DE1157077B - Process for the preparation of photographic silver halide emulsions stabilized with palladium salts - Google Patents
Process for the preparation of photographic silver halide emulsions stabilized with palladium saltsInfo
- Publication number
- DE1157077B DE1157077B DEP31717A DEP0031717A DE1157077B DE 1157077 B DE1157077 B DE 1157077B DE P31717 A DEP31717 A DE P31717A DE P0031717 A DEP0031717 A DE P0031717A DE 1157077 B DE1157077 B DE 1157077B
- Authority
- DE
- Germany
- Prior art keywords
- palladium
- preparation
- silver halide
- photographic silver
- halide emulsions
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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
- G03C1/005—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein
- G03C1/06—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein with non-macromolecular additives
- G03C1/08—Sensitivity-increasing substances
- G03C1/09—Noble metals or mercury; Salts or compounds thereof; Sulfur, selenium or tellurium, or compounds thereof, e.g. for chemical sensitising
-
- 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
- G03C1/06—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein with non-macromolecular additives
- G03C1/08—Sensitivity-increasing substances
-
- 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
- G03C1/06—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein with non-macromolecular additives
- G03C1/34—Fog-inhibitors; Stabilisers; Agents inhibiting latent image regression
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- General Physics & Mathematics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Verfahren zur Herstellung von mit Palladiumsalzen stabilisierten photographischen Halogensilberemulsionen Die Erfindung bezieht sich auf die Herstellung von mit Palladiumsalzen stabilisierten photographischen Halogensilberemulsionen, die Gelatine als Schutzkolloid enthalten.Process for the preparation of photographic stabilized with palladium salts Halide Silver Emulsions The invention relates to the preparation of palladium salts stabilized photographic silver halide emulsions that use gelatin as a protective colloid contain.
Photographische Emulsionen mit einem Zusatz von Palladium-Verbindungen sind bereits bekannt, z. B. in der deutschen Patentschrift 964 561. Ihr Verwendungszweck ist abgestellt auf Empfindlichkeitssteigerung, Übersensibilisierung und Verminderung des Schleiers, insbesondere bei der Lagerung photographisehen Materials bei erhöhten Temperatur- und Feuchtigkeitsbedingungen. Bei der Herstellung derartiger Halogensilberemulsionen beobachtet man häufig Desensibilisierungserscheinungen und auch eine unregelmäßige Wirkungsweise, besonders im Hinblick auf die zu stabilisierende Emulsion.Photographic emulsions with an addition of palladium compounds are already known, e.g. B. in German Patent 964 561. Their intended use is geared to increasing sensitivity, oversensitization and reducing fog, especially when storing photographic material at elevated temperature and humidity conditions. In the production of such halogenated silver emulsions, symptoms of desensitization and also an irregular mode of action are often observed, particularly with regard to the emulsion to be stabilized.
Es wurde festgestellt, daß diese unregelmäßige Wirkung auf Palladiumgelatinatbildung zurückzuführen ist, die je nach Bedingungen beim Einrühren teils mehr teils weniger stattfindet. Wird z. B. Pd(NOG), oder (NH4),PdC]4 in Form einer 1 O/Oigen wäßrigen Lösung der gelatinehaltigen Emulsion zugesetzt, so erhält man eine örtliche Fällung von Palladiumgelatinat, wodurch das Palladium photochemisch teilweise unwirksam bleibt.It was found that this irregular effect can be attributed to the formation of palladium gelatinate, which, depending on the conditions, sometimes takes place more, sometimes less, when stirring in. Is z. B. Pd (NOG) or (NH4) PdC] added aqueous 4 in the form of a 1 O / o solution of the gelatin-containing emulsion, there is obtained a local precipitation of Palladiumgelatinat, whereby the palladium remains photochemically partially ineffective.
Damit stellt sich die Aufgabe, Palladium in solcher Form in die gelatinehaltige photographische Emulsion einzubringen, daß die störende Wechselwirkung mit Gelatine ausgeschaltet ist. Erfindungsgemäß wird dies dadurch gelöst, daß man der Emulsion Palladiumaminosäurecheiatverbindungen zufügt.This is the task of converting palladium in such a form into the gelatine-containing Bring photographic emulsion that the interfering interaction with gelatin is turned off. According to the invention, this is achieved by adding the emulsion Adds palladium amino acid chelate compounds.
Bei der Zugabe derartiger Verbindungen sind ],eine Ausfällungserscheinungen zu beobachten. Geeignete Verbindungen sind z. B. die Chelate des Palladiums mit Glykokoll, x-Alanin, fl-Alanin, Serin, Sarkosin, Arginin, Histidin, Hippursäure, Asparaginsäure, Glutaminsäure, Prolin, Tryptophan u. a.When such compounds are added,], a precipitation phenomenon to observe. Suitable compounds are e.g. B. the chelates of palladium with Glycocolla, x-alanine, fl-alanine, serine, sarcosine, arginine, histidine, hippuric acid, Aspartic acid, glutamic acid, proline, tryptophan and others.
Einen ähnlichen Effekt erhält man auch bei Zugabe des Äthylendiaminchelates des Palladiums. Jedoch hat das Äthylendiamin als Chelatbildner gegenüber den an, photeren Aminosäuren den Nachteil, daß der pII-Wert der Emulsion ins alkalische Gebiet verschoben wird. Außerdem zeigen insbesondere höchstempfindliche Emulsionen bei Zugabe des Äthylendiaminchelates eine erhöhte Schleierneigung.A similar effect is obtained when adding the ethylenediamine chelate of palladium. However, the ethylenediamine has as a chelating agent to the photeren amino acids have the disadvantage that the pII value of the emulsion is alkaline Area is moved. In addition, particularly highly sensitive emulsions show when the ethylenediamine chelate is added, there is an increased tendency to fog.
Palladiumchelate lassen sich ohne Schwierigkeit in gelatinehaltige Halogensilberemulsionen einrühren. Im Vergleich zu (NHI)2PdC1, oder Pd(NO1)2 läßt sich mit den beanspruchten Verbindungen eine wesentliche Verbesserung der Schleierwerte bei der Lagerung und der erhöhten Temperatur- und Feuchtigkeitsbedingungen erzielen. Keine Änderung dieser Wirkung tritt auch bei Emulsionen ein, deren Gelatine teilweise durch künstliche Schutzkolloide, wie Cellulosederivate, Polyvinylalkoholderivate usw., ersetzt wird.Palladium chelates can be converted into gelatin-containing ones without difficulty Stir in halogen silver emulsions. Compared to (NHI) 2PdC1, or Pd (NO1) 2 leaves The claimed compounds result in a significant improvement in the haze values in storage and the elevated temperature and humidity conditions. This effect does not change in the case of emulsions, some of which are gelatin by artificial protective colloids, such as cellulose derivatives, polyvinyl alcohol derivatives etc., is replaced.
Die Erfindung ist im nachstehenden Ausführungsbeispiel des näheren beschrieben.The invention is detailed in the following exemplary embodiment described.
Beispiel Zu einer mit Schwefel- und Goldverbindungen sensibilisierten und auf optimale Empfindlichkeit digerierten Brom-Jodsilberemulsion werden Pd-Glycinchelat, Pd-Glutaminsäurechelat und Pd-Hisfidinchelat im Vergleich zu Pd(N0,), und (NHJ,PdC1 als Gießzusatz vor dem Verguß der Emulsion zugesetzt. Es wurde von den einzelnen Palladiumchelatverbindungen so viel der Emulsion zugesetzt, daß sie im Vergleich zu Pd(N0,), bzw. (NH,),PdC1, die gleiche Menge Palladium enthalten. Die Emulsion wurde auf eine Filmunterlage vergossen und getrocknet.Example of one sensitized with sulfur and gold compounds and bromine-iodine-silver emulsion digested for optimal sensitivity, Pd-glycine chelate, Pd-glutamic acid chelate and Pd-hisfidine chelate compared to Pd (N0,), and (NHJ, PdC1 added as a pouring additive before pouring the emulsion. It was made by the individual Palladium chelate compounds added so much to the emulsion that they were compared to Pd (N0,), or (NH,), PdC1, contain the same amount of palladium. The emulsion was poured onto a film base and dried.
Von dem getrockneten Film werden Proben zwischen zwei Röntgenverstärkerfolien hinter einer Alu-Treppe mit Röntgenstrahlen belichtet. Die belichteten Proben werden in einem handelsüblichen Röntgenentwickler 5 Minuten und 10 Minuten bei 20'C entwickelt. Außerdem wird zur Haltbarkeitsprüfung eine Lagerung des Films bei 55'C und 700/, relativer Feuchtigkeit über 96Stunden durchgeführt. Diese Proben werden in der üblichen Weise belichtet und 5 Minuten im Röntgenentwickler entwickelt.Samples of the dried film are exposed to X-rays between two X-ray intensifying screens behind an aluminum staircase. The exposed samples are developed in a commercially available X-ray developer for 5 minutes and 10 minutes at 20 ° C. In addition, storage of the film at 55 ° C and 700 / relative humidity for 96 hours is carried out to test the durability. These samples are exposed in the usual way and developed for 5 minutes in the X-ray developer.
In der nachfolgenden Tabelle sind die Ergebnisse der photographischen
Prüfung des frischen Films und nach der Lagerung bei erhöhter Temperatur und erhöhter
Feuchtigkeit zusammengestellt. Als Maß für die Empfindlichkeit wurde die Abweichung
der Schwärzung bei gleicher Belichtung bei S = 1,0 bestimmt.
Claims (2)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DEP31717A DE1157077B (en) | 1963-04-30 | 1963-04-30 | Process for the preparation of photographic silver halide emulsions stabilized with palladium salts |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DEP31717A DE1157077B (en) | 1963-04-30 | 1963-04-30 | Process for the preparation of photographic silver halide emulsions stabilized with palladium salts |
Publications (1)
Publication Number | Publication Date |
---|---|
DE1157077B true DE1157077B (en) | 1963-11-07 |
Family
ID=7372421
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DEP31717A Pending DE1157077B (en) | 1963-04-30 | 1963-04-30 | Process for the preparation of photographic silver halide emulsions stabilized with palladium salts |
Country Status (1)
Country | Link |
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DE (1) | DE1157077B (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4154810A (en) * | 1977-11-26 | 1979-05-15 | The Japan Carlit Co., Ltd. | Manufacture of chlorine dioxide by reduction of a specified chlorate |
EP0722115A1 (en) * | 1994-12-16 | 1996-07-17 | Eastman Kodak Company | Photographic element and coating composition |
US5650265A (en) * | 1995-12-22 | 1997-07-22 | Eastman Kodak Company | Silver halide light-sensitive element |
-
1963
- 1963-04-30 DE DEP31717A patent/DE1157077B/en active Pending
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4154810A (en) * | 1977-11-26 | 1979-05-15 | The Japan Carlit Co., Ltd. | Manufacture of chlorine dioxide by reduction of a specified chlorate |
EP0722115A1 (en) * | 1994-12-16 | 1996-07-17 | Eastman Kodak Company | Photographic element and coating composition |
US5614360A (en) * | 1994-12-16 | 1997-03-25 | Eastman Kodak Company | Photographic element and coating composition |
US5650265A (en) * | 1995-12-22 | 1997-07-22 | Eastman Kodak Company | Silver halide light-sensitive element |
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