nitrilotris(methylenephosphonic) acid and 1-hydroxyethylidene-1,1-diphosphonic acid; orthodihydroxybenzene compounds such as 4,5-dihydroxy- m-benzenedisulfonic acid; acyclic or cyclic polyphosphates; and various polymers such as polyacrylic acids.
  • polycarboxylic acids such as citric acid and tartaric acid
  • aminocarboxylic acids such as nitrilotriaacetic acid, ethylenedinitrilotetraacetic acid (EDTA), and diethylenetriaminepentaacetic acid
  • organophosphonic acids such as nitrilotris(methylenephosphonic) acid and 1-hydroxye
  • the concentrations of the fixer solution constituents during processing can be regulated by the usual controlling factors, namely, fixer replenishment rates and replenishing component concentrations, water losses due to evaporation, evaporative losses of volatile components other than water, the amounts and compositions of processing liquids carried into and out of the fixer solution by the photographic recording material, the amount of solution overflow from other vessels containing processing solutions that is introduced into the fixer solution, the amount of solid component carried into the fixer solution by the photographic recording material and then dissolved in the fixer solution, the rate of removal or replacement of any constituent by means such as ion exchange, electrolysis, electrodialysis, and the like.
  • Typical peracid bleaches useful in this invention include the hydrogen, alkali and alkali earth salts of persulfate, peroxide, perborate, perphosphate, and percarbonate, oxygen, and the related perhalogen bleaches such as hydrogen, alkali and alkali earth salts of chlorate, bromate, iodate, perchlorate, perbromate and metaperiodate.
  • perhalogen bleaches such as hydrogen, alkali and alkali earth salts of chlorate, bromate, iodate, perchlorate, perbromate and metaperiodate.
  • the bleaching agent can be present in any effective concentration. Preferred concentrations are from 0.01 to 1.0 moles/liter, more preferably, from 0.05 to 0.5 moles/liter of bleaching agent.
  • the bleaching solution may contain a buffer consisting of an organic acid or inorganic acid and/or a salt thereof.
  • Useful examples include phosphoric acid and salts of phosphate, citric acid and salts of citrate, boric acid and salts of borate or metaborate, acetic acid and salts of acetate, and carbonate.
  • the bleaching solution may also contain a chloride salt such as sodium chloride, potassium chloride, or ammonium chloride, or a bromide salt such as sodium bromide, potassium bromide, or ammonium bromide.
  • accelerators include dimethylaminoethanethiol, dimethylaminoethanethiol isothiouronium salt, aminoethanethiol, and morpholinoethanethiol.
  • the accelerator When used in a pre-solution or in the bleaching solution itself, the accelerator may be used at a concentration of 0.002 to 0.2 moles/liter, with 0.005 to 0.05 preferred.
  • preferred accelerators are silver morpholinoethanethiol, silver aminoethanethiol, and silver dimethylaminoethanethiol, at a concentration of 0.05 to 0. 5 g /m 2 .
  • Scavengers for halogen may be added to the persulfate solution as disclosed in Research Disclosure No. 17556 (1978) and U. S. Patents 4,292,401 and 4,293,639.
  • Other useful discussions of the application of persulfate to photographic bleaching appear in the Journal of the Society of Motion Picture and Television Engineers (SMPTE), Vol. 91, pp. 158-163 (1982); SMPTE, Vol. 91, pp. 1058-1065; and Eastman Kodak Publication H-24, Manual for Processing Eastman Color Films (December, 1988).
  • the photographic elements of this invention can be single color elements or multicolor elements.
  • Multicolor elements typically contain dye image-forming units sensitive to each of the three primary regions of the visible spectrum.
  • Each unit can be comprised of a single emulsion layer or of multiple emulsion layers sensitive to a given region of the spectrum.
  • the layers of the element, including the layers of the image-forming units, can be arranged in various orders as known in the art.
  • the emulsions sensitive to each of the three primary regions of the spectrum can be disposed as a single segmented layer, e.g., as by the use of microvessels as described in Whitmore, U. S. Patent 4,362,806 issued December 7, 1982.
  • the element can contain additional layers such as filter layers, interlayers, overcoat layers, subbing layers and the like.
  • the total thickness of these light sensitive and additional layers will generally be between about 5 and 30 microns. Thinner formulations of about 5 to 25 microns are generally preferred since these are known to provide improved contact with the process solution. For the same reason, more swellable film structures are preferred.
  • the element may be particularly useful with a magnetic recording layer such as those described in Research Disclosure No. 34390, p. 869 (November, 1992), due to the decreased Dmin associated with peracid bleaches.
  • the silver halide emulsions employed in the elements of this invention are negative-working emulsions.
  • suitable emulsions and their preparation are described in Research Disclosure Sections I and II and the publications cited therein.
  • Some of the suitable vehicles for the emulsion layers and other layers of elements of this invention are described in Research Disclosure Section IX and the publications cited therein.
  • the silver halide emulsions can be chemically and spectrally sensitized in a variety of ways, examples of which are described in Sections III and IV of the Research Disclosure.
  • the elements of the invention can include various couplers including, but not limited to, those described in Research Disclosure Section VII, paragraphs D, E, F, and G and the publications cited therein. These couplers can be incorporated in the elements and emulsions as described in Research Disclosure Section VII, paragraph C, and the publications cited therein.
  • the photographic elements of this invention or individual layers thereof can contain among other things brighteners (Examples in Research Disclosure Section V), antifoggants and stabilizers (Examples in Research Disclosure Section VI), antistain agents and image dye stabilizers (Examples in Research Disclosure Section VII, paragraphs I and J), light absorbing and scattering materials (Examples in Research Disclosure Section VIII), hardeners (Examples in Research Disclosure Section X), plasticizers and lubricants (Examples in Research Disclosure Section XII), antistatic agents (Examples in Research Disclosure Section XIII), matting agents (Examples in Research Disclosure Section XVI), and development modifiers (Examples in Research Disclosure Section XXII).
  • the photographic elements can be coated on a variety of supports including, but not limited to, those described in Research Disclosure Section XVII and the references described therein.
  • Photographic elements can be exposed to actinic radiation, typically in the visible region of the spectrum, to form a latent image as described in Research Disclosure Section XVIII and then processed to form a visible dye image, examples of which are described in Research Disclosure Section XIX.
  • Processing to form a visible dye image includes the step of contacting the element with a color developing agent to reduce developable silver halide and oxidize the color developing agent. Oxidized color developing agent in turn reacts with the coupler to yield a dye.
  • a stabilization step follows a fixing step.
  • One or more intervening processing steps may come before the development, bleaching, fixing, and/or the stabilization steps.
  • some processing steps, such as washing steps may be deleted from the processing cycle. Examples of such modifications to the processing cycle contemplated by the invention include: a pre-solution and/or washing cycle before development; a stop solution, bleach accelerator solution, and/or washing treatment after the development step and before the bleaching step; and omission of the washing steps before and/or after the fixing step.
  • the benefits of this invention can also be realized by placing an additional fixing step between the development step and the bleach step. Conventional techniques for processing are illustrated by Research Disclosure, paragraph XIX.
  • Preferred processing sequences for color photographic elements, particularly color negative films and color print papers, which can be used with this invention include the following:
  • the bleaching step is, in each instance, performed using a peracid-bleaching agent.
  • the Photographic Samples were prepared using known materials and methods.
  • Photographic Samples 101 to 104 and 112 to 114 were prepared by applying the following layers to a clear support: two red light-sensitive layers in a red sensitive element, two green light-sensitive layers in a green sensitive element, two blue sensitive layers in a blue light-sensitive element along with subbing layers, antihalation and UV-absorbing layers, interlayers, and protective layers as known in the art.
  • Photographic Sample 105 was prepared by applying the following layers to a clear support: two red light-sensitive layers in a red sensitive element, three green light-sensitive layers in a green sensitive element, two blue sensitive layers in a blue light-sensitive element along with subbing layers, antihalation and UV-absorbing layers, interlayers, and protective layers as known in the art.
  • Photographic Samples 106 to 109 and 111 were prepared by applying the following layers to a clear support: three red light-sensitive layers in a red sensitive element, three green light-sensitive layers in a green sensitive element, two blue sensitive layers in a blue light-sensitive element along with subbing layers, antihalation and UV-absorbing layers, interlayers, and protective layers as known in the art.
  • Photographic Sample 110 was prepared by applying the following layers to a clear support: three red light-sensitive layers in a red sensitive element, three green light-sensitive layers in a green sensitive element, three blue sensitive layers in a blue light-sensitive element along with subbing layers, antihalation and UV-absorbing layers, interlayers, and protective layers as known in the art.
  • Photographic samples 101 through 114 employed the following image dye-forming couplers, image modifiers, masking couplers, dyes and so forth:
  • the quantity of silver retained in the various photographic samples at a Dmax exposure was monitored after processing using X-ray fluorescence techniques. These quantities are reported in Table II below. Also reported in Table II are the contact times (expressed in seconds) of the various photographic samples tested with the fixer solutions.
  • the fixer solution employed in all of these experiments has a concentration of 0.825 mole of thiosulfate per liter (e.g., 0.825 M).
  • Photographic sample 105 comprises approximately 7.4 g/m 2 of silver while photographic samples 106 through 109 typically comprise one-half that amount of silver. These lower silver samples fix much more rapidly than the higher silver film. As shown in Table II, sample 105 in process B retains about 1.5 g silver after 30 seconds fixing while samples 106, 107, 108, and 109, which start off at about one-half the initial silver, only retain about 0.5 g or one-third the amount after 30 seconds of fixing.
  • Table III further illustrates the fixing advantages of this invention.
  • Samples 110 through 114 were processed using simulated seasoned processing solutions and similar results were obtained, e.g., the combination of a peracid bleach followed by a high sodium thiosulfate fix resulted in rapid fixing of the photographic samples.

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  • General Physics & Mathematics (AREA)
  • Silver Salt Photography Or Processing Solution Therefor (AREA)
EP93203591A 1992-12-29 1993-12-20 Verfahren zum Bleichen und Fixieren von farbphotographischem Material mit niedrigem Silbergehalt Withdrawn EP0605038A1 (de)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62183461A (ja) * 1986-02-07 1987-08-11 Fuji Photo Film Co Ltd ハロゲン化銀カラ−写真感光材料の処理方法
JPS62183460A (ja) * 1986-02-07 1987-08-11 Fuji Photo Film Co Ltd ハロゲン化銀カラ−写真感光材料の処理方法
US4857441A (en) * 1986-02-07 1989-08-15 Fuji Photo Film Co., Ltd. Method for processing silver halide-containing photosensitive material for color photography
JPH01292339A (ja) * 1988-05-19 1989-11-24 Fuji Photo Film Co Ltd ハロゲン化銀カラー写真感光材料の処理方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62183461A (ja) * 1986-02-07 1987-08-11 Fuji Photo Film Co Ltd ハロゲン化銀カラ−写真感光材料の処理方法
JPS62183460A (ja) * 1986-02-07 1987-08-11 Fuji Photo Film Co Ltd ハロゲン化銀カラ−写真感光材料の処理方法
US4857441A (en) * 1986-02-07 1989-08-15 Fuji Photo Film Co., Ltd. Method for processing silver halide-containing photosensitive material for color photography
JPH01292339A (ja) * 1988-05-19 1989-11-24 Fuji Photo Film Co Ltd ハロゲン化銀カラー写真感光材料の処理方法

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