Indicator for detection of thermal history

• US 4,675,161 A
• Filed: 12/29/1983
• Issued: 06/23/1987
• Est. Priority Date: 12/29/1982
• Status: Expired due to Fees

• Current Assignee: Sakata Shokai Limited
• Original Assignee: Sakata Shokai Limited
• Inventors: Hirano, Isamu, Hashimoto, Harumi
• Primary Examiner(s): Marcus, Michael S.
• Application Number:
  US06/566,677
• Time in Patent Office: 1,272 Days
• Field of Search: 116/206, 116/207, 116/216, 116/217, 116/219, 374/160, 374/161, 374/162, 252/962, 422/55, 422/56, 422/58, 422/34, 422/236, 436/1, 436/2, 436/93, 436/142, 436/147, 427/413, 427/321.5, 427/321.3
• US Class Current: 422/401
• CPC Class Codes: C12Q 1/22 Testing for sterility conditions
• CPC Class Codes: G01N 31/22 using chemical indicators G01N31/02 takes precedence
• CPC Class Codes: Y10S 428/913 Material designed to be responsive to temperature, light, moisture
• CPC Class Codes: Y10T 428/249996 Ink in pores
• CPC Class Codes: Y10T 428/249997 Encapsulated liquid
• CPC Class Codes: Y10T 436/142222 Hetero-O [e.g., ascorbic acid, etc.]
• CPC Class Codes: Y10T 436/20 Oxygen containing

Abstract

An indicator comprising azo dye(s), epoxy compound(s) and a separating membrane can be utilized for detection of the completion of thermal sterilization treatment in the medical field and also for thermal inspection in such various fields as testing, instrumentation and the like. The indicator can be used also for detection of the completion of alkylene oxide gas sterilization treatment by ethylene oxide gas or the like.

Claims

1. An indicator for detection of thermal history which comprises:

(a) at least one azo dye selected from the group consisting of ##STR18## wherein each R₁ is a hydrogen or an undissociative substituent selected from the group consisting of halogen atoms, lower alkyl groups, lower alkoxy groups, alkoxy alkyl groups, aromatic groups, nitro group and acylamino group, and Y is a group of the formula ##STR19## wherein R₂ has the same definition as R₁ ;

(b) at least one epoxy compound selected from the group consisting of polyethylene oxides;

polypropylene oxides;

polybutylene oxides;

polyepichlorohydrins;

styrene oxide;

glycidyl phenyl ether;

diepoxy or triepoxy compounds obtained by the reaction between a polyhydric alcohol and epichlorohydrin;

epoxy compounds of the type of a glycidyl ester of an acid; and

epoxy resins of the glycidyl ester type, bisphenol A type, bisphenol F type, phenolic novolak type and polyalcohol ether type; and

(c) a separating membrane having a melting or softening point of 50°

to 300°

C., composed of a heat-melting or heat-softening material which does not react with said epoxy compound (b), and having a thickness of 0.5 to 200μ

;

said element (a) and said element (b) are adjacent through said separating member (c) thereby providing an indicator for detection of thermal history.

2. The indicator according to claim 1, wherein there are coated, on a substrate, the element (a) of at least one azo dye, the element (c) of a separating membrane and the element (b) of at least one epoxy compound in that order and in three layers.

3. The indicator according to claim 1, wherein the azo dye is a member selected from the group consisting of ##STR20##

4. The indicator according to claim 1, wherein the epoxy compound is a member selected from the group consisting of;

diepoxy or triepoxy compounds obtained by the reaction between a polyhydric alcohol selected from the group consisting of glycol, glycerine and bisphenol A and epichlorohydrin;

epoxy compounds of the type of a glycidyl ester of an acid selected from the group consisting of acrylic acid, methacrylic acid, acetic acid, lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid, adipic acid and maleic acid.

5. The indicator according to claim 1, wherein the element of the separating membrane is a member selected from the group consisting of vinyl acetate resins, vinyl chloride resins, ethylene-vinyl acetate copolymer resins, vinyl chloride-vinyl acetate copolymer resins, styrene resins, acrylic resins, polyamide resins, alkyd resins, petroleum resins, coumarone-indene resins, cyclized rubbers, urethane resins, styrene-acryl copolymer resins, styrene-maleic acid copolymer resins, maleic acid resins, rosin modified maleic acid resins, polyvinyl alcohols, polyvinyl acetals, zein, casein, CMC, shellac, acrylic emulsions, styrene-acryl emulsions, styrene-shellac emulsions and vinyl acetate emulsions.

6. The indicator according to claim 1 attached to a label.

7. The indicator according to claim 1 attached to a tape.

8. The indicator according to claim 1 attached to a test piece.

9. The indicator according to claim 1 attached to a bag.

10. The indicator according to claim 1, wherein an acid catalyst for controlling the reaction between said azo dye and said epoxy compound is further present therein.

11. The indicator according to claim 10, wherein the acid catalyst is at least one member selected from the group consisting of phosphoric acid, p-toluenesulfonic acid, citric acid, maleic acid and malonic acid.

12. The indicator according to claim 1, wherein said undissociative substituent is selected from the group consisting of methyl, ethyl, propyl, butyl, methoxy, ethoxy, propoxy, butoxy, ethylol, methylol, methoxy methyl, phenyl, phenoxy, benzyl and nitro.

13. The indicator according to claim 12, wherein the element of the separating membrane is a member selected from the group consisting of vinyl acetate resins, vinyl chloride resins, ethylene-vinyl acetate copolymer resins, vinyl chloride-vinyl acetate copolymer resins, styrene resins, acrylic resins, polyamide resins, alkyd resins, petroleum resins, coumarone-indene resins, cyclized rubbers, urethane resins, styrene-acryl copolymer resins, styrene-maleic acid copolymer resins, maleic acid resins, rosin modified maleic acid resins, polyvinyl alcohols, polyvinyl acetals, zein, casein, CMC, shellac, acrylic emulsions, styrene-acryl emulsions, styrene-shellac emulsions and vinyl acetate emulsions.

14. The indicator according to claim 13, wherein an acid catalyst for controlling the reaction between an azo dye and an epoxy compound is further present therein.

15. The indicator according to claim 14, wherein the acid catalyst is at least one member selected from the group consisting of phosphoric acid, p-toluenesulfonic acid, citric acid, maleic acid and malonic acid.

16. The indicator according to claim 15, wherein the element (b) of at least one epoxy compound is contained in microcapsules whose shell is the element (c) of a separating membrane.

17. The indicator according to claim 12, wherein the element (b) of at least one epoxy compound is contained in microcapsules whose shell is the element (c) of a separating membrane.

18. The indicator according to claim 17, wherein a uniform mixture of the element (a) of at least one azo dye and the microcapsules is coated on a substrate in the form of a layer.

19. The indicator according to claim 17, wherein the element (a) of at least one azo dye is coated on a substrate in the form of a layer and thereon the microcapsules are coated also in the form of a layer.

20. The indicator according to claim 13, wherein the acid catalyst is at least one member selected from the group consisting of phosphoric acid, p-toluenesulfonic acid, citric acid, maleic acid and malonic acid.

21. The indicator according to claim 20, wherein the element (b) of at least one epoxy compound is contained in microcapsules whose shell is the element (c) of a separating membrane.

22. The indicator according to claim 12, wherein an acid catalyst for controlling the reaction between an azo dye and an epoxy compound is further present therein.