JPH0572148A - Permeation type defect searching test method and cleaning liquid used in this method - Google Patents

Abstract

PURPOSE:To obtain the result of searching defects efficiently and with high precision by carrying out the permeation type defect searching test method through a closed loop system free from the discharge of the cleaning waste liquid. CONSTITUTION:The permeation processing in which an oily permeation liquid which does not contain a surfactant is applied onto the surface of an inspected article and the permeation liquid is permeated into a defect part is carried out. Then, the cleaning water in which the inorganic salts selected from among the alkaline metals, alkaline- earth metals, and ammonia having an ion diameter parameter of 3-8Angstrom in the dissolved state into water is dissolved in 0.2-0.5wt.% into water is sprayed under a water pressure of 6kg/cm<2> or mpre, and the excessive permeation liquid which is left without permeating into a defect part is cleaing-removed, and the cleaning water which is obtained by separating the excessive permeation liquid by the oil/water separation due to specific gravity difference from the cleaning water containing the excessive permeation liquid formed by the above-described cleaning process is used repeatedly in spreading, After the drying processing of the defect part is searched by the permeation liquid which permeates into the defect part.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a penetrant testing method and a cleaning liquid used in the method, and provides a penetrant testing method capable of efficiently carrying out a penetrant testing without causing pollution problems caused by cleaning waste liquid. It is a thing.

[0002]

2. Description of the Related Art As is well known, the penetrant flaw detection test method has been widely used for a long time for flaw detection of defects such as fine cracks and fine pinholes existing on the surfaces of various devices and members, and is described in "JIS-Z2343". -1982 ". The basic mode is to apply a penetrant with strong permeability, which is obtained by dissolving an oil-soluble visible or fluorescent dye in a solvent, to the surface of the object to be inspected, and then permeate the penetrant into the defect part, and then penetrate the defect part. Instead, the excess penetrant liquid remaining on the surface of the object to be inspected is removed, and the presence of the defect part is detected by the penetrant liquid penetrating the defect part.

The above-mentioned penetrant flaw detection test method has various concrete embodiments depending on the kind of penetrant used and the type of treatment means for removing the excess penetrant. 56-37501 (hereinafter referred to as "first publication")
And Japanese Patent Publication No. 59-28860 (hereinafter referred to as “second
There is a penetrant flaw detection test method which takes the following specific embodiments disclosed in "Gazette". That is, in the first publication,
As the penetrant, an oil-based penetrant that is composed of an oil-based solvent that is not compatible with water and an oil-soluble fluorescent dye and does not contain a surfactant is used, and water vapor is used as a treatment means for removing the excess penetrant. An osmotic flaw detection test method of performing a treatment of spraying the surface of the object to be inspected with an injection pressure of ˜5 kg / cm ² is disclosed, and the second publication discloses an oil that is not compatible with water as a penetrant. A hydrophobic penetrant containing no surfactant and composed of a system solvent and an oil-soluble fluorescent dye or an oil-soluble red dye is used.
A penetrant flaw detection test method is disclosed in which spraying is performed on the surface of an object to be inspected with a water pressure of 4 kg / cm ² .

Then, the first publication describes that "the waste liquid is easily separated into oil and water" (first publication, column 8, lines 19 to 20).
In the second publication, it is described that "the permeate and water can be easily separated by the difference in specific gravity, and the stationary liquid can separate the permeate and water in a short time" (second publication, column 3, lines 14 to 16). As described above, according to the penetrant testing method disclosed in the first and second publications (hereinafter, referred to as "known penetrant testing method"), the excess penetrant is generated by the cleaning treatment using water. It is said that since the permeate can be separated from the water containing the excess permeate (waste liquid) by oil-water separation due to the difference in specific gravity, the treatment of the cleaning waste liquid becomes easy and does not cause pollution problems.

[0005] The surfactant-free oily penetrant used in the known penetrant flaw detection test method is called a solvent-removable fluorescent (or dyeing) penetrant, and there are many commercially available products. The formulation is 2 to 5 parts of an oil-soluble dye, 10 to 40 parts of a base solvent for dissolving the dye, and 50 to 50 of a diluting solvent.
It is 90 parts and is usually used in combination with a cleaning agent composed of an organic solvent.

[0006]

According to the known permeation flaw detection test method, the present inventor, as described above, removes the permeate from the water containing the excess permeate produced by the washing treatment by separating the oil and water by the difference in specific gravity. Focusing on the fact that separation is possible, from the viewpoint of pollution control, cleaning treatment cost reduction (especially water saving), the idea of performing cleaning treatment by repeatedly using water from which permeate has been separated Got Also,
In realizing the above idea, the inventor of the present invention has the equipment, operability, water-operated means for spraying water, which is disclosed in the second publication, rather than the means for using water vapor disclosed in the first publication. It was judged that it was advantageous in terms of setting the circulation system route. Therefore, starting each of the penetrant liquids exemplified in the first and second publications,
Experiments were carried out using all of the available commercially available oil-free penetrants and found to have the following problems.

That is, the first problem is at room temperature (20-25
(2) The separation of the permeate by oil-water separation in a stationary state at a temperature of ℃) requires a long time of at least about 30 minutes or more. The second problem is 4 kg when water is used instead of steam. It is a point that the excess penetrant could not be sufficiently washed by spraying with a moderate water pressure unless a large amount of water was used, and a highly accurate flaw detection result could not be obtained. Therefore,
In view of the above problems, the present invention establishes a technical means that enables rapid separation of the permeate from the water containing the excess permeate generated by the cleaning process by oil-water separation at room temperature, and a relatively small amount. By establishing a technical means that can thoroughly wash the excess penetrant by spraying the wash water, and obtain highly accurate flaw detection results, the wash water from which the penetrant has been separated can be used repeatedly in the cleaning process, and the penetrant can penetrate efficiently. It is a technical issue to provide a new penetration flaw detection test method that can perform flaw detection tests.

[0008]

The above technical problems can be achieved by the present invention as follows.

That is, according to the present invention, a base solvent which is not compatible with water, a diluting solvent which is not compatible with water, and an osmotic liquid which is composed of an oil-soluble dye and does not contain a surfactant are coated. A cleaning process that is applied to the surface of the object to be inspected to permeate the penetrant liquid into the defective area, and then the excess penetrant remaining on the surface of the object to be inspected without penetrating into the defective area is washed away with water. In the penetrant flaw detection test method, in which a treatment is performed, and then a drying treatment for drying the surface of the inspection object is performed, and then the presence of the defect portion is inspected by the penetrant liquid that permeates the defect portion, the cleaning treatment is performed. 0.2 to 0.5% by weight of one or more inorganic salts selected from alkali metals, alkaline earth metals and ammonium having an ionic diameter parameter of 3 to 8Å in a state of being dissolved in water on the surface with respect to water. A small amount of dissolved wash water With blowing in Kutomo 6 kg / cm ² or more pressure the excess permeate wash water repeated use and separated by oil-water separation by specific gravity difference from the wash water containing the excess permeate resulting from the cleaning process該吹care- Penetrant testing method characterized by being carried out.

In addition, one or more inorganic salts selected from alkali metals, alkaline earth metals and ammonium having an ionic diameter parameter of 3 to 8Å in a state of being dissolved in water are added in an amount of 0.2 to 0. It is a cleaning liquid used for the penetrant testing method in which 5% by weight is dissolved.

The structure of the present invention will be described in more detail as follows. First, the penetrant testing method according to the present invention is the same as the conventional penetrant testing method except for the cleaning process. That is, the permeation treatment is carried out according to a conventional method as a penetrant, a commercially available solvent-removable fluorescent (or dyeing) penetrant, for example, "fluorescent penetrant OD-".
1700A "(trade name, manufactured by Mark Tech Co., Ltd.) and" Dyeing Penetrant P-ST "(trade name, manufactured by Mark Tech Co., Ltd.)
It is sufficient to apply this to the surface of the object to be inspected and to permeate the defective portion.

The drying treatment may also be carried out according to a conventional method by air-drying or heat-drying the surface of the object to be inspected after the washing treatment described later.

When the drying process is completed, the presence of the defective portion is detected by the penetrant liquid that has permeated the defective portion. Flaw detection,
According to a conventional method, when a fluorescent penetrant is used, it may be performed under irradiation of an ultraviolet lamp (black light) in a dark place, and when a dyeing penetrant is used, it may be performed under white light.

In the cleaning treatment, at least 6 kg / cm of the cleaning water according to the present invention is applied to the surface of the object to be inspected after the permeation treatment is completed.
^The washing water is sprayed at a water pressure of ² or more, and the washing water containing the excess penetrant generated by the washing treatment is separated from the excess penetrant by oil / water separation due to the difference in specific gravity.

In this case, with a water pressure of 6 kg / cm ² or more, the excess penetrant liquid remaining on the surface of the object to be inspected can be sufficiently washed without penetrating into the defective portion, and the higher the water pressure, the longer the washing time. Can be shortened, for example, 20 kg / cm
If the water pressure is ² , it can be sufficiently washed in 15 to 25 seconds.
10-30 kg / cm ² considering the cleaning time and equipment
Water pressure of some degree is practical. A well-known high-pressure pump and a spray nozzle can be used for spraying.

Further, the washing water according to the present invention sprayed on the surface of the object to be inspected is collected, and the excess permeate is separated by the oil-water separation due to the difference in specific gravity, and then sprayed again. It is sufficient to maintain the stationary state for 5 to 20 minutes, and the stationary state for 30 minutes or longer is not necessary at the longest. The separated penetrant liquid can be reused if it is not contaminated by dust adhering to the object to be inspected or dust around the location of the flaw detection test, and if it is heavily contaminated, it is treated by burning.

The cleaning liquid according to the present invention comprises one or more inorganic salts selected from alkali metals, alkaline earth metals and ammonium having an ionic diameter parameter of 3 to 8Å in a state of being dissolved in water (hereinafter referred to as "specific inorganic salts"). ") Is dissolved in water in an amount of 0.2 to 0.5% by weight.

Specific examples of the specific inorganic salts are as follows. Magnesium sulfate, ammonium sulfate, sodium sulfite, magnesium chloride, sodium hexametaphosphate, sodium nitrite, sodium carbonate, sodium tripolyphosphate, sodium orthosilicate, sodium hydrogen carbonate, monobasic sodium phosphate, sodium orthosilicate. The cleaning liquid according to the present invention can be easily prepared, and one or two or more of the above-mentioned specific inorganic salts can be weighed out and dissolved in water.

The amount of the specific inorganic salt dissolved is important. If the amount is less than 0.2% by weight with respect to water, the standing time required for oil-water separation due to the difference in specific gravity will exceed 30 minutes and excess permeate remaining on the surface of the object to be inspected will be removed. The cleaning time required for this is also long (for example, 20 kg /
When spraying with a water pressure of cm ² , about 35 seconds or more is required to perform sufficient washing. )turn into. These time shortening effects increase substantially in proportion to the dissolved amount, but the desired effect can be obtained up to 0.5% by weight with respect to water, so it is not necessary to set it to 0.5% by weight or more. .. A practically preferable dissolved amount is in the range of 0.35 to 0.45% by weight with respect to water.

If necessary, a commercially available water-soluble rust preventive (for example, triethanolamine) can be added to the cleaning water according to the present invention. Will not be adversely affected.

Next, in carrying out the penetrant flaw detection test method according to the present invention as described above, if a penetrant having a specific gravity of less than 1 is used, the stationary state required for oil-water separation due to the difference in specific gravity is maintained. The time can be shortened further. Examples of the penetrant having a specific gravity of less than 1 include those having the following formulations.

2 to 5 parts of oil-soluble dye, trioctyl phosphate, tributyl phosphate, dioctyl phthalate, dibutyl maleate, dinonyl phthalate, dioctyl dodecanedioate, and dioctyl fumarate. 40 parts, xylene, dimethylnaphthalene, creosote oil, solvent naphtha, Solvesso 100 (trade name, manufactured by Exxon) and KMC113
A penetrant liquid containing no surfactant and consisting of 50 to 90 parts of a diluting solvent consisting of one or more of (trade name, manufactured by Kureha Co., Ltd.).

Further, as the washing water, 0.2 to
By using a solution containing 0.5% by weight of sodium pyrophosphate or sodium metasilicate dissolved therein, it is possible to shorten the cleaning time required to remove the excess penetrant remaining on the surface of the inspection object. ..

[0024]

The operation of the present invention is as follows. First, in the method of the present invention, at least 6 kg / c is applied to the surface of the inspection object.
15 ~ by spraying the wash water according to the present invention at a water pressure of m ² , preferably 10-30 kg / cm ^2.
In a short time of 25 seconds, the surplus penetrant remaining on the surface of the object to be inspected can be sufficiently washed. This is because the washing water according to the present invention dissolves a specific amount of a specific inorganic salt. to cause. This is because, as described above, when merely spraying water, sufficient cleaning cannot be performed in such a short time.

Next, in the method of the present invention, 5
With a short standing time of ~ 30 minutes, the excess permeate can be separated from the wash water containing the excess permeate produced by the washing treatment by oil-water separation due to the difference in specific gravity. This is because the wash water contains a specific amount of a specific inorganic salt dissolved therein. Because,
This is because, as described above, the excess permeate cannot be separated in such a short time when only water is used.

Unfortunately, the theoretical elucidation of each of the above-mentioned time-reducing actions of the wash water according to the present invention, in other words, the water in which a specific amount of a specific inorganic salt is dissolved, has not yet been carried out. The inventor has found that even when the same inorganic salt is used, when sodium pyrophosphate or sodium metasilicate is used, even if it has a remarkable effect of shortening the cleaning time, the stationary state holding time for oil-water separation Based on the fact that the shortening effect is relatively small, it is considered that there is a key to elucidation of the ionic diameter parameter of a specific inorganic salt in a state of being dissolved in water.

Incidentally, Japanese Patent Application Laid-Open No. 51-138055 and Japanese Patent Application Laid-Open No. 1-210004 disclose technical means of using inorganic salts for oil-water separation, but these all use a surfactant. It is the separation of oil and water in the existing system, and the action is completely different from the separation of oil and water in the system in which the surfactant is not present in the present invention.

[0028]

EXAMPLES Next, the present invention will be described in more detail by way of examples and comparative examples.

1. Preparation of Wash Water Each specific inorganic salt was dissolved in water to prepare the following 13 kinds of wash water. Wash water A: 30 l of wash water in which 0.45% by weight of magnesium sulfate is dissolved in water. Wash water B: 30 l of wash water in which 0.45% by weight of ammonium sulfate is dissolved in water. Wash water C: Wash water 3 in which 0.45% by weight of sodium sulfite is dissolved in water
0l. Wash water D: 30 l of wash water in which 0.45% by weight of magnesium chloride is dissolved in water. Wash water E: Sodium hexametaphosphate is 0.4 against water
30 l of washing water dissolved in 5% by weight. Wash water F: 30 l of wash water in which sodium nitrite is dissolved in 0.20% by weight with respect to water. Wash water G: 0.45% by weight of sodium carbonate based on water
30 l of dissolved wash water. Wash water H: Sodium tripolyphosphate is 0.45 with respect to water
30 liters of wash water dissolved in weight%. Wash water I: Sodium orthosilicate is 0.4 with respect to water
30 l of washing water dissolved in 5% by weight. Wash water J: 30 l of wash water in which 0.45% by weight of sodium hydrogen carbonate is dissolved in water. Wash water K: monobasic sodium phosphate is 0.45 with respect to water
30 liters of wash water dissolved in weight%. Wash water L: Sodium orthosilicate is 0.4 against water
30 l of washing water dissolved in 5% by weight.

Further, sodium pyrophosphate and sodium metasilicate were dissolved in water to prepare the following two kinds of washing water. Wash water M: sodium pyrophosphate is 0.45 with respect to water
30 liters of wash water dissolved in weight%. Wash water N: sodium metasilicate is 0.20 with respect to water
30 liters of wash water dissolved in weight%.

2. Oil-water separation test 100 ml of each of the washing waters A to N was weighed,
Each wash water was sealed in a mayonnaise empty bottle (150 CC) together with 0.2 ml of a commercially available solvent-removable fluorescent penetrant OD-1700A (described above), shaken for 1 minute with a paint shaker, and then at 25 ° C. The oil-water separation test was carried out by standing still and measuring the time until no fluorescent green was observed at all in the separation lower layer (wash water layer) under irradiation of an ultraviolet lamp with the naked eye. Table 1 shows the time from the time of standing to the time when no fluorescent green color was observed at all. For comparison, Table 1 also shows the results of an oil-water separation test conducted in the same manner as above using just water.

3. Detergency test Using each of the above-mentioned cleaning waters A to N, a OD-
1700A (above) was applied using a brush, left for 5 minutes, and then sprayed with washing water at a water pressure of 20 kg / cm ² , and the fluorescent green was visually observed on the coated surface under irradiation of an ultraviolet lamp. A detergency test was performed by measuring the time until it was not observed at all using a stopwatch. Table 1 shows the time from the start of spraying to the time when no fluorescent green color was observed at all. In addition, in Table 1,
For comparison, the results of the detergency test conducted in exactly the same manner as above using pure water are also shown.

[Table 1]

4. Implementation of Penetrant Testing Method Using the above-mentioned cleaning water A, the following fluorescent penetrant testing method was implemented. A B-type test piece of JIS-Z-2343-1982 standard (break depth: 50 μ) was pretreated by ultrasonic cleaning in acetone for 30 minutes, and then the test surface was brushed to OD-1700A (previously described). ) Is applied and left for 5 minutes to perform an infiltration treatment, and then a high pressure pump (MW-310 type: manufactured by Maruyama Seisakusho) and a nozzle hole diameter of 1 are applied to the applied surface.
mm spray with a water pressure of 20 kg / cm ² ,
Washing is performed by spraying water for 20 seconds in a flat spray with a spray angle of 25 °, and then the test piece is kept at 80 ° C for 2 seconds.
After performing a drying treatment for drying for a minute, the test surface was visually observed in the dark under irradiation of an ultraviolet lamp. In addition, the cleaning water A containing the excess penetrant generated in the cleaning process
Was left at room temperature for about 10 minutes, and the permeate was separated by oil-water separation and used again for washing. As a result, a clear defect-indicating fluorescent pattern was visually confirmed on the test surface. The oil-water separation of the wash water A containing the excess permeate also proceeded smoothly by standing for about 10 minutes, and the transparent wash water A could be repeatedly used for washing.

5. Execution of Penetrant Testing Method Using the above-described cleaning water B, the following dye penetrant testing method was carried out. A B-type test piece of JIS-Z-2343-1982 standard (break depth: 50 μ) was pretreated by ultrasonic cleaning in acetone for 30 minutes, and then the test surface was brushed with a commercially available solvent-removable dye. Penetrating liquid PS
T (above) is applied and left to stand for 5 minutes for the permeation treatment, and then a high pressure pump (MW-310 type:
(Maruyama Manufacturing Co., Ltd.) and a spray having a nozzle hole diameter of 1 mm are used to perform a cleaning treatment of spraying cleaning water B for 20 seconds at a water pressure of 20 kg / cm ² and at a flat spray angle of 25 °. Is dried naturally, and then a thin layer of white inorganic differential powder (commercially available developer for penetrant flaw detection) is formed on the test surface according to a conventional method, and then the test surface is visually observed under white light. I observed. The wash water B containing the excess permeate generated in the washing treatment was left standing at room temperature for about 15 minutes to separate the permeate by oil / water separation and used again for washing. As a result, a clear defect indicating red pattern was confirmed on the test surface with the naked eye. Further, the oil-water separation of the wash water B containing the excess permeate also proceeded smoothly by standing for about 15 minutes, and the transparent wash water B could be repeatedly used for washing.

6. Execution of Penetrant Testing Method Using the above-mentioned cleaning water E, the following fluorescent penetrant testing method was carried out. A B-type test piece of JIS-Z-2343-1982 standard (break depth: 50 μ) was pretreated by ultrasonic cleaning in acetone for 30 minutes, and then a penetrant of the following formulation was applied to the test surface by brushing. The coating is applied and left to stand for 5 minutes for the permeation treatment, and then the coating surface is covered with a high-pressure pump (MW-310 type: manufactured by Maruyama Seisakusho) and a nozzle hole diameter of 1 mm.
And a spray treatment of 25 kg / cm ² at a spray angle of 25 °, and spraying water for about 20 seconds to perform a cleaning treatment, and then drying the test piece at 80 ° C. for 2 minutes. Then, the test surface was visually observed in the dark under irradiation of an ultraviolet lamp. The wash water E containing the excess permeate generated in the washing treatment was allowed to stand at room temperature for about 10 minutes to separate the permeate by oil / water separation and used again for washing. As a result, a clear defect-indicating fluorescent pattern was visually confirmed on the test surface. Further, the oil-water separation of the wash water E containing the surplus penetrant also proceeded smoothly by standing for about 10 minutes, and the transparent wash water E could be repeatedly used for washing. The formulation of the fluorescent penetrant is as follows. Florescent St. Brightnis Agent 75 (trade name, manufactured by Morton) 1 part Florescent St. Brightnis Agent 68 (trade name, manufactured by Nippon Kayaku) 2 parts Solvesso 150 (trade name, manufactured by Exxon Co.) 68 parts Isopar G ( (Product name, manufactured by Exxon) 19 parts Octyl phosphate 10 parts

7. Execution of Penetrant Testing Method Using the cleaning water M, the following fluorescent penetrant testing method was carried out. A B-type test piece of JIS-Z-2343-1982 standard (break depth: 50 μ) was pretreated by ultrasonic cleaning in acetone for 30 minutes, and then the test surface was brushed to OD-1700A (previously described). ) Is applied and left for 5 minutes to perform an infiltration treatment, and then a high-pressure pump (MW-310 type: manufactured by Maruyama Seisakusho) and a spray having a nozzle hole diameter of 1 mm are used to apply water pressure of 20 kg / cm to the applied surface.
² , a flat spray with a spray angle of 25 ° is sprayed with water for about 15 seconds, and then the test piece is heated to 80
A drying process of drying at 0 ° C. for 2 minutes was performed, and the test surface was visually observed in the dark under irradiation of an ultraviolet lamp.
The wash water M containing excess permeate generated in the washing treatment was left standing at room temperature for about 35 minutes to separate the permeate by oil / water separation and used again for washing. As a result, a clear defect-indicating fluorescent pattern was visually confirmed on the test surface. Further, for the oil-water separation of the wash water M containing the excess permeate,
Although it was required to stand for about 35 minutes, clear washing water M could be separated and repeatedly used for washing.

[0037]

As described above, according to the present invention as described above,
Since the penetrant can be completely separated in a short time of 5 to 30 minutes in a stationary state at room temperature, efficient cleaning water can be repeatedly used, and the penetrant flaw detection test method can be efficiently performed by the closed loop method that does not generate cleaning waste liquid. , Can be implemented. Further, according to the present invention, the excess penetrant remaining on the surface of the object to be inspected can be sufficiently washed in a short time of 15 to 25 seconds, so that an efficient and highly accurate flaw detection result can be obtained. Therefore, it can be said that the industrial applicability of the present invention is extremely high.

Claims (2)

[Claims] 1. A penetrant containing a base solvent which is not compatible with water, a diluting solvent which is not compatible with water, and an oil-soluble dye, and which does not contain a surfactant, on the surface of the object to be inspected. After the coating, a permeation treatment is performed to permeate the permeation liquid into the surface opening defect (hereinafter referred to as "defect"), and then the excess permeation liquid remaining on the surface of the object to be inspected without permeating into the defect is treated with water. After performing a cleaning process of cleaning and removing by using, followed by a drying process of drying the surface of the object to be inspected, in the penetrant flaw detection test method for detecting the presence of a defective part by the penetrant liquid that has permeated the defective part, In the state of being dissolved in water on the surface of the object to be inspected, one or two or more kinds of inorganic salts selected from alkali metals, alkaline earth metals and ammonium having an ionic diameter parameter of 3 to 8 Å are mixed with 0.2 to water.
~ 0.5 wt% of at least 6 kg of dissolved wash water
/ Cm ² or more of water pressure, and the washing water containing the excess permeate generated by the washing treatment in the spraying is repeatedly used with the wash water separated from the excess permeate by oil-water separation due to the difference in specific gravity. Penetrant testing method characterized by. 2. One or more inorganic salts selected from alkali metals, alkaline earth metals and ammonium having an ionic diameter parameter of 3 to 8 Å in a state of being dissolved in water, in an amount of 0.2 to 0. A cleaning liquid used in the penetrant testing method in which 5% by weight is dissolved.