JPH0412417B2 - - Google Patents

Description

[Detailed description of the invention]

The present invention relates to a penetrant liquid for penetrant flaw detection and a penetrant test method using the penetrant liquid. The present invention is based on the "Organic Solvent Poisoning Prevention Regulations" established by the Ministry of Labor of Japan, hereinafter abbreviated as "Organic Regulations". - The purpose of the present invention is to provide a penetrant liquid for penetrant flaw detection that does not fall under the category of hazardous materials according to the Fire Service Act and has highly sensitive flaw detection ability. Another object of the present invention is to provide a penetrant liquid for penetrant flaw detection that can be applied with a water or base cleaning liquid and has a highly sensitive flaw detection ability. A further object of the present invention is to provide a penetrant flaw detection method that can be carried out safely without being subject to regulations by organic regulations or the Fire Service Act, and which can provide highly sensitive flaw detection results. In general, penetrant testing is well known as a typical non-destructive testing method. This method is used to detect minute defects such as cracks and pinholes that are open on the surface of metals, ceramics, etc., and is particularly used to detect open defects on the surface of mechanical parts, mechanical parts and structures (for example, storage tanks). It is widely used to detect surface opening defects in welded parts of pipes, piping, etc.). As is well known, the embodiment of this penetrant flaw detection method consists of the following four operations. (1) Penetration operation: Apply oil-soluble visible (usually red) or fluorescent light (usually ultraviolet Highly permeable (usually surface tension 26-32dyne/
cm) A liquid - "penetrating liquid" - is applied by means such as coating, spraying, dipping, etc. and left until the penetrating liquid penetrates into the opening defect. Note that when the surface of the object to be inspected is clean, pre-cleaning is unnecessary. (2) Cleaning operation: Excess penetrating liquid remaining on the surface of the object to be inspected without penetrating into the opening defect is wiped off with a rag using a liquid such as a solvent or water - "cleaning liquid" - or by spray cleaning, etc. Remove by. (3) Development operation: Inorganic white fine powder - developer - is applied to the surface of the object to be inspected in order to suck out the penetrant remaining in the opening defect to the surface and enlarge and reveal the defect containing the penetrant. Form a uniform thin layer. (4) Inspection: After the development operation, the inorganic white fine powder layer is allowed to stand for a predetermined period of time, and the penetrating liquid is sucked out to the surface of the layer by capillary action, causing a defect-indicating bled pattern to appear.
When the dye is a visible dye, under white light,
When the dye is a fluorescent dye, defect indications are observed under ultraviolet lamp irradiation. The conventional techniques related to the penetrant liquid and cleaning liquid used in the penetrant flaw detection method as described above are as follows. First, the oldest known oil-soluble dyes are 0.5 to 3 parts by weight (hereinafter referred to as "parts"),
40 to 60 parts of high-boiling esters and 40 to 60 parts of oily organic solvent
There is a combination of a penetrating liquid with a composition of 60 parts and a cleaning liquid consisting of a petroleum-based organic solvent. In addition, a self-emulsifying penetrating liquid containing 0.5 to 3 parts of an oil-soluble dye, 5 to 20 parts of high-boiling esters, 60 to 80 parts of an oily organic solvent, and 5 to 30 parts of a surfactant, and a cleaning liquid consisting of water. Combinations of are also well known. Furthermore, in recent years,
Avoid the use of oil-based organic solvents from the perspective of regulations, and from the perspective of the Fire Service Act, combine water-based penetrants that use water as the main component and cleaning solutions consisting of water, and combine water-based penetrants and water-based cleaning solutions. A combination of these has been proposed. That is, it consists of a penetrating liquid with a composition composition of 0.01 to 3 parts of an oil-soluble dye, 5 to 40 parts of a surfactant, and 60 to 90 parts of water, as disclosed in, for example, JP-A-50-120389, and water. For example, Japanese Patent Application Laid-Open No. 50-104690 (Japanese Patent Publication No. 53-25673)
No.) A penetrating liquid and water having a composition composition disclosed in the publication and consisting of 1 to 1.5 parts of a water-soluble or alcohol-soluble dye, 0.1 to 30 parts of a surfactant, 0.1 to 50 parts of a water-soluble organic solvent, and 50 to 99.5 parts of water. , in combination with a water-based cleaning solution consisting of a water-soluble organic solvent and a surfactant. However, when penetrant testing is carried out by a combination of
The disadvantage is that the defect indication is low compared to the case of a combination of the above, and more specifically, the defect indication is difficult to observe because the appearance of the defect indication bleed pattern in the inspection in (4) above is unclear (insufficient). There is. fact,
The combination of is not yet popular, and the combination of is currently generally adopted. In view of the above-mentioned current situation, the present inventor has conducted systematic research with the aim of obtaining flaw detection capability comparable to the flaw detection capability in the case of a combination of. Ta. In the case of a combination of the following, the factors that make it difficult to avoid the appearance of the defective bled pattern are mainly A. The amount of dye dissolved in the penetrant is insufficient, and B. It was discovered that the wettability of the penetrant to the test object was insufficient. Furthermore, when a water-soluble or alcohol-soluble dye is used as in the prior art example, the color density of the defect-indicating bleeding pattern is insufficient, and there is a tendency for so-called "over-cleaning" to occur in the cleaning operation described in (2) above. First, we conducted many experiments to find a formulation that could solve problems A and B, and we also confirmed that there was a risk of liquid separation due to changes over time from the viewpoint of stability during storage and penetrating power. As a result of repeated experiments in search of a one-component formulation of a solubilizing system rather than an emulsifying system, the penetrating liquid according to the present invention was completed. That is, the penetrant liquid for penetrant flaw detection (hereinafter referred to as
Improved penetrant. ) is as follows. 0.5 to 3 parts of oil-soluble dye, 5 to 25 parts of nonionic surfactant, 10 to 55 parts of water-soluble glycol ether or its ester with a boiling point of 200℃ or higher, 5 to 10 parts of aromatic carboxylic acid ester, boiling point center at 200℃ Above
Consisting of 1 to 5 parts of aliphatic hydrocarbon with a surface tension of 28 dyne/cm or less, the balance being water, 26 to 28 dyne/cm
It is an improved penetrating liquid with a surface tension of . The above-mentioned improved penetrant liquid can be handled as a substantially non-volatile substance and has almost no odor, so it is not subject to regulations, and since it does not have a flash point, it is not subject to regulations under the Fire Service Act. It is a one-component solubilization system that completely solves the problems A and B mentioned above without causing any damage. Next, the composition will be explained. As the oil-soluble dye, all the oil-soluble dyes used in the conventional penetrating liquid and the oil-soluble dyes mentioned above can be used. For example, Sudan Red-7B (product name: manufactured by BASF) and Oil Red, which have traditionally been considered the best oil-soluble dyes for use in penetrants.
Red oil-soluble dyes such as RR (product name: Orient Chemical Co., Ltd.), flobenol yellow 618 (product name:
Of course, fluorescent dyes such as Day Glo Co., Ltd.) and White Fluoro B (trade name: Sumitomo Chemical Co., Ltd.) can be used. Additionally, it is used for paints.
Lurafics Red−430 (product name: manufactured by BASF),
Red oil-soluble dyes such as Lurafics Rubine B (trade name: manufactured by BASF) can also be used. The blending ratio is 0.5 to 3 parts, preferably 1 to 3 parts. If it is less than 0.5 part, practical flaw detection sensitivity cannot be obtained. Further, even if 3 parts or more is used, no significant improvement in flaw detection sensitivity is observed. As the nonionic surfactant, those used in the above-mentioned conventional penetrating liquid and the like can be used. Examples include the following various surfactants.

[Table] It goes without saying that nonionic surfactants other than those in the above table can be used as long as they have the same chemical structure and HLB value as the various surfactants shown in the above table. In addition, in order to maintain the solubilization system of the improved penetrant itself over a wide temperature range, nonionic surfactants must be used.
Preferably HLB in the range of 9 to 12, 20° to 50°C
The solubilized system can be maintained in a temperature range of about 40°C (in general, penetrant testing is carried out in an atmosphere below about 40°C). The blending ratio is 5 to 25 parts, preferably 10 to 20 parts. If the amount is less than 5 parts, the improved permeate itself cannot be maintained as a solubilized system. Also, if the amount is more than 25 parts, the viscosity will increase, the permeability will decrease, and the flaw detection sensitivity will deteriorate (normally, the suitable viscosity of the penetrant is 37.8℃ (100〓)).
10 centistokes or less, preferably 5 centistokes or less. In the improved penetrant, when the amount of surfactant is 25 parts or less, the viscosity of the liquid itself does not exceed 5 centistokes. Next, as the water-soluble glycol ether or its ester having a boiling point of 200°C or higher, for example, the following can be used.

【table】

[Table] Yes.
The mixing ratio is 10 to 60 parts, preferably 20 to 40 parts. If the amount is less than 10 parts, the improved penetrant itself cannot be maintained as a solubilized system. The upper limit is determined in relation to the flash point, and can be up to about 55 parts if the amounts of other ingredients are taken into consideration. As the aromatic carboxylic acid ester, for example, the following can be used. Benzoic acid esters such as methyl benzoate, ethyl benzoate, butyl benzoate, benzyl benzoate, diethylene glycol benzoate, and dipropylene glycol benzoate. Salicylic acid esters such as methyl salicylate, ethyl salicylate, butyl salicylate, and benzyl salicylate. Phthalate esters such as dimethyl phthalate, diethyl phthalate, and dibutyl phthalate. The blending ratio is 5 to 10 parts. If it is less than 5 parts, it will not function sufficiently as a solubilizing agent for oil-soluble dyes, which will be described later. Furthermore, if 10 parts or more is added, the aromatic dicarboxylic acid ester itself cannot be solubilized. Next, aliphatic hydrocarbons with a boiling point center of 200°C or higher and a surface tension of 28 dyne/cm or less (note that aliphatic hydrocarbons, which are petroleum distillates, have a range of boiling points, so
It was decided to specify the central value of the boiling point, and it was indicated as "the central boiling point is 200℃ or higher." ), for example, the following can be used:

[Table] Of course, even if it is not in the above table, the boiling point center is
It can be used as long as it has a surface tension of 28 dyne/cm or less at a temperature of 200°C or higher. The blending ratio is 1 to 5 parts. If it is less than 1 part, the surface tension lowering ability described below will not be sufficiently exhibited. Moreover, when 5 parts or more is blended, the aliphatic hydrocarbon itself cannot be solubilized. Finally, tap water may be used as the water, but when used for nuclear equipment, follow the usual method.
Use ion exchange water or distilled water. The blending ratio is the remainder of the other components used in the blending ratio described above. When all other ingredients are combined in minimum amounts
78.5 parts of water will be used. Now, in the improved penetrating liquid having the above-mentioned composition, each component other than water, which is blended in 5 parts or more in the blending ratio, has a boiling point or center of boiling point of 200°C or higher, so the evaporation rate is extremely slow, making it difficult to handle. can be treated as substantially non-volatile and is not subject to organic rules. Incidentally, the evaporation rate of water-soluble glycol ether or its ester with a boiling point of 200℃ or higher is extremely slow, less than 1 when expressed as butyl acetate < 100, and when expressed in terms of vapor pressure, it is 0.1mmHgat20.
℃ is less than that (0.1mmHg compared to 760mmHg)
0.1/760×100=0.13%, and only 0.13% of volatile vapor is generated at 200℃. ). In addition, although the improved penetrant containing the above-mentioned composition contains a substance with a flash point, due to the presence of water, the improved penetrant itself does not have a flash point, so it is regulated by the Fire Service Act. I don't even receive it. That is, a water-soluble glycol ether or its ester having a boiling point of 200° C. or higher has no flash point when it coexists with about 20 parts or more of water. still,
As mentioned above, if all other ingredients other than water are used in the minimum amount within the mixing ratio range, 78.5 parts of water will be used, and no flash point problem will occur. If the ingredients vary within the blending ratio, approximately
Care must be taken to ensure that at least 20 parts of water is present. Aromatic carboxylic acid ester and boiling point center is 200
C or higher, aliphatic hydrocarbons have no flash point when they coexist with water as a solubilized system. Next, it is confirmed that the improved penetrating liquid having the above composition contains an aromatic carboxylic acid ester and an aliphatic hydrocarbon having a boiling point center of 200°C or higher and a surface tension of 28 dyne/cm or less. This is a major feature. The former is mainly used to solve problem A, and the latter is mainly used to solve problem B. First, the former aromatic carboxylic acid ester will be explained. Aromatic carboxylic acid esters usually have a boiling point of 200℃
These are the non-volatile esters that are generally called plasticizers. Due to its chemical structure, aromatic carboxylic acid esters have a carboxyl group, which is a polar group (aqueous), within the molecule that shows oiliness as a whole, and has a balance of large oiliness and a little waterness. It is something that Therefore, it exhibits intermediate properties between "oil-soluble dye" and "nonionic surfactant - water-soluble glycol ether or its ester - water", and since it has an aromatic ring in the molecule, it is aromatic. It is a substance that shows affinity with oil-soluble dyes that have group rings,
These properties interact in a complex manner, and in the system of "nonionic surfactant - water-soluble glycol ether or its ester - water", it acts as an extremely effective solubilizing agent for "oil-soluble dye". be. This fact was discovered for the first time by the present inventor, and incidentally, aromatic hydrocarbons that do not have any polar groups, such as alkylbenzenes, alkylnaphthalenes, bisphenols, and diphenyls, can be used as "oil-soluble dyes." Although it dissolves, it is too oily and cannot be dissolved in the system of "nonionic surfactant - water-soluble glycol ether or its ester - water", and even esters with carboxyl groups are not compatible with aliphatic carboxylic acid esters, such as maleic esters. , sebacic acid esters, adipic acid esters, oleic acid esters, etc., can hardly dissolve "oil-soluble dyes," and even though they have the same aromatic carboxylic acid in their molecules, their alkali salts, such as benzoic acid Acid alkali salts, salicylic acid alkali salts, etc. have too strong polarity due to the carboxyl group and alkali (indicating water solubility). Or, it cannot mediate the dissolution of the "oil-soluble dye" in the system of "nonionic anionic surfactant - water-soluble glycol ether or its ester - water". In order to exert the effect as a solubilizing agent as described above, it is necessary to mix 5 parts or more, and in this case, the oil-soluble dye is completely dissolved at a high concentration of 0.5 to 3 parts. be able to. If the amount is more than 10 parts, the improved penetrant itself cannot be maintained in a solubilized system. Next, when the boiling point center of the latter is above 200℃, 28dyne/
Describe aliphatic hydrocarbons with a surface tension of less than cm. Now, regarding the relationship between the wettability of the penetrating liquid and the surface tension value of the penetrating liquid, those skilled in the art use the surface tension value as a measure of the wettability of the penetrating liquid. Of course, it is generally accepted that the wettability of a liquid is best expressed by its "contact angle," but the measured value of the contact angle is greatly influenced by the type of object and surface condition. Although it is suitable for measuring the wettability (easiness of getting wet) of an object, it is not necessarily optimal for measuring the wettability of the wetting liquid itself, and the measurement method is complicated. The surface tension value is used as a guideline for the wettability of the penetrating liquid itself, and empirically, when the surface tension value of the penetrating liquid is 32 dyne/cm or more, the penetrating liquid attached to the surface of the test object is "Liquid gathers in the center in a heaped state."
Similarly, in the case of 32 to 30 dyne/cm, it is said to be "slightly approaching," in the case of 30 to 28 dyne/cm, it is said to be "spreading a little," and in the case of 28 dyne or less, it is said to be "spreading rapidly to the surrounding area." ”. Those skilled in the art believe that a penetrating liquid with a surface tension value of 28 dyne/cm or less has sufficient wettability. Now, aliphatic hydrocarbons with a boiling point center of 200°C or higher and 28 dyne/cm or less are unique in the "oil-soluble dye - nonionic surfactant - water-soluble glycol ether or its ester - aromatic carboxylic acid ester - water" system. It exhibits the effect of lowering the surface tension value. This fact was discovered for the first time by the inventor. In other words, from the blending composition of the improved penetrant, the boiling point center is
When excluding aliphatic hydrocarbons of 28 dyne/cm or less at temperatures above 200℃, the surface tension of the liquid should be 28 dyne/cm.
It is impossible to achieve the following no matter how much the blending ratio is changed within the range of the blending composition ratio. For example, the minimum amount of oil-soluble dye is 0.5 parts, the maximum amount of nonionic surfactant is 25 parts, the minimum amount of water-soluble glycol ether or its ester with a boiling point of 200℃ or higher is 10 parts, and the minimum amount of aromatic carboxylic acid ester. When 5 parts of the amount are used and the remaining part (59.5 parts) is water, the surface tension value of the liquid is approximately 32 dyne/cm.
However, if one part of the above aliphatic hydrocarbon is blended into this liquid, the surface tension of the liquid will be approximately
It drops to 28dyne/cm. However,
For example, the minimum amount of oil-soluble dye is 0.5 parts, the maximum amount of nonionic surfactant is 25 parts, the minimum amount of water-soluble glycol ether or its ester with a boiling point of 200°C or higher is 10 parts, and the remainder (64.5 parts) is water. The surface tension value of the liquid when formulated is approximately 31 dyne/cm,
Even if one part of the above-mentioned aliphatic hydrocarbon is added to this liquid, the surface tension of the liquid is only reduced to about 30 dyne/cm. In the improved permeate, aliphatic hydrocarbons with a boiling point center of 200°C or higher and 28 dyne/cm or lower are estimated to combine with aromatic carboxylic acid esters to maximize surface tension lowering ability. In order to make the surface tension value of the improved penetrant liquid 28 dyne/cm or less, at least one part of it must be added.
If the amount is more than 5 parts, the improved penetrant itself cannot be maintained in a solubilized system. By adding 5 parts, the surface tension value of the improved penetrant can be set to 26 dyne/cm. As mentioned above, the improved penetrating liquid is one in which the above-mentioned A and B have been solved, has a sufficient amount of oil-soluble dye dissolved in it, has sufficient wettability, and does not contain water-soluble or alcohol-soluble dye. Not only is there no inconvenience when using it, but it also has excellent flaw detection ability. Furthermore, within the range of the above-mentioned blending ratio, the solubilized one-component type has an appropriate viscosity. If necessary, commercially available water-soluble rust preventives such as sodium nitrite, triethanolamine, etc. can be added, and up to 2 parts will not cause any adverse effects. The improved penetrant is extremely easy to produce, and the desired product can be obtained by mixing and stirring predetermined amounts of each component. Although the order of addition is not specified, it is preferable to mix each component other than water in advance, add water while stirring, and further stir thoroughly. The improved penetrant as described above can be used in exactly the same way as the conventional penetrant, as seen in Example 1 below. That is, the penetrant flaw detection method consisting of the four operations (1) to (4) described above may be carried out using the improved penetrant liquid. The improved penetrating liquid is a one-component solubilized type,
As mentioned above, in the normal temperature atmosphere in which penetrant testing is performed, the solubilized system is maintained and does not separate. However, under special conditions in which the temperature atmosphere is as high as 50℃ or higher (for example, when the object to be inspected has not been cooled to room temperature after heat treatment), nonionic The improved penetrating solution in which the surfactant does not lose its surfactant ability may separate into two layers, making it impossible to maintain a one-component solubilized system. This is a phenomenon known as the so-called "cloud point phenomenon." The present inventor has obtained the knowledge that when an anionic surfactant is blended into the improved penetrating liquid, it is possible to prevent the cloud point phenomenon from occurring not only in an atmosphere at a temperature of 50°C or higher but also at 100°C. . In other words, although anionic surfactants have almost no effect on solubilizing oil-soluble components in water, they have the distinct effect of suppressing the cloud point phenomenon when incorporated into the improved penetrant. They discovered that it has the desired effect. Although the theoretical elucidation of the above-mentioned effects of anionic surfactants has not yet been fully elucidated, when added to the improved penetrating liquid, the highly water-based anionic surfactants react with the nonionic surfactants and water at high temperatures. It is thought that it acts as a mediator for compatibility over time. As the anionic surfactant, for example, higher fatty acid alkali salts, alkyl phosphate ester alkali salts, alkylbenzenesulfonic acid alkali salts, alkyl sulfonic acid alkali salts, alkyl sulfate ester alkali salts, etc. can be used. The commercially available product is NIKKOR SLP-N (product name: Nikko Chemical).
Co., Ltd.) etc. are suitable. The blending ratio of the anionic surfactant is 0.5 to 4 parts. If less than 0.5 part is added, the above effect will not be fully exhibited. Moreover, since the cloud point phenomenon at 100° C. can be completely suppressed by adding 4 parts, it is meaningless to add more than this. It should be noted that the addition of up to 4 parts of anionic surfactant does not have any adverse effect on the improved permeate. Furthermore, the present inventor has discovered that a liquid formulated by removing only oil-soluble dyes from the formulation of the improved penetrating liquid has extremely excellent cleaning power, and can easily clean not only oil stains but also Lutzker paint, Magic ink, etc. I learned that it can be removed. If this liquid is used for pre-cleaning in the penetrant operation described in (1) above when performing penetrant testing, or as the "cleaning liquid" in the cleaning operation described in (2) above, it will comply with regulations and the Fire Service Act. Each operation can be carried out safely without any regulations, and extremely sensitive flaw detection results can be obtained. That is, a liquid having a formulation obtained by removing only the oil-soluble dye from the composition of the improved penetrating liquid (hereinafter referred to as improved cleaning liquid) is as follows. 5 to 25 parts of nonionic surfactant, water-soluble glycol ether or its ester with a boiling point of 200°C or higher
10 to 55 parts, aromatic carboxylic acid ester 5 to 10 parts,
This is an improved cleaning liquid with a surface tension of 26 to 28 dyne/cm, consisting of 1 to 5 parts of an aliphatic hydrocarbon with a boiling point center of 200°C or higher and a surface tension of 28 dyne/cm or less, and the remainder water. The composition of the improved cleaning solution is the same as described above for the improved penetrant, except that it does not contain an oil-soluble dye. The improved cleaning liquid has extremely excellent cleaning power due to its composition and low surface tension, and if used for pre-cleaning in the infiltration operation described in (1) above, it will be used for pre-cleaning. It exhibits cleaning power comparable to organic solvent type cleaning liquids such as industrial gasoline, mineral turpentine, xylol, 1-1-1 trichloroethane, perchlorethylene, acetone, etc., and removes oil stains etc. on the inspected object. Can be removed by washing. Furthermore, when used as a "cleaning liquid" in the cleaning operation (2) above, most of the conventional penetrating liquid can be washed away. What should be noted is that when used in combination with an improved penetrant, suitably highly sensitive flaw detection results can be obtained, as seen in the Examples below. In other words, the above-mentioned organic solvent type cleaning liquids are generally highly volatile, excluding special cases with low volatility such as mineral turpentine, and do not remain on the surface of the inspected object after pre-cleaning, and do not penetrate. It does not inhibit the agent from penetrating into the opening defect. However, in order to avoid being subject to organic regulations and fire service regulations, it is necessary to use water or a water-based cleaning solution instead of an organic solvent type cleaning solution. When it is necessary to pre-clean the surface of the test object, it is almost always the case that the surface of the test object is contaminated with oil, and in such cases it is difficult to remove it with water, so water-based cleaning solutions are not recommended is used. Currently, the formulation of water-based cleaning agents that are effective for pre-cleaning oil stains, etc. is 0.1 to 10 parts of surfactant, 10 to 30 parts of alcohol, and the balance water, and its viscosity is 1 to 2 centistokes. /
It is about 100F°. When performing pre-cleaning using such a water-based cleaning solution, it is almost inevitable that the water-based cleaning solution will enter the open defect area on the surface of the object to be inspected because it is weaker than the organic solvent type cleaning solution listed above. It will remain. When applying the improved penetrant to a test object in such a state, the water-based cleaning solution and the improved penetrant have different components and viscosities, so it is difficult to mix, dissolve, and diffuse between the two solutions. , replacement does not occur smoothly, and the improved penetrant solution dissolves into the water-based cleaning solution in the open defect area, resulting in a diluted state. For this reason, the performance of the improved penetrating liquid is not fully exhibited, and the defect indicating pattern during the inspection described in (4) above may become pale and blurred. However, when the improved cleaning solution is pre-cleaned in the infiltration operation described in (1) above, a cleaning solution having the same liquid composition as the infiltration solution remains in the defect. In this case, it comes into contact with the penetrating liquid in the subsequent penetrating step, but
Because they have the same viscosity and the same liquid composition, the liquids can be mixed, dissolved, diffused, and replaced smoothly, unlike when using conventional water-based cleaning liquids, which contain a lot of water and have a significantly different composition from the penetrating liquid. This allows for a substantially undiluted modified penetrant to exist within the open defect, resulting in a clear defect indicator pattern. In addition, when using the improved cleaning solution as the "cleaning solution" in the cleaning operation described in (2) above, since the solutions have good compatibility with each other, excess improved penetrating solution on the surface of the object to be inspected is easily removed, and as a result, the background It is possible to detect a clear defect indication pattern without any defects. Even when the improved penetrant and improved cleaning solution are used in combination, the operation is exactly the same as when using the conventional penetrant and cleaning solution, and as seen in Example 2 below, the above-mentioned (1) to All you have to do is perform the four operations in (4).
In this case, all operations can be performed without being subject to regulations of organic regulations or fire service laws. Next, the present invention will be explained in more detail with reference to Examples. Example 1 Preparation of improved penetrant solution Sudan Red-7B (manufactured by BASF: CI Name.
Solaent Red-19) 1 part ethyl carbitol (Daphanol DE: manufactured by Dow Chemical Company) 20 parts Nitsukol BO-7 (manufactured by Nikko Chemicals Company: oleyl alcohol ethoxylate) 10 parts benzyl benzoate 5 parts sodium oleate 2 1 part Isopar M (manufactured by Etsuo Kagaku Co., Ltd.) 2 parts Water 60 parts The above ingredients were mixed and thoroughly stirred to obtain an improved penetrating liquid consisting of a red transparent liquid. The properties of the improved infiltrate thus obtained were as follows.

[Table] Penetrant Flaw Detection Method The above-mentioned improved penetrant solution was applied with a brush to a weld line burn crack test piece with a clean surface and left for 10 minutes. Next, excess penetrating liquid on the surface of the test piece was wiped off with a rag soaked in water. Excess penetrating liquid could be removed by wiping once. Next, a thin layer of inorganic white fine powder was applied to the surface of the test piece.
Manufactured by Tokushu Toyo Co., Ltd.: Aerosol type whose main ingredient is fine silicic acid powder. ). Next, after 5 minutes, the surface of the test piece was observed under white light, and there was almost no background.
Furthermore, a defect display blot pattern that clearly indicates even the smallest defects was clearly observed. For comparison, a commercially available oil-based penetrating liquid (``Dyeing Penetrating Liquid UP-St'', manufactured by Tokushu Toyo Co., Ltd.), a commercially available solvent-type cleaning liquid (``Cleaning Liquid UR-St'', manufactured by Tokushu Toyo Co., Ltd.), and Commercially available “Quick-drying developer UD-St”: Manufactured by Tokushu Toyo Co., Ltd.
When we compared the results of penetrant testing using the same procedure as above, we confirmed that the level of background and the level of removability with water were almost the same. Furthermore, it was confirmed that the defect detection ability was also at the same level. Example 2 Preparation of improved cleaning solution Ethyl carbitol 20 parts Nitskol BO-7 10 parts Benzyl benzoate 5 parts Sodium oleate 2 parts Isopar M 2 parts Water 61 parts The above ingredients were mixed and stirred thoroughly to make it colorless and transparent. An improved cleaning solution consisting of a liquid is obtained. The properties of the improved cleaning liquid thus obtained are as follows.

[Table] Using the improved penetrant liquid of Example 1 and the above-mentioned improved cleaning liquid, penetrant testing was carried out as follows. A very thin layer of machine oil 46 was applied to the surface of the weld line quench crack test piece, and after 5 minutes it was wiped off with a rag soaked in the above cleaning solution. The wiping property was good, and one wiping was sufficient. Thereafter, the penetrating solution was applied by brushing and left for 10 minutes. Next, the excess penetrating liquid on the surface of the test piece was wiped off with a rag soaked in the above-mentioned cleaning liquid. Excess penetrating liquid could be removed by wiping once. Next, a thin layer of inorganic white fine powder was applied to the surface of the test piece using a commercially available quick-drying developer UD-T (manufactured by Tokushu Toyo Co., Ltd.).
It was formed using an aerosol-type product whose main component is fine silicic acid powder. Next, after 5 minutes, the surface of the test piece was observed under white light, and a defect-indicating bleed pattern clearly indicating even the smallest defects was clearly observed. For comparison, a commercially available oil-based penetrating solution (“Dyeing Penetrating Solution”)
UP-T”: manufactured by Tokushu Toyo Co., Ltd.) and a commercially available organic solvent type cleaning liquid (“Cleaning liquid UR-T”: manufactured by Tokushu Toyo Co., Ltd.)
and commercially available “quick-drying developer UD-T”: special paint
When compared with the case where the above-mentioned penetrant flaw detection was carried out in combination with the above-mentioned penetrant flaw detection (manufactured by Co., Ltd., aerosol type), in the case of the present invention, there was no influence of contamination due to machine oil.
It was confirmed that even the smallest defects were detected and the results were equivalent to those using conventional products. Example 3 Preparation of improved penetrant Ruragics Rubine B (manufactured by BASF) 1.5 parts Diethyl carbitol 40 parts Adekanol LO-3 (primary linear alcohol ethoxylate manufactured by Asahi Denka Kogyo Co., Ltd.) 20 parts salicylic acid Benzyl 5 parts TSN-2 (cycloparaffin manufactured by Tsurusaki Yuka Co., Ltd.)
5 parts triethanolamine 1 part water 27.5 parts The above ingredients are mixed and thoroughly stirred to obtain an improved penetrating liquid consisting of a red transparent liquid. Preparation of improved cleaning solution Diethyl carbitol 40 parts Adekanol LO-3 20 parts Benzyl salicylate 5 parts TSN-2 5 parts Triethanolamine 1 part Water 29 parts The above components were mixed and thoroughly stirred to form an improved colorless and transparent liquid. Obtain the cleaning solution. The properties of the improved penetrating liquid and improved cleaning liquid thus obtained were as follows.

[Table] Penetrant testing method Grooves on the surface of a clean "JIS-Z-2343 Type A comparison test piece (2024S-Al alloy quench crack test piece with a groove for comparison test in the center)" The left half of the border contains the above penetrating solution, and the right half contains a commercially available non-volatile penetrating solution ("Dyeing Penetrant P") for comparison.
-LT-1: Tokushu Paint Co., Ltd.) was applied by brushing and left for 15 minutes. Next, remove the excess penetrating liquid from the surface of the test piece using a cloth soaked in the above cleaning liquid on the left side, and use a commercially available water/alcohol-based cleaning liquid ("Cleaning Liquid R-LT": Tokushu Toyo Co., Ltd.) on the right side. Each was wiped off with a rag containing 100% chlorine. The ease of wiping off was almost the same for both. Next, a thin layer of inorganic white fine powder was applied to the surface of the test piece using a commercially available "nonflammable quick-drying developer UD-NU".
(manufactured by Tokushu Paint Co., Ltd.). Next, when the surface of the test piece was observed under white light after 5 minutes, it was clearly observed that the left half of the test piece had a defect display blot pattern that more clearly indicates even the smallest defects than the right half. It was done. In addition, in order to investigate the pre-cleaning power of the above cleaning solution,
Prepare 3 SUS39 grade stainless steel mirror plates,
Each surface was coated with Magic Ink Black, Magic Ink Red, and Lacquer Paint White, and left to air dry for 1 hour. Then, for the left side, use a rag soaked in the above cleaning solution, and for the right side, use a rag soaked in a commercially available water/alcohol-based cleaning solution ("Washing Liquid R-LT": manufactured by Tokushu Toyoku Co., Ltd.). I wiped each one off. As a result, on the left side, Magic Black, Magic Red, and Lutzker Paint White were all removed smoothly after wiping once or twice, while on the right side, even after repeated wiping several times, None of Zumagic Black, Magic Red, and Lutzker Paint White were removed at all. Example 4 Preparation of improved penetrant fluid Flobenol Yellow 618 (manufactured by Daye Glo: CI
Name.Fluorescent Brightening Agent 75)
0.7 parts White Fluoro B (CI manufactured by Sumitomo Chemical Industries)
Name.Fluorescent Brightening Agenh63)
1 part butyl triglycol (manufactured by Nippon Nyukazai: triethylene glycol monobutyl ether) 30 parts NITSUKOL HCO-20 (hardened castor oil ethoxylate, manufactured by Nikko Chemicals) 15 parts NITSUKOL SLP-N (sodium lauryl phosphate,
Nikko Chemicals Co., Ltd.) 4 parts DMP (dimethyl phthalate, Daihachi Chemical Co., Ltd.)
10 parts Exor D-80 (manufactured by Etsuo Chemical Co., Ltd.: normal paraffin/cycloparaffin mixture) 5 parts sodium nitrite 0.3 parts water 34 parts The above ingredients were mixed and stirred thoroughly to form a yellow transparent liquid. Obtain improved penetrating solution Preparation of improved cleaning solution Butyl triglycol 30 parts Nitsukol HCO-20 15 parts Nitsukol SLP-N 4 parts DMP 10 parts Exol D-80 5 parts Sodium nitrite 0.3 parts Water 35.7 parts Mix the above ingredients, Stir thoroughly to obtain an improved cleaning solution consisting of a colorless and transparent liquid. The properties of the improved penetrating liquid and improved cleaning liquid were as follows.

[Table] Ultrasonic cleaning using acetone as pre-cleaning
"JISZ-2343B type comparative test piece (Ni-Cr plating bending crack test piece, depth 50μ,
Place the two pieces (with an opening defect of 5μ in width) and the iron block for the stand in a dryer set at 60°C for 1 hour and check the surface temperature, then take them out and remove the iron block for the stand (the temperature will drop quickly with only the B-type test piece). A type B test piece was placed on top of the test piece (used to prevent this from occurring), and one piece was treated with the above penetrant solution, and the surface of the other piece was treated with a commercially available non-volatile high-sensitivity penetrant solution for comparison. Liquid (“Fluorescent Penetrant Liquid OD-2800I”: Special Paint Co., Ltd.)
Co., Ltd.) was applied by brushing and left for 15 minutes. The improved penetrant solution applied uniformly and no change was observed in the penetrant solution. Next, both test pieces were wiped with a cloth soaked in the above-mentioned improved cleaning solution. Wiping was confirmed under an ultraviolet light. The ease of wiping off was almost the same for both. Next, the test piece was used as a commercially available dry developer DN-600P-1 (made by Tokushu Toyo Co., Ltd.), which is an inorganic white fine powder.
The specimen was immersed in a powder whose main component is fine silicic acid powder for 5 minutes and then pulled out. Next, when the surface of the test piece was observed under an ultraviolet lamp, it was found that the test piece using the improved penetrating liquid had clearer indications than the test piece using "OD2800I". As a result, it was confirmed that the improved penetrating liquid and cleaning liquid can also be used for hot materials.

Claims (1)

[Claims] 1. Oil-soluble dye 0.5 to 3 parts (meaning parts by weight).
same as below. ), 5 to 25 parts of nonionic surfactant,
10 to 55 parts of water-soluble glycol ether or its ester with a boiling point of 200°C or higher, 5 to 10 parts of aromatic carboxylic acid ester, 28 dyne/cm with a boiling point center of 200°C or higher
1 to 5 parts of an aliphatic hydrocarbon having a surface tension of:
A penetrant liquid for penetrant testing that consists of water and has a surface tension of 26 to 28 dyne/cm. 2 0.5 to 3 parts of oil-soluble dye, 5 to 25 parts of nonionic surfactant, 10 to 55 parts of water-soluble glycol ether or its ester with a boiling point of 200°C or higher, 5 to 10 parts of aromatic carboxylic acid ester, boiling point center of 200°C 1 to 5 parts of an aliphatic hydrocarbon having a surface tension of 28 dyne/cm or less at temperatures above ℃, 0.5 to 4 parts of an anionic surfactant,
A penetrant liquid for penetrant testing that consists of water and has a surface tension of 26 to 28 dyne/cm. 3. After applying a penetrant liquid for penetrant testing to the surface of the object to be inspected and letting the penetrant liquid penetrate into the opening defect, remove excess penetrant liquid that remains on the surface of the object without penetrating into the opening defect. Then, by forming a thin layer of inorganic white fine powder on the surface of the object to be inspected, and sucking out the penetrating liquid that has penetrated into the opening defect due to capillary action between the powders to the surface of the thin layer. In the penetrant testing method, in which a defect-indicating bleeding pattern appears and the defect is detected using the pattern, an oil-soluble dye of 0.5 to 3 is used as the penetrant liquid for penetrant testing.
parts, nonionic surfactant 5 to 25 parts, boiling point 200℃
10 to 55 parts of the above water-soluble glycol ether or its ester, 5 to 10 parts of aromatic carboxylic acid ester
1 to 5 parts of aliphatic hydrocarbon having a boiling point center of 200°C or higher and a surface tension of 28 dyne/cm or less, and the balance water, and using a penetrant liquid for penetrant testing with a surface tension of 26 to 28 dyne/cm. A penetrant flaw detection method, characterized in that the excess penetrant liquid is washed and removed using a liquid having a composition obtained by removing only an oil-soluble dye from the penetrant liquid composition for penetrant flaw detection. 4 After the surface of the object to be inspected is cleaned by pre-cleaning, a penetrant liquid for penetrant testing is applied to the surface, and the penetrant liquid is allowed to penetrate into the opening defect. Excess penetrating liquid remaining on the surface of the object to be inspected is washed away, and then a thin layer of inorganic white fine powder is formed on the surface of the object to be inspected, and the penetrating liquid penetrates into the opening defect due to capillary action between the powders. In the penetrant testing method, in which a defect-indicating bleed pattern appears by sucking out a liquid onto the surface of the thin layer, and the defect is detected using the pattern, an oil-soluble dye of 0.5 to 3 is used as the penetrant liquid for penetrant testing.
parts, nonionic surfactant 5 to 25 parts, boiling point 200℃
10 to 55 parts of the above water-soluble glycol ether or its ester, 5 to 10 parts of aromatic carboxylic acid ester
1 to 5 parts of aliphatic hydrocarbon having a boiling point center of 200°C or higher and a surface tension of 28 dyne/cm or less, and the balance water, and using a penetrant liquid for penetrant testing with a surface tension of 26 to 28 dyne/cm. , characterized in that the surface of the object to be inspected is cleaned by pre-cleaning and the excess penetrant liquid is washed and removed using a liquid having a composition obtained by removing only an oil-soluble dye from the penetrant liquid composition for penetrant flaw detection. penetrant testing method.