Classifications

• • 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
  • G03C1/00—Photosensitive materials
  • G03C1/76—Photosensitive materials characterised by the base or auxiliary layers
  • G03C1/825—Photosensitive materials characterised by the base or auxiliary layers characterised by antireflection means or visible-light filtering means, e.g. antihalation
• • 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
  • G03C1/00—Photosensitive materials
  • G03C1/005—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein
  • G03C1/035—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein characterised by the crystal form or composition, e.g. mixed grain
• • 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
  • G03C1/00—Photosensitive materials
  • G03C1/76—Photosensitive materials characterised by the base or auxiliary layers
  • G03C1/7614—Cover layers; Backing layers; Base or auxiliary layers characterised by means for lubricating, for rendering anti-abrasive or for preventing adhesion

Definitions

• the present invention relates to a silver halide photographic material favorably processable in a so-called "dot-to-dot work" step in a photomechanical process and, more precisely, to a silver halide photographic material having improved photographic properties for daylight dot-to-dot work processing.
• Silver halide photographic materials for illuminated rooms as referred to herein mean photographic materials to which a light having a wavelength of 400 nm or more and containing no ultraviolet light components is applicable as a safelight.
• JP-A-63-183438 the term "JP-A” as used herein means an "unexamined published Japanese patent application”
• JP-A-63-296034 JP-A-63-306436
• JP-A-1-108123 U.S. Patent 4,659,647.
• Photographic emulsions of fine grains are advantageous in increasing their Dmax and also in saving silver in them, but the problem that their tone reproducibility was noticeably worsened when they are subjected to so-called dry-dot work (by over-exposure so as to thicken dots to a desired dot %) which is intrinsic in the dot-to-dot working field has been generated. This is because the transmitted light causes halation in the emulsions.
• a method of increasing the amount of backing dyes to be incorporated into the photographic materials In order to solve the problem.
• a conventional method of localizing an acidic dye having therein a sulfo group or a carboxyl group in a specific layer with a mordant agent there is known a conventional method of localizing an acidic dye having therein a sulfo group or a carboxyl group in a specific layer with a mordant agent.
• a mordant agent for this purpose, there are known polymers of ethylenic unsaturated compounds having a dialkylaminoalkyl ester residue, such as those described in British Patent 685,475; products formed by reacting a polyvinyl alkyl ketone and an aminoguanidine, such as those described in British Patent 850,281; vinyl-pyridine polymers and vinyl-pyridinium cationic polymers, such as those described in U.S.
• Patents 2,548,564, 2,484,430, 3,148,061 and 3,756,814. These are cationic polymer mordants containing secondary or tertiary amino groups, nitrogen-containing heterocyclic groups or their quaternary cationic groups in their polymer structures so as to effectively mordant the above-mentioned acidic dyes.
• the mordanted acidic dyes often diffuse to other layers.
• the photographic materials for photoengraving to produce printing plates are subjected to reduction with a reducer so as to adjust their densities and gradations, and the reducer to be used contains a water-soluble iron complex as a reducing agent. If the above-mentioned cationic mordant agent is applied to such photographic materials for photoengraving, it will bond to the iron complex by electrostatic bonding to disadvantageously give yellow stains in the processed photographic materials.
• the object of the present invention is to provide a silver halide photographic material for illuminated room, which may have a reduced amount of silver, which may well be subjected to dry-dot work to give improved high-quality images and which has few stains even processed by rapid processing.
• a silver halide photographic material comprising a support having thereon at least one silver halide emulsion layer, wherein the emulsion of the silver halide emulsion layer comprises a silver halide having a silver chloride content of 90 mol% or more containing a transition metal of 1 ⁇ 10 ⁇ 6 mol or more per mol of silver; the material has a layer containing a dye subjected to a fine crystalline solid dispersion between the emulsion layer and the support; the material has an interlayer comprising a hydrophilic colloid and an uppermost layer comprising a hydrophilic colloid and solid grains having a mean grain size of from 1 to 5 ⁇ m above the emulsion layer; and the thickness of the interlayer is at least 0.8 times the thickness of the uppermost layer.
• the silver halide in the emulsion layer has a mean grain size of 0.2 ⁇ m or less and the amount of silver in the emulsion layer is 3.5 g/m2 or less.
• the compounds of formulae (I) to (VII) each has at least one dissociating group having a pKa value of from 4 to 11 in a mixed solution of water and ethanol at a ratio of 1:1 by volume, in one molecule.
• dyes to be used in the present invention in the form of their solid dispersions are those described in International Patent WO88/04794; European Patents EP-0274723A1, 0276566, 0299435; JP-A-52-92716, JP-A-55-155350, JP-A-55-155351, JP-A-61-205934, JP-A-48-68623; U.S. Patents 2,527,583, 3,486,897, 3,746,539, 3,933,798, 4,130,429, 4,040,841; JP-A-3-7931, JP-A-3-282244, JP-A-3-167546, JP-A-5-113623.
• Dyes which are preferably used in the present invention are those having an absorption maximum of from 300 to 500 nm. Specific examples of the dyes preferably used in the present invention are mentioned below, which, however, are not limited thereto.
• Light that has passed through the light-sensitive emulsion layer during exposure is reflected by the support and the reflected light again passes through the emulsion layer to cause halation which worsens the image to be formed.
• the dye which is subjected to a fine crystalline solid dispersion is added to the non-light-sensitive hydrophilic colloid layer between the emulsion layer and the support.
• the amount of the dye to be coated is preferably from 10 mg to 80 mg, more preferably from 20 mg to 60 mg, per m2 of the photographic material.
• Such dyes employable in the present invention can be easily produced by the methods described in International Patent WO88/04794; European Patents EP-0274723A1, 0276566, 0299435; JP-A-52-92716, JP-A-55-155350, JP-A-55-155351, JP-A-61-205934, JP-A-48-68623; U.S. Patents 2,527,583, 3,486,897, 3,746,539, 3,933,798, 4,130,429, 4,040,841; JP-A-3-7931, JP-A-3-282244, JP-A-3-167546 or according to these methods.
• the silver halide photographic material of the present invention may contain other dyes so as to ensure its safelight safety and external-light safety.
• the dyes to be used for this purpose are not limited and the examples thereof include water-soluble dyes and solid disperse dyes.
• the silver halide grains used in the photographic material of the present invention preferably contain at least one transition metal.
• L are a halogeno ligand (e.g., fluoride, chloride, bromide, iodide), a cyanido ligand, a cyanato ligand, a thiocyanato ligand, a selenocyanato ligand, a tellurocyanato ligand, an acido ligand and an aquo ligand.
• a halogeno ligand e.g., fluoride, chloride, bromide, iodide
• a cyanido ligand e.g., fluoride, chloride, bromide, iodide
• a cyanido ligand e.g., fluoride, chloride, bromide, iodide
• a cyanido ligand e.g., fluoride, chloride, bromide, iodide
• a cyanido ligand e
• M More preferred examples of M are rhodium, ruthenium, rhenium, osmium and iridium.
• transition metal coordination complexes for use in the present invention are mentioned below, which, however, are not limited thereto.
• the content of the transition metal in the silver halide grains of the present invention is 1 ⁇ 10 ⁇ 6 mol or more, preferably from 1 ⁇ 10 ⁇ 6 to 5 ⁇ 10 ⁇ 4 mol, more preferably from 5 ⁇ 10 ⁇ 6 to 2 ⁇ 10 ⁇ 4 mol, per mol of the silver halide.
• One silver halide grain may be added in combination with one or more different transition metals.
• transition metal distribution in the silver halide grains of the present invention is not specifically limited, but preferably, more transition metals are in the outside area of one grain.
• the silver halide emulsion used in the silver halide photographic material of the present invention is preferably an emulsion of a silver chlorobromide or silver chloroiodobromide having a silver chloride content of 90 mol% or more. Increase in the silver bromide or silver iodide content in the silver halide is not preferred, as worsening the safelight safety of the photographic material in daylight rooms or lowering the gamma ( ⁇ ) value of the material.
• the mean grain size of the silver halide in the emulsion layer is 0.2 ⁇ m or less, preferably from 0.08 to 0.19 ⁇ m, and more preferably from 1.3 to 1.8 ⁇ m.
• the amount of silver in the emulsion layer is 3.5 g/m2 or less, preferably from 1.0 to 3.4 g/m2, and more preferably from 1.5 to 3.3 g/m2.
• the photographic material of the present invention preferably contain a matting agent such as silica, magnesium oxide or polymethyl methacrylate in the photographic emulsion layer or other hydrophilic colloid layers so as to increase the adhesiveness of the layers.
• a matting agent such as silica, magnesium oxide or polymethyl methacrylate
• the upper protective layer contains the matting agent.
• the ratio by weight of the matting agent to the hydrophilic colloid in the layer is from 0.02 to 1.
• the matting agent is preferably in the form of grains having a mean grain size of from 1 to 5 ⁇ m, more preferably from 3 to 5 ⁇ m.
• the photographic material of the present invention may contain solid grains, such as those of silica, silver halides, magnesium oxide, calcium carboxylates or polymethyl methacrylates, in the photographic emulsion layer or other hydrophilic colloid layers, for the purpose of easily thickening the dots to be formed by exposure.
• the upper protective layer (uppermost layer) contains such grains.
• the ratio by weight of the light-scattering agent comprising such grains to the hydrophilic colloid in the layer is from 0.02 to 1.
• the grains have a mean grain size of from 0.1 to 5 ⁇ m, more preferably from 3 to 5 ⁇ m.
• the compound of the solid grains may be the same as or different from that of the matting agent.
• the thickness of the upper protective layer in the photographic material of the present invention is generally from 0.2 to 1 ⁇ m, preferably from 0.3 to 0.8 ⁇ m.
• the photographic material of the present invention has an interlayer between the silver halide emulsion layer and the upper protective layer, and the thickness of the interlayer is at least 0.8 times, preferably from 1.0 to 2.0 times, and more preferably from 1.2 to 1.8 times, the thickness of the upper protective layer (uppermost layer) so as to easily thicken the dots to be formed by exposure.
• the developing agent used in the developer which is used in processing the photographic material of the present invention is not specifically limited, but the developer is desired to contain dihydroxybenzenes in order to easily form hard images having a good dot quality.
• the developer is desired to contain dihydroxybenzenes in order to easily form hard images having a good dot quality.
• dihydroxybenzenes a combination of dihydroxybenzenes and 1-phenyl-3-pyrazolidones, or a combination of dihydroxybenzenes and p-aminophenols may also be employed.
• 1-Phenyl-3-pyrazolidone and derivatives thereof may also be used as a developing agent in the present invention.
• Examples thereof include 1-phenyl-3-pyrazolidone, 1-phenyl-4,4-dimethyl-3-pyrazolidone, 1-phenyl-4-methyl-4-hydroxymethyl-3-pyrazolidone, 1-phenyl-4,4-dihydroxymethyl-3-pyrazolidone, 1-phenyl-5-methyl-3-pyrazolidone, 1-p-aminophenyl-4,4-dimethyl-3-pyrazolidone, 1-p-tolyl-4,4-dimethyl-3-pyrazolidone and 1-p-tolyl-4-methyl-4-hydroxymethyl-3-pyrazolidone.
• Examples of p-aminophenol developing agents also usable in the present invention include N-methyl-p-aminophenol, p-aminophenol, N-( ⁇ -hydroxyethyl)-p-aminophenol, N-(4-hydroxyphenyl)glycine, 2-methyl-p-aminophenol and p-benzylaminophenol. More preferred is N-methyl-p-aminophenol.
• the amount of the developing agent used in the developer for use in the present invention is preferably from 0.05 mol/liter to 0.8 mol/liter.
• the content of the former in the developer is from 0.05 mol/liter to 0.5 mol/liter and that of the latter therein is 0.06 mol/liter or less.
• the developer for use in the present invention may contain, as a preservative, a sulfite such as sodium sulfite, potassium sulfite, lithium sulfite, ammonium sulfite, sodium bisulfite, potassium metabisulfite and formaldehyde-sodium bisulfite.
• a sulfite such as sodium sulfite, potassium sulfite, lithium sulfite, ammonium sulfite, sodium bisulfite, potassium metabisulfite and formaldehyde-sodium bisulfite.
• the content of such a sulfite is preferably 0.3 mol/liter or more, more preferably 0.4 mol/liter or more.
• the upper limit of the sulfite content is preferably 2.5 mol/liter or less, more preferably up to 1.2 mol/liter or less.
• the developer may contain an alkali agent for the purpose of properly adjusting the pH value thereof.
• an alkali agent usable is a pH adjusting agent or a pH buffer, such as sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium tertiary phosphate, potassium tertiary phosphate, sodium silicate and potassium silicate.
• the developer may further contain additives other than the above-mentioned components.
• additives include, for example, a development inhibitor such as boric acid, borax, sodium bromide, potassium bromide and potassium iodide; an organic solvent such as ethylene glycol, diethylene glycol, triethylene glycol, dimethylformamide, methyl cellosolve, hexylene glycol, ethanol and methanol; an antifoggant such as mercapto compounds (e.g., 1-phenyl-5-mercaptotetrazole, sodium 2-mercaptobenzimidazole-5-sulfonate), indazole compounds (e.g., 5-nitroindazole) and benzotriazole compounds (e.g., 5-methylbenzotriazole).
• a development inhibitor such as boric acid, borax, sodium bromide, potassium bromide and potassium iodide
• an organic solvent such as ethylene glycol, diethylene glycol, triethylene glycol, dimethylformamide,
• additives such as a color toning agent, a surfactant, a defoaming agent, a water softener and a hardening agent, if desired.
• additives such as a color toning agent, a surfactant, a defoaming agent, a water softener and a hardening agent, if desired.
• amino compounds such as those described in JP-A-56-106244 and imidazole compounds such as those described in JP-B-48-35493 (the term "JP-B” as used herein means an "examined Japanese patent publication" are preferred, as effective in promoting the developability of the developer and elevating the sensitivity of the photographic material being processed with the developer.
• the developer for use in the present invention may contain the compounds described in JP-A-56-24347 as a silver stain inhibitor; the compounds described in JP-A-62-212651 as an uneven development inhibitor; and the compounds described in JP-A-61-267759 as a dissolution aid.
• the developer may also contain, as a buffer, a boric acid described in JP-A-62-186259, saccharides (e.g., saccharose) described in JP-A-60-93433, oximes (e.g., acetoxime), phenols (e.g., 5-sulfosalicylic acid) and tertiary phosphates (e.g., sodium salts, potassium salts).
• a boric acid described in JP-A-62-186259
• saccharides e.g., saccharose
• oximes e.g., acetoxime
• phenols e.g., 5-sulfosalicylic acid
• tertiary phosphates e.g., sodium salts, potassium salts.
• Preferred is a boric acid.
• the fixer used in the present invention is an aqueous solution containing a fixing agent.
• a fixing agent e.g., water-soluble aluminium compounds
• an acetic acid and a dibasic acid e.g., tartaric acid, citric acid, their salts.
• it has a pH value of 3.8 or more, more preferably from 4.0 to 5.5.
• the fixing agent usable are sodium thiosulfate, ammonium thiosulfate, etc. Especially preferred is ammonium thiosulfate, in view of its fixing rate.
• the amount of the fixing agent in the fixer may be varied suitably but is, in general, approximately from 0.1 mol/liter to 5 mol/liter.
• Water-soluble aluminium salts which acts in the fixer as a hardening agent are compounds that are generally known as hardening agents in acidic film-hardening fixers. Examples thereof include aluminium chloride, aluminium sulfate and potassium alum.
• dibasic acid usable are tartaric acid, derivatives thereof, citric acid and derivatives thereof.
• the dibasic acid may be used singly or in combination.
• the compound is effectively in the fixer in an amount of 0.005 mol or more per liter of the fixer, more preferably from 0.01 mol/liter to 0.03 mol/liter.
• dibasic acid examples include tartaric acid, potassium tartarate, sodium tartarate, potassium sodium tartarate, ammonium tartarate and ammonium potassium tartarate.
• citric acid As examples of usable citric acid and its derivatives, mentioned are citric acid, sodium citrate, potassium citrate, etc.
• the fixer may further contain, if desired, a preservative (e.g., sulfites, bisulfites), a pH buffer (e.g., acetic acid, boric acid), a pH adjusting agent (e.g., ammonia, sulfuric acid), an image stability-improving agent (e.g., potassium iodide), and a chelating agent.
• a preservative e.g., sulfites, bisulfites
• a pH buffer e.g., acetic acid, boric acid
• a pH adjusting agent e.g., ammonia, sulfuric acid
• an image stability-improving agent e.g., potassium iodide
• the fixing temperature and the fixing time may follow the developing temperature and the developing time.
• the fixing temperature may be from about 20°C to about 50°C and the fixing time may be from 10 seconds to one minute.
• Rinsing water to be used for rinsing the processed photographic material of the present invention may contain an anti-fungal agent (e.g., compounds described in Horiguchi, Anti-bacterial and Anti-fungal Chemistry , and JP-A-62-115154), a rinsing accelerating agent (e.g., sulfites), and a chelating agent.
• an anti-fungal agent e.g., compounds described in Horiguchi, Anti-bacterial and Anti-fungal Chemistry , and JP-A-62-115154
• a rinsing accelerating agent e.g., sulfites
• the photographic material is, after developed and fixed, is rinsed and dried.
• the rinsing is to remove almost completely the silver salts dissolved by fixation and is effected preferably at about 20°C to about 50°C for 10 seconds to 3 minutes.
• the drying is effected at about 40°C to about 100°C.
• the drying time may be varied appropriately, depending on the ambient conditions, but, in general, may be from about 5 seconds to about 3 minutes and 30 seconds.
• the photographic material of the present invention may be processed, using a roller-conveying type automatic developing machine which is described in, for example, U.S. Patents 3,025,779 and 3,545,971.
• the machine is referred to simply as a roller-conveying type processor.
• the process by the roller-conveying type processor is composed of four steps of development, fixation, rinsing and drying. Most preferably, the process for processing the photographic material of the present invention follows the four steps, though not excluding other steps (e.g., stopping step).
• a countercurrent rinsing system having two or three rinsing stages so as to save water to be used therein.
• the photographic material of the present invention is suitably processed in an automatic developing machine for 30 to 60 seconds for dry-to-dry processing (the time means a total time needed from the start of the processing at which the top of the photographic material to be processed is introduced into the developing zone to the end of the same at which the end of the processed material is taken out from the drying zone).
• the developer for use in the present invention is preferably wrapped with a wrapping material having a low oxygen permeability such as described in JP-A-61-73147.
• the replenishing system described in JP-A-62-91939 is preferably employed for replenishing the developer in the process of the present invention.
• the silver halide photographic material gives a high Dmax, it may still maintain its high density even though the dot area formed is reduced when the material is subjected to reduction after processed to form an image.
• the reducer usable in the present invention is not specifically limited. For instance, usable are those described in Mees, The Theory of the Photographic Process , pp. 738 to 744 (1954, published by Macmillan), Tetsuo Yano, Theory and Practice of Photographic Processing , pp. 166 to 169 (1978, published by Kyoritsu Publishing, Japan), and in JP-A-50-27543, JP-A-52-68429, JP-A-55-17123, JP-A-55-79444, JP-A-57-10140, JP-A-57-142639 and JP-A-61-61155.
• reducers containing one or more oxidizing agents selected from permanganates, persulfates, ferric salts, cupric salts, ceric salts, red prussiate of potash and bichromates, and optionally containing inorganic acids such as sulfuric acid and alcohols; as well as reducers containing oxidizing agents, such as red prussiate of potash and ferric ethylenediamine-tetraacetates, and silver halide solvents, such as thiosulfates, rhodanides, thioureas and their derivatives, and optionally containing inorganic acids such as sulfuric acid.
• oxidizing agents selected from permanganates, persulfates, ferric salts, cupric salts, ceric salts, red prussiate of potash and bichromates, and optionally containing inorganic acids such as sulfuric acid and alcohols
• reducers containing oxidizing agents such as red prussiate of potash and ferr
• Typical examples of the reducer usable in the present invention include so-called Farmer's reducer, ferric ethylenediamine-tetraacetates, potassium permanganate, ammonium persulfate reducer (Kodak R-5) and ceric salt reducers.
• the reduction of the photographic material of the present invention is effected at from 10°C to 40°C, preferably at from 15°C to 30°C, to be completed within several seconds to several ten minutes, preferably within several minutes.
• the photographic material for photomechanical process of the present invention one may have a lot of latitude in the reduction of the material under this condition.
• the reducer is made to act on the silver image formed in the emulsion layer, via the non-light-sensitive upper layer containing the compound of the present invention.
• various methods may be employable for the reduction.
• the photographic material for photomechanical process of the present invention is dipped in a reducer while stirring, or a reducer may be applied to the surface of the photographic material with a brush or roller.
• an aqueous solution of silver nitrate and an aqueous solution of sodium chloride containing 1.2 ⁇ 10 ⁇ 4 mol, per mol of silver, of (NH4)2Rh(H2O)Cl5 were simultaneously added thereto over a period of 14 minutes, while the potential of the reaction system was controlled at 95 mV, to prepare cubic silver chloride grains having a mean grain size of 0.15 ⁇ m.
• a lower protective layer containing 5 mg/m2 of 5-nitroindazole, 8 mg/m2 of lipoic acid, 6 mg/m2 of C2H5SO2SNa, 50 mg/m2 of hydroquinone, 15 mg/m2 of 1-hydroxy-2-benzaldoxime and 230 mg/m2 of polyethyl acrylate latex (mean grain size: 0.05 ⁇ m), its thickness being determined by adjusting the amount of gelatin therein as shown in Table 1 below; and an upper protective layer (uppermost layer) containing 55 mg/m2 of a matting agent (silicon dioxide; mean grain size: 3.5 ⁇ m), 135 mg/m2 of methanol silica (mean grain size: 0.02 ⁇ m), 25 mg/m2 of sodium dodecylbenzenesulfonate as a coating aid, 20 mg/m2 of sodium salt of sulfate ester of polyoxyethylene nonylpheny
• the support used herein had the following backing layer and back-protecting layer.
• the swelling degree of the back surface of the support was 110 %.
• Backing Layer Gelatin 170 mg/m2 Sodium Dodecylbenzenesulfonate 32 mg/m2 Sodium Dihexyl- ⁇ -sulfosuccinate 35 mg/m2 SnO2/Sb (9/1, by weight; mean grain size: 0.25 ⁇ m) 318 mg/m2
• the developer used for processing the exposed samples had the following composition:
• Sample Nos. 6 and 7 of the present invention were good in that the exposure time for dry-dot work was short and the quality of the images formed was good.

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• Chemical & Material Sciences (AREA)
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• Materials Engineering (AREA)
• Physics & Mathematics (AREA)
• General Physics & Mathematics (AREA)
• Crystallography & Structural Chemistry (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Silver Salt Photography Or Processing Solution Therefor (AREA)

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Citations (4)

• 1993
  • 1993-09-30 JP JP24471693A patent/JPH07104428A/ja active Pending
• 1994
  • 1994-09-29 EP EP19940115396 patent/EP0646836B1/fr not_active Expired - Lifetime
  • 1994-09-29 DE DE1994622363 patent/DE69422363T2/de not_active Expired - Lifetime

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