CN107478645B - Preparation and application of stainless steel surface ferrite pollution color development detection reagent - Google Patents

Preparation and application of stainless steel surface ferrite pollution color development detection reagent Download PDF

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CN107478645B
CN107478645B CN201710617511.1A CN201710617511A CN107478645B CN 107478645 B CN107478645 B CN 107478645B CN 201710617511 A CN201710617511 A CN 201710617511A CN 107478645 B CN107478645 B CN 107478645B
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stainless steel
color development
cellulose ether
detection reagent
ferrite
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CN107478645A (en
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周志证
程从前
赵杰
赵登攀
赖摇铃
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ZHOU ZHIZHENG
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Guangzhou Industrial And Environmental Protection New Materials Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour

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Abstract

The invention discloses a preparation method and application of a stainless steel surface ferrite pollution color development detection reagent. A preparation method of a stainless steel surface ferrite pollution color development detection reagent comprises the following steps: 1) dissolving nonionic cellulose ether in water at the temperature of 60-100 ℃ to prepare a thickening agent solution; 2) adding phenanthroline color developing agent and polyether siloxane surfactant into the thickener solution, stirring and mixing, cooling to room temperature to prepare a detection reagent stock solution, and inspecting and packaging the stock solution to obtain the stainless steel surface ferrite pollution color developing detection reagent. Also discloses a method for detecting the ferrite pollution color development on the surface of stainless steel. The invention improves the defects of the phenanthroline method in the practical application process, omits a filter paper material, improves the detection efficiency, enables large-area detection to be possible, and has very high practical application significance.

Description

Preparation and application of stainless steel surface ferrite pollution color development detection reagent
Technical Field
The invention relates to a preparation method and application of a stainless steel surface ferrite pollution color development detection reagent.
Background
Stainless steel is widely used in various industries such as nuclear energy, chemical industry, medicine, food, building, appearance decoration and the like due to good chemical properties, physical and mechanical properties, processability and exquisite appearance metal texture. Ferrite pollution at the joint of stainless steel and welding seams thereof is a phenomenon commonly existing in material application. Such contamination can result from a variety of factors, including: the processing process, the transportation process and the like are in contact with different materials, and the environmental impurities are in contact with corrosion or pollution and the like. The pollution can cause various undesirable consequences, namely rust spots and rust stains are generated to affect the appearance, the service life of the material is influenced seriously, and even the hidden danger of secondary catastrophic consequences can be generated, and the method is particularly applied to the engineering fields of nuclear power, chemical industry and the like with nearly strict requirements on the quality of the material.
At present, methods for detecting ferrite pollution on the surface of stainless steel are many, and a potassium ferricyanide-nitric acid test method, a copper sulfate method and a phenanthroline method are most representative. The sensitivity of the copper sulfate method is insufficient; the potassium ferricyanide-nitric acid method, i.e. the blue spot method, has the potential hidden danger of damaging the base material and the defects of unstable reagent, potential toxicity and the like. In order to overcome the defects of the blue spot method, CN101825574A discloses a method for detecting iron pollution by using a phenanthroline reagent, which has the characteristics of sensitive and rapid color development, simple and convenient use, no pollution and no surface damage. The method realizes color development detection by soaking and pasting the filter paper on the surface of the detected material, and has the problems of inconvenient construction, difficult large-area detection, low iron pollution positioning detection precision and the like in the actual detection process due to the difficulty in effective spreading of the filter paper after soaking. Therefore, CN102279182A discloses a detection membrane based on phenanthroline color developing solution, which realizes positioning and large-area detection of iron contamination, but the detection membrane is dried due to dehydration after being placed for a long time, and it is difficult to detect iron contamination on the surface of a component with a complex shape. How to rapidly form a detection film with high sensitivity on the surface of a part so as to meet the requirements of field detection and quality control management of parts with complex shapes such as nuclear power stations, petrochemical pump valves, pipelines, pipe racks and the like becomes a difficult point for developing a color reagent and a corresponding detection method.
Disclosure of Invention
The invention aims to provide a preparation method and application of a stainless steel surface ferrite pollution color development detection reagent.
The technical scheme adopted by the invention is as follows:
a preparation method of a stainless steel surface ferrite pollution color development detection reagent comprises the following steps:
1) dissolving nonionic cellulose ether in water at the temperature of 60-100 ℃ to prepare a thickening agent solution;
2) adding phenanthroline color developing agent and polyether siloxane surfactant into the thickener solution, stirring and mixing, cooling to room temperature to prepare a detection reagent stock solution, and inspecting and packaging the stock solution to obtain a stainless steel surface ferrite pollution color development detection reagent;
the mass ratio of the phenanthroline color developing agent to the nonionic cellulose ether to the polyether siloxane surfactant is 100: (1-10): (0.1-0.5).
The nonionic cellulose ether is at least one of methyl cellulose ether, ethyl cellulose ether, hydroxyethyl cellulose ether, hydroxypropyl cellulose ether, hydroxybutyl cellulose ether, hydroxyethyl methyl cellulose ether, hydroxypropyl methyl cellulose ether and hydroxybutyl methyl cellulose ether.
The polyether siloxane surfactant is at least one of Tego245, Tego250, Tego260, Tego265, Tego270, Tego280, Tego500 and Tego 505.
The package of the step 2) of the preparation method is a common sealed package or a binary package.
A method for detecting ferrite pollution color development on the surface of stainless steel comprises the following steps:
1) cleaning the surface of the stainless steel material to be measured;
2) spraying the prepared stainless steel surface ferrite pollution color development detection reagent on the surface of a detected material to form a reagent solution wet film on the surface of the detected material;
3) and observing the color development effect of the wet film of the reagent solution, and judging whether ferrite pollution exists according to whether the wet film develops red.
In the step 2) of the detection method, when the detection reagent is in a common sealed package, compressed air is used for spraying construction through a precision spray gun.
In the step 2) of the detection method, when the detection reagent is in a binary package, the spraying construction is directly carried out.
In the step 2) of the detection method, the construction distance between the spraying device and the surface of the detected material is 20-50 cm.
In the step 3) of the detection method, the color development time is 3-300 seconds.
The invention has the beneficial effects that:
the invention improves the defects of the phenanthroline method in the practical application process, omits a filter paper material, improves the detection efficiency, enables large-area detection to be possible, and has very high practical application significance.
Detailed Description
A preparation method of a stainless steel surface ferrite pollution color development detection reagent comprises the following steps:
1) dissolving nonionic cellulose ether in water at the temperature of 60-100 ℃ to prepare a thickening agent solution;
2) adding phenanthroline color developing agent and polyether siloxane surfactant into the thickener solution, stirring and mixing, cooling to room temperature to prepare a detection reagent stock solution, and inspecting and packaging the stock solution to obtain a stainless steel surface ferrite pollution color development detection reagent;
the mass ratio of the phenanthroline color developing agent to the nonionic cellulose ether to the polyether siloxane surfactant is 100: (1-10): (0.1-0.5).
Preferably, the nonionic cellulose ether is at least one of methyl cellulose ether, ethyl cellulose ether, hydroxyethyl cellulose ether, hydroxypropyl cellulose ether, hydroxybutyl cellulose ether, hydroxyethyl methyl cellulose ether, hydroxypropyl methyl cellulose ether, hydroxybutyl methyl cellulose ether; further preferably, the nonionic cellulose ether is hydroxyethyl cellulose ether. The nonionic cellulose ether of the present invention is a thickener.
The polyether siloxane surfactant is at least one of Tego245, Tego250, Tego260, Tego265, Tego270, Tego280, Tego500 and Tego 505; further preferably, the polyether siloxane surfactant is Tego 270.
The polyether siloxane surfactant adopted by the invention is used as a wetting agent, and aims to wet and spread the surface of a stainless steel substrate by a reagent solution, but cannot obviously promote color diffusion.
The phenanthroline color developing agent is a reagent consisting of citric acid, sodium citrate, phenanthroline and a reducing agent (hydroxylamine hydrochloride or ascorbic acid), and CN101825574A, CN102279182A and the like disclose related components and matching proportions.
Preferably, the packaging of step 2) of the preparation method is a normal sealed packaging or a binary packaging.
Further, the common sealing package is a sealing package under normal temperature and normal pressure. The packaging material of the common sealed package does not contain aluminum, magnesium and alloy thereof, carbon steel or cast iron, and can be selected from glass bottles, plastic bottles and the like. The detection reagent in common sealing package is sprayed by a precise spray gun by using compressed air.
Furthermore, the binary package is that a capsule is put in a pressure tank, a detection reagent is put in the capsule, the mouth of the capsule is connected with a nozzle, and compressed air is filled between the capsule and the pressure tank. The binary packaging pressure tank is made of metal selected from aluminum, magnesium and alloy thereof, carbon steel or cast iron and the like. The binary package is constructed by extruding a detection reagent through a nozzle and atomizing and spraying the detection reagent by means of the pressure of compressed air on the capsule.
A method for detecting ferrite pollution color development on the surface of stainless steel comprises the following steps:
1) cleaning the surface of the stainless steel material to be measured;
2) spraying the prepared stainless steel surface ferrite pollution color development detection reagent on the surface of a detected material to form a reagent solution wet film on the surface of the detected material;
3) and observing the color development effect of the wet film of the reagent solution, and judging whether ferrite pollution exists according to whether the wet film develops red.
In the step 2) of the detection method, the method is divided into two construction modes according to the packaging form of the detection reagent: when the detection reagent is in common sealed package, compressed air is used for spraying construction through a precision spray gun; and when the detection reagent is in a binary package, directly spraying for construction.
Further, when the detection reagent is in a common sealed package, compressed air is used for spraying construction through a precision spray gun, and the minimum pressure of air supplied to the spray gun is 35 psi.
Further, when the detection reagent is in a binary package, the pressure of compressed air in the binary package is 100-120 psi.
Preferably, in the step 2) of the detection method, the construction distance between the spraying device and the surface of the detected material is 20-50 cm, namely the construction distance between the precision spray gun or the binary packaging device and the surface of the detected material is 20-50 cm.
Preferably, in the step 3) of the detection method, the color development time is 3-300 seconds; more preferably, in the step 3) of the detection method, the color development time is 10 to 300 seconds.
Further, in step 3) of the detection method, if the wet film shows red color, ferrite contamination is present.
The present invention will be described in further detail with reference to specific examples.
The reagent solution is prepared by the following specific process according to the formula:
1. adding a certain amount of water into a glass bottle with a plastic stirring device;
2. gradually heating to 60-100 ℃ under stirring;
3. after the temperature is stable, adding the thickening agent while stirring, and maintaining the temperature until the thickening agent is completely dissolved;
4. maintaining the temperature, and adding the other components in the formula amount respectively;
5. cooling to room temperature while stirring, and packaging after quality inspection is qualified.
The reagent solution synthesized above has the following indices:
1. the coating has wettability and spreadability on a stainless steel base material;
2. has color developing capability to ferrite;
3. the color development of ferrite is positioned without diffusion;
4. the atomized wet film has no sagging phenomenon.
The method for carrying out the ferrite pollution on the surface of the stainless steel by using the reagent solution comprises the following steps:
1. cleaning the surface of the tested material by using clean water to remove dust particles; if heavy oil dirt exists, the heavy oil dirt also needs to be cleaned; the reagent solution has the capability of removing slight oil stains;
2. constructing the surface of a detected base material at a distance of 20-50 cm, so that a thin and uniform reagent solution wet film is formed on the surface of the detected base material;
3. the color development effect of the surface of the static viewing reagent wet film is developed within 3-300 seconds;
4. after the detection is finished, the reagent solution is lightly wiped by wet cloth and then is washed clean by clear water; the waste water after cleaning is nontoxic and pollution-free and can be directly discharged.
The following describes the present invention with reference to practical examples.
Selecting a 316 stainless steel plate with 100 x 100cm as a base material, and cleaning and dust-free the surface; the ferrite body was prepared by marking the surface of 316 stainless steel with tinplate.
Referring to CN101825574A, two groups of phenanthroline reagent solutions, comparative example 1 and comparative example 2, were prepared, and the formulation compositions are shown in table 1 below. The reagent solution of the present invention is example 1, and its formulation composition is also shown in Table 1. Three sets of experiments each were run with 5 parallel panel tests. The construction methods of the three groups of spraying detection reagents are consistent, and all the detection reagents are ordinary sealed and packaged, and the spraying construction is carried out by using compressed air through a precision spray gun. This construction method is a preferred example of the present invention. The construction method of the invention is not limited to spray gun spraying construction, and can also be used for binary packaging construction, and is not further limited, and different construction modes can be selected according to actual conditions, so that the detection effect of the invention can be realized.
TABLE 1 test formulations for comparative examples and examples
The results show that:
comparative example 1: the scratches show red marks, and the diffuse diffusion of red is caused because the reagent solution diffuses, so that the color points are difficult to locate;
comparative example 2: red linear traces appear on scratches, the color appears by permeating through filter paper, the reagent is slightly slow and slightly diffused, and the accurate positioning is difficult;
example 1: the scratch has red linear trace, is clear and stable, has no color condensation and diffusion, and has sensitive, quick and accurate color development.
Compared with the prior art, the invention has the following advantages:
1. thickening of the reagent solution: on the premise of keeping the pH value of the phenanthroline reagent solution in a buffer solution, the reagent is thickened, so that the reagent is colored and has coagulability, the diffusion is effectively prevented, and the pollution point is accurately positioned;
2. wet spreading of reagent solution: because the surface tension of the reagent solution is large and the reagent solution is not easy to wet and spread on the surface of the stainless steel, the reagent solution after being viscous and thickened is not easy to form a uniform wet film after being atomized, the problem is solved by adding the surfactant, and the diffuse diffusion of the color is not obviously influenced;
3. the construction mode of spraying compressed air by a precision spray gun or directly spraying by a binary packaging device is provided, the method for attaching the filter paper is improved, the filter paper is saved, the construction efficiency is improved, and meanwhile, large-area detection is realized.

Claims (8)

1. A preparation method of a stainless steel surface ferrite pollution color development detection reagent is characterized by comprising the following steps: the method comprises the following steps:
1) dissolving nonionic cellulose ether in water at the temperature of 60-100 ℃ to prepare a thickening agent solution;
2) adding phenanthroline color developing agent and polyether siloxane surfactant into the thickener solution, stirring and mixing, cooling to room temperature to prepare a detection reagent stock solution, and inspecting and packaging the stock solution to obtain a stainless steel surface ferrite pollution color development detection reagent; the mass ratio of the phenanthroline color developing agent to the nonionic cellulose ether to the polyether siloxane surfactant is 100: (1-10):
(0.1 to 0.5); the polyether siloxane surfactant is at least one of Tego245, Tego250, Tego260, Tego265, Tego270, Tego280, Tego500 and Tego 505.
2. The method for preparing a color development detection reagent for ferrite contamination on a stainless steel surface according to claim 1, characterized in that: the nonionic cellulose ether is at least one of methyl cellulose ether, ethyl cellulose ether, hydroxyethyl cellulose ether, hydroxypropyl cellulose ether, hydroxybutyl cellulose ether, hydroxyethyl methyl cellulose ether, hydroxypropyl methyl cellulose ether and hydroxybutyl methyl cellulose ether.
3. The method for preparing a color development detection reagent for ferrite contamination on a stainless steel surface according to claim 1, characterized in that: the package of step 2) is a common sealed package or a binary package.
4. A detection method for ferrite pollution color development on the surface of stainless steel is characterized by comprising the following steps: the method comprises the following steps:
1) cleaning the surface of the stainless steel material to be measured;
2) spraying the stainless steel surface ferrite pollution color development detection reagent prepared according to any one of claims 1-3 on the surface of a detected material to form a reagent solution wet film on the surface of the detected material;
3) and observing the color development effect of the wet film of the reagent solution, and judging whether ferrite pollution exists according to whether the wet film develops red.
5. The method for detecting the ferrite contamination color development on the surface of stainless steel according to claim 4, wherein: and in the step 2), when the detection reagent is in a common sealed package, compressed air is used for spraying construction through a precision spray gun.
6. The method for detecting the ferrite contamination color development on the surface of stainless steel according to claim 4, wherein: and in the step 2), when the detection reagent is in a binary package, directly spraying and constructing.
7. The method for detecting ferrite contamination and color development on the surface of stainless steel according to claim 5 or 6, wherein: in the step 2), the construction distance between the spraying device and the surface of the material to be detected is 20-50 cm.
8. The method for detecting the ferrite contamination color development on the surface of stainless steel according to claim 4, wherein: in the step 3), the color development time is 3-300 seconds.
CN201710617511.1A 2017-07-26 2017-07-26 Preparation and application of stainless steel surface ferrite pollution color development detection reagent Active CN107478645B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5756275A (en) * 1995-11-30 1998-05-26 Fuji Photo Film Co., Ltd. Color-developing agent, silver halide photographic light-sensitive material and image-forming method
US5851749A (en) * 1995-11-30 1998-12-22 Fuji Photo Film Co., Ltd. Color-developing agent, silver halide photographic light-sensitive material and image-forming method

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101825574B (en) * 2010-04-16 2012-05-16 大连理工大学 Solution and method for detecting ferrite pollution on surface of austenitic stainless steel
CN102279182B (en) * 2011-05-12 2012-11-21 大连理工大学 Preparation method of detection membrane for iron pollution on surface of austenitic stainless steel

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5756275A (en) * 1995-11-30 1998-05-26 Fuji Photo Film Co., Ltd. Color-developing agent, silver halide photographic light-sensitive material and image-forming method
US5851749A (en) * 1995-11-30 1998-12-22 Fuji Photo Film Co., Ltd. Color-developing agent, silver halide photographic light-sensitive material and image-forming method

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Denomination of invention: Preparation and Application of a Reagent for Detecting Ferrite Contamination on Stainless Steel Surface

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