JP5093574B2 - Penetration testing method - Google Patents

Penetration testing method Download PDF

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JP5093574B2
JP5093574B2 JP2007115869A JP2007115869A JP5093574B2 JP 5093574 B2 JP5093574 B2 JP 5093574B2 JP 2007115869 A JP2007115869 A JP 2007115869A JP 2007115869 A JP2007115869 A JP 2007115869A JP 5093574 B2 JP5093574 B2 JP 5093574B2
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寿博 津葉本
弘美 國井
嘉高 佐野
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本発明は、自動車部材などの各種部材の表面に存在する微細な開口欠陥部の探傷に適用される浸透探傷試験方法及び該浸透探傷試験方法に用いる水洗性水ベース浸透液に関するものである。 The present invention relates to a penetrant flaw detection test method applied to flaw detection of fine opening defects existing on the surface of various members such as automobile members, and a water-washable water-based penetrant used in the penetrant flaw detection test method.

周知のとおり、非破壊検査方法の一種である「JIS Z 2343-1〜4:2001」に規格化されている浸透探傷試験は、自動車部材(例えば、ピストンロッド)などの各種部材の表面に存在する微細な開口欠陥部(例えば、微細なクラックやピンホール)の探傷に汎用されており、その基本的態様は、当該JIS規格に示されているように、染色浸透液(通常、油溶性赤色染料を溶剤に溶解させた浸透性の強い液体が用いられる)又は蛍光浸透液(通常、紫外線灯:ブラックライト:照射下で黄緑色蛍光を発する油溶性蛍光染料を溶剤に溶解させた浸透性の強い液体が用いられる)を被検査物表面に付着させて開口欠陥部に浸透させた後、当該欠陥部内に浸透せずに被検査物表面に残留している余剰浸透液を除去し、次いで、染色浸透液を用いた場合には、当該被検査物表面に炭酸マグネシウム粉末や炭酸カルシウム粉末などの無機質白色粉末(当業者間では「現像剤」と呼ばれている)の薄層を形成し該薄層によって開口欠陥部内に浸透している染色浸透液を薄層表面に吸い出させることによって欠陥指示ニジミ模様を現出させ、自然光又は白色光の下で観察して当該ニジミ模様によって開口欠陥部の存在・位置を探傷し、蛍光浸透液を用いた場合には、前記現像剤を用いることなく、暗室における紫外線灯(当業者間では「ブラックライト」と呼ばれている)の照射下で当該被検査物表面を観察して黄緑色に発光している欠陥指示蛍光模様によって開口欠陥部の存在・位置を探傷するというものである(以下、この基本的態様を採る探傷試験を「周知浸透探傷試験」という)。   As is well known, the penetrant testing standardized in “JIS Z 2343-1 to 4: 2001”, which is a kind of non-destructive inspection method, exists on the surface of various members such as automobile members (for example, piston rods). It is widely used for flaw detection of fine opening defects (for example, fine cracks and pinholes), and its basic mode is dyed penetrant (usually oil-soluble red as shown in the JIS standard). A highly penetrating liquid in which a dye is dissolved in a solvent is used) or a fluorescent penetrating liquid (usually ultraviolet light: black light: penetrating oil-soluble fluorescent dye that emits yellow-green fluorescence under irradiation in a solvent) A strong liquid is used) is adhered to the surface of the object to be infiltrated and penetrates into the opening defect portion, and then the excess permeate remaining on the surface of the object to be inspected without penetrating into the defect portion is removed. When using a dye penetrant, A thin layer of inorganic white powder (called “developer” among those skilled in the art) such as magnesium carbonate powder or calcium carbonate powder is formed on the surface of the object to be inspected, and penetrates into the opening defect portion by the thin layer. The defect-indicating bleed pattern appears by sucking out the dye penetrant liquid onto the surface of the thin layer, and is observed under natural light or white light. Is used, and without using the developer, the surface of the object to be inspected becomes yellowish green under the irradiation of an ultraviolet lamp (called “black light” by those skilled in the art) in a dark room. In this method, the presence / position of the opening defect portion is detected by a defect indicating fluorescent pattern that emits light (hereinafter, the flaw detection test employing this basic mode is referred to as a “well-known penetrant flaw detection test”).

周知浸透探傷試験に用いられている染色浸透液及び蛍光浸透液(以下、両液を指称して「浸透液」ということもある)には、種々様々な処方の製品が市販・汎用されており、当業者において汎用されている市販品を油溶性赤色染料(例えば、オイルレッド5B:商品名:オリエント株式会社やSudan Red 462:商品名:BASF社)又は油溶性蛍光染料(例えば、Fluorol 7GA:商品名:GAF社:やフロレッセントブライトニスエージェント68:商品名:日本化薬株式会社)を溶解するために用いられている主溶剤によって大別すれば、水及び水と相溶する水溶性有機溶剤を主溶剤とする水ベース浸透液と可燃性の非水溶性有機溶剤(通常、高沸点有機溶剤)を主溶剤とする油ベース浸透液に分類できる。なお、油ベース浸透液には希釈溶剤(通常、揮発性低・中沸点有機溶剤)が配合されている。   A wide variety of prescription products are commercially available and widely used for dyeing and fluorescent penetrants (hereinafter sometimes referred to as “penetrant”), which are used in well-known penetrant testing. The oil-soluble red dye (for example, Oil Red 5B: trade name: Orient Co., Ltd. or Sudan Red 462: trade name: BASF) or the oil-soluble fluorescent dye (for example, Fluorol 7GA: Product name: GAF: Fluorescent bright varnish agent 68: Product name: Nippon Kayaku Co., Ltd.) It can be classified into a water-based penetrant containing an organic solvent as a main solvent and an oil-based penetrant containing a flammable water-insoluble organic solvent (usually a high-boiling organic solvent) as a main solvent. The oil-based penetrant contains a diluent solvent (usually a volatile low / medium boiling organic solvent).

そして、当業者間では、周知浸透探傷試験における余剰浸透液の除去に当たり、水ベース浸透液を用いた場合には水洗によって除去するので、水ベース浸透液は「水洗性水ベース浸透液」と呼ばれており、油ベース浸透液を用いた場合には、油ベース浸透液がその処方中に界面活性剤を含んでいないものであるときは有機溶剤を染み込ませたウエスなどで拭き取って除去しているので、この油ベース浸透液は「溶剤除去性油ベース浸透液」と呼ばれており、また、油ベース浸透液がその処方中に界面活性剤(通常、ノニオン系界面活性剤)を含んでいるものであるときには水洗によって除去するので、この油ベース浸透液は「水洗性油ベース浸透液」と呼ばれている。   And, among those skilled in the art, when removing a surplus permeate in a well-known permeation test, if a water-based permeate is used, the water-based permeate is removed by washing with water. If an oil-based penetrant does not contain a surfactant in the formulation, wipe it off with a cloth soaked with an organic solvent and remove it. Therefore, this oil-based permeate is called “solvent-removable oil-based permeate”, and the oil-based permeate contains a surfactant (usually a nonionic surfactant) in its formulation. This oil base permeate is called “water washable oil base permeate” because it is removed by washing with water.

水洗性水ベース浸透液の代表的な市販品には、スーパーチェックP-LK(商品名:水及び水と相溶する水溶性有機溶剤を主溶剤とし、油溶性赤色染料、界面活性剤などが配合されている液体:マークテック株式会社)やスーパーグローOD-18S(商品名:水及び水と相溶する水溶性有機溶剤を主溶剤とし、油溶性蛍光染料、界面活性剤などが配合されている液体:マークテック株式会社)が挙げられ、溶剤除去性油ベース浸透液の代表的な市販品には、スーパーチェックUP-ST(商品名:可燃性の非水溶性有機溶剤を主溶剤とし、油溶性赤色染料、希釈溶剤などが配合されている液体:マークテック株式会社)が挙げられ、水洗性油ベース浸透液の代表的な市販品には、スーパーチェックUP-G3(商品名:可燃性の非水溶性有機溶剤を主溶剤とし、油溶性赤色染料、界面活性剤、希釈溶剤などが配合されている液体:マークテック株式会社)やエコグローEG-2000(商品名:可燃性の非水溶性有機溶剤を主溶剤とし、油溶性蛍光染料、界面活性剤、希釈溶剤などが配合されている液体:マークテック株式会社)が挙げられる。   Representative commercial products for water-based water-based penetrants include Super Check P-LK (trade name: water and water-soluble organic solvents that are compatible with water, oil-soluble red dyes, surfactants, etc. Formulated liquid: Marktech Co., Ltd. and Super Glow OD-18S (Product name: Water and water-soluble organic solvents compatible with water are used as the main solvent, and oil-soluble fluorescent dyes, surfactants, etc. are included. Liquid: Marktech Co., Ltd.), and typical commercial products of solvent-removable oil-based penetrants include Super Check UP-ST (trade name: flammable water-insoluble organic solvent as the main solvent, Liquids containing oil-soluble red dyes, dilution solvents, etc .: Mark Tech Co., Ltd. are listed, and typical commercial products for washable oil-based penetrants include Super Check UP-G3 (trade name: flammable) Oil-soluble Liquids containing color dyes, surfactants, diluting solvents, etc .: Mark Tech Co., Ltd. and Eco Glow EG-2000 (trade name: Combustible water-insoluble organic solvents as main solvents, oil-soluble fluorescent dyes, interfaces A liquid in which an activator, a diluting solvent and the like are blended: Marktec Corporation).

なお、前記各技術的手段以外にも、可燃性の非水溶性有機溶剤(水に対して相溶性を有さない有機溶剤)に油溶性赤色染料又は油溶性蛍光染料を溶解してなり、界面活性剤を含まない油ベース浸透液を用い、周知浸透探傷試験における余剰浸透液の除去に当たり、水を高水圧にて被検査物表面に吹き付けて除去するという技術的手段が実用されており(特許文献1参照)、また、油溶性赤色染料又は油溶性蛍光染料5〜10重量%と該染料を溶解する沸点190℃以上の高沸点有機溶剤からなる主溶剤と該主溶剤と相溶する沸点110℃以下の揮発性有機溶剤からなる希釈溶剤30〜80重量%とが配合されている浸透液を用い、周知浸透探傷試験において開口欠陥部に浸透させたとき、配合されている当該希釈溶剤の50〜80重量%が蒸発して当該浸透液を自己濃縮させて極微細な開口欠陥部を探傷するという技術的手段が提案されている(特許文献2参照)。   In addition to the above technical means, an oil-soluble red dye or an oil-soluble fluorescent dye is dissolved in a flammable water-insoluble organic solvent (an organic solvent that is not compatible with water), and an interface is formed. An oil-based penetrant that does not contain an activator is used to remove excess penetrant in well-known penetrant flaw detection tests by spraying water onto the surface of the test object at high water pressure (patented) Reference 1), a main solvent composed of 5 to 10% by weight of an oil-soluble red dye or oil-soluble fluorescent dye and a high-boiling organic solvent having a boiling point of 190 ° C. or higher that dissolves the dye, and a boiling point of 110 compatible with the main solvent. When a penetrating liquid containing 30 to 80% by weight of a diluting solvent composed of a volatile organic solvent at a temperature of 0 ° C. or lower is blended and permeated into an opening defect part in a well-known penetrant flaw detection test, 50 ~ 80% by weight of the permeate is evaporated There has been proposed a technical means for concentrating and detecting flaws in extremely fine openings (see Patent Document 2).

特開平5−72148号公報Japanese Patent Laid-Open No. 5-72148 特開平8−271448号公報JP-A-8-271448

前記水洗性水べース浸透液の処方は、主溶剤が水と水溶性有機溶剤とを引火点を有しない割合にて混合されているので、消防法の規格を満たしているため、取り扱いや貯蔵量の問題がないから、浸透液が大量使用されている自動車工場などにおいて汎用されている。   The prescription for the water-based water-based penetrant is that the main solvent is a mixture of water and a water-soluble organic solvent at a ratio that does not have a flash point. Since there is no problem with the amount of storage, it is widely used in automobile factories where large amounts of penetrants are used.

しかし、周知浸透探傷試験における余剰浸透液の除去に当たり、前記水洗性水ベース浸透液の主溶剤が水と水溶性有機溶剤であるため、水洗によって余剰浸透液だけではなく、開口欠陥部内に浸透している浸透液まで洗い流されてしまうこと(当業界では「過洗浄」と呼ばれている)があり、この場合には、探傷精度が低下し、浸透液が本来具備している性能を発揮できなくなるという問題点がある。   However, when removing the excess permeate in the well-known penetrant testing, the main solvent of the water-based water-based permeate is water and a water-soluble organic solvent. In some cases, the penetrant solution is washed away (referred to as “overwashing” in the industry). In this case, the flaw detection accuracy is reduced, and the penetrating solution originally exhibits the performance. There is a problem of disappearing.

もっとも、前記溶剤除去性油ベース浸透液や前記水洗性油ベース浸透液を用いる場合には、主溶剤が非水溶性有機溶剤であるため前記過洗浄は生じないが、いずれの油ベース浸透液もその主溶剤が可燃性の非水溶性有機溶剤であるから消防法の危険物に該当し、取り扱いや貯蔵量・貯蔵設備の安全性に関する問題点がある。   Of course, when the solvent-removable oil-based permeate or the water-washable oil-based permeate is used, the main solvent is a water-insoluble organic solvent, so the overwash does not occur. Since the main solvent is a flammable, non-water-soluble organic solvent, it falls under the category of dangerous materials under the Fire Service Act, and there are problems with handling, storage amount, and safety of storage equipment.

本発明は、前記水洗性水ベース浸透液及び該浸透液を用いる周知浸透探傷試験に内在する前記問題点に鑑み、引火点を有さず、かつ、水洗による余剰浸透液の除去に当たって、前記過洗浄の発生が可及的に抑制でき、前記水洗性油ベース浸透液の前掲市販品と同等の探傷性能を具備している浸透探傷試験用水洗性水ベース浸透液及び該浸透液を用いる浸透探傷試験方法を提供することを技術的課題とする。   In view of the problems inherent in the water-washable water-based penetrant and the known penetrant flaw detection test using the penetrant, the present invention does not have a flash point and is used to remove the excess penetrant by washing. Occurrence of cleaning can be suppressed as much as possible, and the water-cleaning water-based penetrant for penetrant testing and having the same flaw detection performance as that of the above-mentioned commercially available water-based oil-based penetrant and penetrant flaw detection using the penetrant Providing a test method is a technical issue.

本発明者は、前記技術的課題を達成するため、水洗性水ベース浸透液における油溶性赤色染料及び油溶性蛍光染料を溶解させる主溶剤とする水と各種有機溶剤との組合せについて、思考錯誤的な数多くの試作・実験を重ねた結果、油溶性赤色染料及び油溶性蛍光染料を溶解する有機溶剤と水とを該有機溶剤が該水に溶解して単一相になっている状態と該有機溶剤が該水から分離して二相になっている状態との二つの相状態間を温度変化によって可逆的に変化すると共に引火点を有さない割合にて混合して主溶剤とし、当該主溶剤に油溶性赤色染料又は油溶性蛍光染料と界面活性剤とを配合して水洗性水ベース浸透液を調製し、当該浸透液を用い、周知浸透探傷試験における余剰浸透液の除去に当たり、当該浸透液が二相に分離する温度以上の温水によって洗浄すれば、前記過洗浄の発生が可及的に抑制でき、前記水洗性油ベース浸透液の前掲市販品と同等の精度によって探傷できるという刮目すべき知見を得、前記技術的課題を達成したものである。   In order to achieve the above technical problem, the present inventor has thought and error about the combination of water and various organic solvents as the main solvent for dissolving the oil-soluble red dye and oil-soluble fluorescent dye in the water-washable water-based penetrant. As a result of many trial manufactures and experiments, the organic solvent that dissolves the oil-soluble red dye and the oil-soluble fluorescent dye and water are dissolved in the water to form a single phase and the organic solvent. The solvent is separated from the water and is in a two-phase state. The two solvents are reversibly changed by temperature change and mixed at a ratio that does not have a flash point. A water-washable water-based penetrant is prepared by blending a solvent with an oil-soluble red dye or oil-soluble fluorescent dye and a surfactant, and using the penetrant, the permeate is removed when removing the surplus penetrant in a well-known penetrant test. Above the temperature at which the liquid separates into two phases If washed with water, the occurrence of the overwash can be suppressed as much as possible, and the remarkable technical knowledge that flaw detection can be performed with the same accuracy as the above-mentioned commercial product of the washable oil-based penetrant has been obtained. Achieved.

前記技術的課題は、次のとおりの本発明によって解決できる。   The technical problem can be solved by the present invention as follows.

即ち、本発明に係る浸透探傷試験方法は、有機溶剤と水とを該有機溶剤が該水に溶解して単一相になっている状態と該有機溶剤が該水から分離して二相になっている状態との二つの相状態間を温度変化によって可逆的に変化すると共に引火点を有しない割合にて混合してなる主溶剤と該有機溶剤に溶解する油溶性赤色染料又は油溶性蛍光染料と界面活性剤とが配合されている浸透探傷試験用水洗性水ベース浸透液を、当該浸透液の相状態が前記単一相になっている状態で被検査物表面に付着させ、当該浸透液を被検査物表面の開口欠陥部に浸透させた後、当該浸透液の相状態が前記二相に変化する温度以上の温水によって当該被検査物表面を洗浄して開口欠陥部内に浸透せずに被検査物表面に残留している余剰浸透液を除去し、次いで開口欠陥部内に浸透している浸透液によって開口欠陥部の存在を探傷するものである(請求項1)。  That is, in the penetrant testing method according to the present invention, the organic solvent and water are dissolved in the water to form a single phase, and the organic solvent is separated from the water into two phases. An oil-soluble red dye or oil-soluble fluorescence that dissolves in the organic solvent and a main solvent obtained by reversibly changing between two phase states with the state of being in a reversible state with a change in temperature and having no flash point A water-based water-based penetrant for penetrant flaw detection, in which a dye and a surfactant are blended, is attached to the surface of the object to be inspected in a state where the phase of the penetrant is the single phase, and the penetrant After infiltrating the liquid into the opening defect portion of the surface of the object to be inspected, the surface of the object to be inspected is washed with warm water at a temperature equal to or higher than the temperature at which the phase state of the permeating liquid changes to the two phases and does not penetrate into the opening defect portion Remove excess permeate remaining on the surface of the test object, Is intended to flaw detection of the presence of the opening defect by permeate pervades portion (claim 1).

本発明に係る浸透探傷試験方法及び該浸透探傷試験方法に用いる水洗性水ベース浸透液によれば、当該浸透液は、有機溶剤が水に溶解して単一相になっている状態と有機溶剤が水から分離して二相になっている状態との二つの相状態間を温度変化によって可逆的に変化するという特性を備えているので、当該浸透探傷試験における余剰浸透液の除去に当たり、当該浸透液が二相に分離する温度以上の温水によって洗浄すると、開口欠陥部内に浸透している浸透液が二相に分離し、分離した上相部が少量の水を含んだ有機溶剤成分なので、温水に溶け出すことが殆どないから前記過洗浄の発生を可及的に抑制でき、かつ、分離した下相部が少量の有機溶剤成分を含んだ水なので、溶解している油溶性(赤色又は蛍光)染料成分は上相部に移行して上相部の染料濃度が高くなるから前記観察時において、鮮明な欠陥指示(ニジミ又は蛍光)模様が得られ、前記溶剤除去性油ベース浸透液の前掲市販品を用いた場合と同等の精度によって探傷できる。 According to the penetrant flaw detection test method and the water-based water-based penetrant used in the penetrant flaw detection test method according to the present invention, the permeate contains a state in which the organic solvent is dissolved in water and is in a single phase. Since it has the property of reversibly changing between the two phase states with the two phases separated from the water by the temperature change, in removing the excess permeate in the penetration test, When washing with warm water above the temperature at which the permeate separates into two phases, the permeate penetrating into the opening defect part separates into two phases, and the separated upper phase part is an organic solvent component containing a small amount of water, Since it hardly dissolves in warm water, the occurrence of the overwash can be suppressed as much as possible, and the separated lower phase part contains water containing a small amount of an organic solvent component. Fluorescent) dye component moves to the upper phase Since the dye concentration in the upper phase is increased, a clear defect indication (brightness or fluorescence) pattern is obtained at the time of observation, with the same accuracy as when using the above-mentioned commercially available solvent-removable oil-based penetrant. Can detect flaws.

しかも、本発明に係る浸透探傷試験方法に用いる水洗性水ベース浸透液は引火点を有しないので、消防法の危険物に該当しないから、取り扱いや貯蔵量・貯蔵設備の安全に関する問題が発生しない。 Moreover, since the water-based water-based penetrant used in the penetrant testing method according to the present invention does not have a flash point, it does not fall under the dangerous goods of the Fire Service Act, so there are no problems with handling, storage amount, and safety of storage facilities. .

本発明の実施の形態は次のとおりである。   The embodiment of the present invention is as follows.

実施の形態1. Embodiment 1 FIG.

本実施の形態に係る浸透探傷試験方法に用いる水洗性水ベース浸透液は、ジエチレングリコールモノエチルエーテルアセテート(以下「EDGAC」という)、プロピレングリコールモノメチルエーテルアセテート(以下「PMA」という)、ジエチレングリコールジエチルエーテル(以下「DEDG」という)及びエチレングリコールモノブチルエーテル(以下「BCL」という)から選ばれる一種又は二種以上の有機溶剤と水とを該有機溶剤が水に溶解して単一相になっている状態と該有機溶剤が該水から分離して二相になっている状態との二つの相状態間を温度変化によって可及的に変化すると共に引火点を有しない割合にて混合した主溶剤に、当該有機溶剤に溶解する油溶性赤色染料又は油溶性蛍光染料と界面活性剤とが配合されている液状物である。 The washable water-based penetrant used in the penetrant testing method according to the present embodiment includes diethylene glycol monoethyl ether acetate (hereinafter referred to as “EDGAC”), propylene glycol monomethyl ether acetate (hereinafter referred to as “PMA”), diethylene glycol diethyl ether ( A state in which one or two or more organic solvents selected from ethylene glycol monobutyl ether (hereinafter referred to as “BCL”) and water are dissolved in water to form a single phase. And the main solvent in which the organic solvent is separated from the water into a two-phase state and is mixed as much as possible with a change in temperature and does not have a flash point. An oil-soluble red dye or oil-soluble fluorescent dye that dissolves in the organic solvent and a surfactant are blended. That is a liquid material.

前記油溶性赤色染料と油溶性蛍光染料及びその配合割合は、周知浸透探傷試験用浸透液に常用されているものを適用すればよく、前者にはオイルレッド5B(商品名:オリエント株式会社)やSudan Red 462(商品名:BASF社)が、後者にはFluorol 7GA(商品名:GAF社)やフロレッセントブライトニスエージェント68(商品名:日本化薬株式会社)が好適であり、その配合割合はいずれの染料を用いる場合にも0.2〜2重量%が好適であり、1〜2重量%がより好適であり、0.2重量%未満では、前記観察時において鮮明な欠陥指示(ニジミ又は蛍光)模様を得られないので探傷精度が著しく低下し、一方、2重量%を超えても探傷精度はさほど向上しない。   The oil-soluble red dye, the oil-soluble fluorescent dye, and the blending ratio thereof may be those commonly used in known penetrant flaw detection penetrants. For the former, oil red 5B (trade name: Orient Co., Ltd.) Sudan Red 462 (trade name: BASF) is suitable, and Fluorol 7GA (trade name: GAF) and Fluorescent Bright Varnish Agent 68 (trade name: Nippon Kayaku Co., Ltd.) are suitable for the latter. In any of the dyes, 0.2 to 2% by weight is preferable, 1 to 2% by weight is more preferable, and if it is less than 0.2% by weight, a clear defect indication (brightening or fluorescent) pattern is observed during the observation. Therefore, the flaw detection accuracy is remarkably lowered. On the other hand, even if it exceeds 2% by weight, the flaw detection accuracy is not so improved.

前記界面活性剤及びその配合割合も、周知浸透探傷試験用浸透液に常用されているものを適用すればよく、ノニオン系界面活性剤、より具体的には、HLB値8〜13のポリオキシアルキレンアルキルエーテル、例えば、ノイゲンNL-Dash408(商品名:第一工業株式会社)が好適であるが、ポリオキシエチレン脂肪酸エステルなどのエステル系界面活性剤を用いて浸透液を強化することも可能であり、その配合割合はいずれの界面活性剤を用いる場合にも3〜7重量%が好適であり、3重量%未満では、充分な浸透力が得られないので探傷精度が著しく低下し、一方、7重量%を超えても探傷精度はさほど向上しない。   What is necessary is just to apply what is normally used for the penetration liquid for well-known penetrant flaw detection tests, and, as for the said surfactant and its mixture ratio, Nonionic surfactant, More specifically, the polyoxyalkylene of HLB value 8-13 Alkyl ethers such as Neugen NL-Dash408 (trade name: Daiichi Kogyo Co., Ltd.) are suitable, but it is also possible to reinforce the permeate using an ester surfactant such as polyoxyethylene fatty acid ester. The blending ratio is preferably 3 to 7% by weight when any surfactant is used, and if it is less than 3% by weight, sufficient penetrating power cannot be obtained, so that the flaw detection accuracy is remarkably lowered. Even if the weight percentage is exceeded, the flaw detection accuracy does not improve so much.

前記主溶剤における前記有機溶剤に対する水の混合割合は1:1〜1:2であり、この混合割合に範囲内であれば、前掲各油溶性赤色染料又は前掲各油溶性蛍光染料と前掲各界面活性剤とを、それぞれ所要割合量で配合・溶解させてなる浸透液が、室温(約20℃)においては前記単一相になっている状態を維持しており、当該浸透液を加温(約35℃〜60℃)すると前記二相になっている状態に変化すること及び当該浸透液が引火点を有しないことを保証できる。   The mixing ratio of water to the organic solvent in the main solvent is 1: 1 to 1: 2, and if the mixing ratio is within the range, each oil-soluble red dye described above or each oil-soluble fluorescent dye described above and each interface described above. An osmotic solution prepared by mixing and dissolving the active agent in a required proportion amount maintains the state of the single phase at room temperature (about 20 ° C.), and the osmotic solution is heated ( About 35 ° C. to 60 ° C.), it can be guaranteed that the two-phase state is changed and that the permeate has no flash point.

本実施の形態に係る浸透探傷試験方法に用いる水洗性水ベース浸透液の調製は容易であり、前記有機溶剤に対する水の混合割合を1:1〜1:2の範囲内とした主溶剤92〜96重量%、前掲各油溶性赤色染料又は前掲各油溶性蛍光染料1〜2重量%、前掲各界面活性剤3〜7重量%の各配合割合範囲内において全体量100重量%となるように各材料を秤取し、秤取した各材料をステンレス製タンクに投入し、室温(約20℃)において電動ミキサーなどを使用し、各材料が混和・溶解して単一相の状態となるまで攪拌すればよい。 Preparation of a water-washable water-based penetrant used in the penetrant testing method according to the present embodiment is easy, and the main solvent 92 to 92 has a water mixing ratio of 1: 1 to 1: 2 with respect to the organic solvent. 96% by weight, each oil-soluble red dye described above or each oil-soluble fluorescent dye 1-2% by weight, each surfactant 3 to 7% by weight within each mixing ratio range so that the total amount is 100% by weight. Weigh the materials, put each weighed material into a stainless steel tank, and use an electric mixer etc. at room temperature (about 20 ° C) and stir until each material is mixed and dissolved into a single phase. do it.

なお、前記有機溶剤に対する水の混合割合が1:1〜1:2の範囲内である限り、必要に応じて水に完全に相溶する水溶性有機溶剤(例えば、ジエチルグリコールモノブチルエーテル−以下「BDG」という−)を5〜16重量%の範囲内で添加しても本発明の効果は変わらないが、BDGを添加する場合には、その添加量に応じて前記有機溶剤の量を減らす必要がある(後出実施例4,5参照)。   As long as the mixing ratio of water to the organic solvent is in the range of 1: 1 to 1: 2, a water-soluble organic solvent (for example, diethyl glycol monobutyl ether-hereinafter “ The effect of the present invention does not change even when-"BDG" is added within the range of 5 to 16% by weight. However, when BDG is added, the amount of the organic solvent must be reduced according to the amount added. (See Examples 4 and 5 below).

実施の形態2.   Embodiment 2. FIG.

本実施の形態に係る浸透探傷試験方法は、実施の形態1に係る浸透探傷試験方法に用いる水洗性水ベース浸透液を使用するものであり、その基本的態様は周知浸透探傷試験と同様であり、先ず、室温(約20℃)の検査作業雰囲気において、同室温で貯蔵されていた実施の形態1に係る浸透探傷試験方法に用いる水洗性水ベース浸透液を被検査物表面に塗布して付着させて開口欠陥部に浸透させ(浸透処理)、次いで、当該被検査物表面を約60℃〜70℃の温水を使用し、水圧:約0.3〜0.5Mpa・流量:1〜3L/minにて当該欠陥部内に浸透せずに被検査物表面に残っている余剰浸透液を洗浄・除去する(洗浄処理)。

The penetrant testing method according to the present embodiment uses a water-washable water-based penetrant used in the penetrant flaw testing method according to the first embodiment, and the basic aspect thereof is the same as the well-known penetrant test. First, in the inspection working atmosphere at room temperature (about 20 ° C.), the water-washable water-based penetrating solution used in the penetrant testing method according to Embodiment 1 stored at the room temperature is applied to the surface of the object to be inspected. Then, it penetrates into the opening defect part (penetration treatment), and then the surface of the object to be inspected uses hot water of about 60 ° C. to 70 ° C., water pressure: about 0.3 to 0.5 MPa, flow rate: 1 to 3 L / min The excess permeate remaining on the surface of the object to be inspected without penetrating into the defective portion is washed and removed (cleaning process).

洗浄後の被検査物表面が乾燥後、当該浸透液が油溶性赤色染料を用いたものである場合には、被検査物表面に前記無機質白色粉末からなる現像剤の薄層を形成し該薄層によって開口欠陥部内に浸透している浸透液を当該薄層表面に吸い出させることによって欠陥指示赤色ニジミ模様を現出させ(現像処理)、自然光又は白色光に下で当該被検査物表面を観察して当該ニジミ模様によって開口欠陥部に存在・位置を探傷する方法である。   When the surface of the object to be inspected after drying is dried, and the permeation liquid uses an oil-soluble red dye, a thin layer of the developer composed of the inorganic white powder is formed on the surface of the object to be inspected. The permeation liquid penetrating into the opening defect portion by the layer is sucked out to the surface of the thin layer so that a defect-indicating red rainbow pattern appears (development processing), and the surface of the object to be inspected is exposed to natural light or white light. This is a method of observing and detecting the presence / position of the opening defect portion by the bleed pattern.

また、当該浸透液が油溶性蛍光染料を用いたものである場合には、前記現像処理を行うことなく、洗浄後の被検査物が乾燥後、暗室における紫外線灯の照射下で当該被検査物表面を観察して黄緑色に発光している欠陥指示蛍光模様によって開口欠陥部の存在・位置を探傷する方法である。   In addition, when the penetrating liquid uses an oil-soluble fluorescent dye, the object to be inspected after drying is dried and then subjected to ultraviolet light irradiation in a dark room without performing the development processing. This is a method in which the presence / position of an opening defect portion is detected by a defect indicating fluorescent pattern that emits yellowish green light by observing the surface.

本実施の形態では、前記洗浄処理において、前記温水が前記水圧・流量をもって被検査物表面に吹き付けられると、洗浄開始当初は被検査物表面に接触した温水が該被検査物の温度(通常、被検査物は鋼鉄などの金属製部材であるため、その温度は室温:約20℃:よりも遙かに低い)まで冷やされ、冷やされた水とその水圧によって当該被検査物表面に残留している余剰浸透液が除去され始め、洗浄が進むにつれて当該被検査物表面の温度は吹き付けられている温水によって上昇して温水の温度に近づき、開口欠陥部内に浸透している浸透液が二相に分離し、分離した上相部は少量の水を含んだ有機溶剤成分であるため、吹き付けられた温水に溶け出すことが殆ど無いから、前記過洗浄の発生が可及的に抑制されており、かつ、分離した下相部は少量の有機溶剤成分を含んだ水であるため、浸透液に溶解している油溶性(赤色又は蛍光)染料成分が上相部に移行して上相部に染料濃度が高くなっているため、油溶性赤色染料を用いた浸透液の場合には前記現像剤薄層表面に鮮明な欠陥指示赤色ニジミ模様が現出し、油溶性蛍光染料を用いた浸透液の場合には暗室における紫外線灯の照射下で発光する黄緑色の欠陥指示蛍光模様の輝度が高く、いずれの場合にも、前記観察時において欠陥指示模様の判別が容易であるから、高精度をもって探傷できる。   In the present embodiment, in the cleaning process, when the warm water is sprayed onto the surface of the inspection object with the water pressure and flow rate, the hot water that has contacted the inspection object surface at the beginning of cleaning is the temperature of the inspection object (usually, Since the object to be inspected is a metal member such as steel, its temperature is cooled to room temperature: about 20 ° C, much lower than that), and remains on the surface of the object to be inspected by the cooled water and its water pressure. As the excess permeate begins to be removed and cleaning proceeds, the temperature of the surface of the object to be inspected rises due to the hot water being sprayed and approaches the temperature of the hot water, and the permeate that has permeated into the opening defect is in two phases. Since the separated upper phase part is an organic solvent component containing a small amount of water, it hardly dissolves in the sprayed warm water, and the occurrence of the overwash is suppressed as much as possible. And the separated lower phase Is water containing a small amount of organic solvent component, so the oil-soluble (red or fluorescent) dye component dissolved in the penetrating liquid moves to the upper phase part and the dye concentration is higher in the upper phase part. In the case of a penetrating liquid using an oil-soluble red dye, a clear defect-indicating red blemishes pattern appears on the surface of the developer thin layer. In the case of a penetrating liquid using an oil-soluble fluorescent dye, an ultraviolet lamp in a dark room is used. The brightness of the yellow-green defect indicating fluorescent pattern that emits light under irradiation is high, and in any case, the defect indicating pattern can be easily determined at the time of observation, so that flaw detection can be performed with high accuracy.

本発明を実施例及び比較例を挙げてより詳しく説明する。なお、以下に挙げる各実施例及び比較例における浸透液の分離温度並びに引火点の各測定並びに浸透探傷性能評価は、それぞれ次の方法によって行ったものである。   The present invention will be described in more detail with reference to examples and comparative examples. In addition, each of the separation temperature and flash point measurement of the penetrant and the penetrant flaw detection performance evaluation in each of the following examples and comparative examples were performed by the following methods.

分離温度の測定:測定対象浸透液をガラスビーカーに入れ、室温(約20℃)より徐々に加温しながら、目視にて観察し、当該浸透液が明確に二相分離し始めた時点の温度を測定した。   Measurement of separation temperature: Place the permeate to be measured in a glass beaker, gradually warm from room temperature (approx. 20 ° C), visually observe, and the temperature at which the permeate begins to clearly separate into two phases Was measured.

引火点の測定:測定対象浸透液の引火点と引火点の有無をJIS K 2265-4に準拠して測定した。   Measurement of flash point: The flash point of the permeated liquid to be measured and the presence or absence of the flash point were measured according to JIS K 2265-4.

性能評価:表面に長さ6mm、幅10μm、深さ100μmの人工きず(開口欠陥部)が設けられているステンレス製試験片、表面に長さ6mm、幅10μm、深さ150μmの人工きず(同上)が設けられているステンレス製試験片及び表面に長さ6mm、幅10μm、深さ200μmの人工きず(同上)が設けられているステンレス製試験片を使用し、室温(約20℃)において、測定対象浸透液を各試験片表面に塗布して付着させ、5分間静置した後、約65℃の温水を水圧0.3Mpa・流量1L/minにて当該各試験片表面に吹き付けて洗浄し、次いで、エアブローによって試験片表面の水滴を除いた後、熱風循環式乾燥機を使用して約60℃の熱風によって当該各試験片を5分間乾燥し、次いで、評価対象浸透液が油溶性赤色染料を用いたものである場合には、当該各試験片表面に市販の染色浸透探傷用現像剤(スーパーチェック現像剤UD-ST:商品名:主成分は無機質白色微粉末:マークテック株式会社)を用いて無機質白色微粉末の薄層を形成し、白色灯の下で目視にて当該薄層表面を観察して評価し、評価対象浸透液が油溶性蛍光染料を用いたものである場合には、現像剤を使用することなく、暗室において紫外線灯の照射下で目視にて当該各試験片表面を観察して評価した。   Performance evaluation: Stainless steel test piece with 6mm length, 10μm width and 100μm depth (open defect) on the surface, 6mm length, 10μm width and 150μm depth on the surface (same as above) ) And a stainless steel test piece with a surface of 6 mm long, 10 μm wide and 200 μm deep (same as above), and at room temperature (about 20 ° C.) After applying the permeation liquid to be measured to the surface of each test piece and allowing it to stand for 5 minutes, the hot water of about 65 ° C. is sprayed on the surface of each test piece at a water pressure of 0.3 Mpa and a flow rate of 1 L / min, and washed. Next, after removing water droplets on the surface of the test piece by air blowing, each test piece is dried for 5 minutes with hot air at about 60 ° C. using a hot air circulation dryer, and then the permeation liquid to be evaluated is an oil-soluble red dye. On the surface of each test piece. A thin layer of inorganic white fine powder is formed using a developer for penetrating flaw detection (Super Check Developer UD-ST: Product Name: Main component is inorganic white fine powder: Marktech Co., Ltd.) and visually observed under white light When the permeated liquid to be evaluated is an oil-soluble fluorescent dye, it is visually observed under the irradiation of an ultraviolet lamp in a dark room without using a developer. The surface of each test piece was observed and evaluated.

なお、比較例においては、約60℃の温水に代えて約20℃の水を使用した場合についても評価した。   In the comparative example, the case where about 20 ° C. water was used instead of about 60 ° C. hot water was also evaluated.

評価基準は、人工きずの深さに対応した明瞭な欠陥指示模様が視認できた場合を「○」とし(注:浸透液が油溶性赤色染料を用いたものである場合には、きずが深いほど欠陥指示模様の色彩が濃く、かつ、大きくなり、浸透液が油溶性蛍光染料を用いたものである場合には、きずが深いほど欠陥指示模様の輝度が高くなる)、視認できた欠陥指示模様が、一部途切れていたり、色彩が薄いか、或いは輝度が低く、明瞭さを欠く場合を「△」とし、欠陥指示模様を視認できない(注:欠陥指示模様が出ない)場合を「×」とした。   The evaluation standard is “○” when a clear defect indication pattern corresponding to the depth of the artificial flaw is visible (Note: If the penetrant is an oil-soluble red dye, the flaw is deep. If the defect indicating pattern is darker and larger in color, and the penetrant uses an oil-soluble fluorescent dye, the defect indicating pattern becomes brighter as the flaw is deeper). If the pattern is partly discontinuous, the color is light, or the brightness is low and the clarity is not clear, “△” indicates that the defect indicating pattern cannot be visually recognized (note: the defect indicating pattern does not appear). "

実施例1:EDGAC46.5重量%、水46.5重量%、ノニオン系界面活性剤(ノイゲンNL-Dash408:商品名:HLB12:第一工業株式会社)5.0重量%及び油溶性蛍光染料(Fluorol7GA:商品名:GAF社)2.0重量%の処方となるように各材料を秤取し、秤取した各材料をステンレス製タンクに投入し、室温(約20℃)において電動ミキサーを使用して30分間攪拌することにより、当該各材料が混和・熔解して単一相の状態となっている水洗性水ベース蛍光浸透液を調製した。なお、当該浸透液におけるEDGACに対する水の混合割合は1:1である。   Example 1: EDGAC 46.5 wt%, water 46.5 wt%, nonionic surfactant (Neugen NL-Dash408: trade name: HLB12: Daiichi Kogyo Co., Ltd.) 5.0 wt% and oil-soluble fluorescent dye (Fluorol7GA: trade name) : GAF) Weigh each material so that it becomes a prescription of 2.0% by weight, put each weighed material into a stainless steel tank, and stir for 30 minutes using an electric mixer at room temperature (about 20 ° C) Thus, a water-washable water-based fluorescent penetrating solution in which the respective materials were mixed and melted to form a single phase was prepared. The mixing ratio of water to EDGAC in the permeation solution is 1: 1.

ここに得られた水洗性水ベース蛍光浸透液の分離温度は50℃であり、引火点はなく、探傷性能評価結果は、いずれの試験片についても「○」であった。   The separation temperature of the washable water-based fluorescent penetrating solution obtained here was 50 ° C., there was no flash point, and the flaw detection performance evaluation results were “◯” for all the test pieces.

実施例2:EDGAC46.5重量%をDEDG38.0重量%に、水の割合を57.0重量%に、ノニオン系界面活性剤の割合を3.0重量%に、それぞれ代えた以外は、実施例1と同一条件にて、当該各材料が混和・溶解して単一相の状態となっている水洗性水ベース蛍光浸透液を調製した。なお、当該浸透液におけるDEDGに対する水の混合割合は1:1.5である。   Example 2: Same as Example 1 except that 46.5% by weight of EDGAC was changed to 38.0% by weight of DEDG, 57.0% by weight of water, and 3.0% by weight of nonionic surfactant. Under the conditions, a washable water-based fluorescent permeation solution in which the respective materials were mixed and dissolved to form a single phase was prepared. In addition, the mixing ratio of water with respect to DEGD in the permeation solution is 1: 1.5.

ここに得られた水洗性水ベース蛍光浸透液の分離温度は40℃であり、引火点はなく、探傷性能評価は、きず深さ100μmの試験片については「△」、他の試験片については「○」であった。   The separation temperature of the washable water-based fluorescent penetrant obtained here is 40 ° C., there is no flash point, and the flaw detection performance evaluation is “△” for a test piece having a scratch depth of 100 μm, and for other test pieces. It was “○”.

実施例3:EDGAC31.0重量%、DEDG30.0重量%、水31.0重量%、ノニオン系界面活性剤(同上)7.0重量%、油溶性蛍光染料(同上)1.0重量%とした以外は、実施例1と同一条件にて、当該各材料が混和・溶解して単一相の状態となっている水洗性水ベース蛍光浸透液を調製した。なお、当該浸透液におけるEDGAC及びDEDGに対する水の混合割合は1:1.96である。   Example 3: Example except that 3% by weight of EDGAC, 30.0% by weight of DEDG, 31.0% by weight of water, 7.0% by weight of nonionic surfactant (same as above), 1.0% by weight of oil-soluble fluorescent dye (same as above) A water-washable water-based fluorescent permeation solution in which the respective materials were mixed and dissolved in a single phase under the same conditions as in 1 was prepared. In addition, the mixing ratio of water with respect to EDGAC and DEDG in the permeation solution is 1: 1.96.

ここに得られた水洗性水ベース蛍光浸透液の分離温度は37℃であり、引火点はなく、探傷性能評価結果は、いずれの試験片についても「○」であった。   The separation temperature of the washable water-based fluorescent penetrating solution obtained here was 37 ° C., there was no flash point, and the flaw detection performance evaluation results were “◯” for all the test pieces.

実施例4:PMA31.0重量%、水46.5重量%、ノニオン系界面活性剤(同上)5.0重量%、BDG15.5重量%及び油溶性赤色染料(オイルレッド5B:商品名:オリエント株式会社)2.0重量%の処方となるように各材料を秤取し、秤取した各材料をステンレス製タンクに投入し、室温(約20℃)において電動ミキサーを使用して30分間攪拌することにより、当該各材料が混和・溶解して単一相の状態となっている水洗性水ベース赤色浸透液を調製した。なお、当該浸透液におけるPMAに対する水の混合割合は1:1.5である。   Example 4: PMA 31.0% by weight, water 46.5% by weight, nonionic surfactant (same as above) 5.0% by weight, BDG 15.5% by weight and oil-soluble red dye (Oil Red 5B: trade name: Orient Corporation) 2.0 Each material is weighed so as to give a prescription of wt%, and each weighed material is put into a stainless steel tank and stirred at room temperature (about 20 ° C) for 30 minutes using an electric mixer. A washable water-based red penetrant in which the material was mixed and dissolved to form a single phase was prepared. The mixing ratio of water to PMA in the permeation solution is 1: 1.5.

ここに得られた水洗性水ベース赤色浸透液の分離温度は35℃であり、引火点はなく、探傷性能評価結果は、いずれの試験片についても「○」であった。   The separation temperature of the washable water-based red penetrant obtained here was 35 ° C., there was no flash point, and the flaw detection performance evaluation result was “◯” for any test piece.

実施例5:PMA31.0重量%をBCL44.0重量%に、水の割合を44.0重量%に、BOGの割合を5.0重量%に、それぞれ代えた以外は、実施例4と同一条件にて、当該各材料が混和・溶解して単一相の状態となっている水洗性水ベース赤色浸透液を調製した。なお、当該浸透液におけるBCLに対する水の混合割合は1:1である。   Example 5: Under the same conditions as in Example 4, except that PMA 31.0% by weight was changed to BCL 44.0% by weight, the water ratio was changed to 44.0% by weight, and the BOG ratio was changed to 5.0% by weight. A water-washable water-based red penetrant in which the respective materials were mixed and dissolved to form a single phase was prepared. The mixing ratio of water to BCL in the permeation solution is 1: 1.

ここに得られた水洗性水ベース赤色浸透液の分離温度は60℃であり、引火点はなく、探傷性能評価結果は、いずれの試験片についても「○」であった。   The separation temperature of the washable water-based red penetrant obtained here was 60 ° C., there was no flash point, and the flaw detection performance evaluation result was “◯” for any test piece.

実施例6:PMA31.0重量%をDEDG31.0重量%に、水の割合を65.0重量%に、ノニオン系界面活性剤(同上)の割合を3.0重量%に、油溶性赤色染料(同上)の割合を1.0重量%にそれぞれ代え、BDGを用いなかった以外は、実施例4と同一条件にて、当該各材料が混和・溶解して単一相の状態となっている水洗性水ベース赤色浸透液を調製した。なお、当該浸透液におけるDEDGに対する水の混合割合は1:2である。   Example 6: PMA 31.0% by weight DEDG 31.0% by weight, water ratio 65.0% by weight, nonionic surfactant (same as above) ratio 3.0% by weight, oil-soluble red dye (same as above) A water-washable water-based red permeation in which each material is mixed and dissolved in a single phase under the same conditions as in Example 4 except that the ratio was changed to 1.0% by weight and BDG was not used. A liquid was prepared. In addition, the mixing ratio of water with respect to DEGG in the permeation solution is 1: 2.

ここに得られた水洗性水ベース赤色浸透液の分離温度は50℃であり、引火点はなく、探傷性能評価は、きず深さ100μmの試験片については「△」、他の試験片については「○」であった。   The separation temperature of the washable water-based red penetrant obtained here is 50 ° C., there is no flash point, and the flaw detection performance evaluation is “△” for a test piece with a scratch depth of 100 μm, and for other test pieces. It was “○”.

比較例1:EDGACの割合を18.0重量%に、水の割合を78.0重量%に、ノニオン系界面活性剤の割合を3.0重量%に、油溶性蛍光染料の割合を1.0重量%に、それぞれ代えた以外は、実施例1と同一条件にて、当該各材料が混和・溶解して単一相の状態となっている比較用水洗性水ベース蛍光浸透液を調製した。なお、当該浸透液におけるEDGACに対する水の混合割合は1:4.3である。   Comparative Example 1: The ratio of EDGAC was changed to 18.0 wt%, the ratio of water to 78.0 wt%, the ratio of nonionic surfactant to 3.0 wt%, and the ratio of oil-soluble fluorescent dye to 1.0 wt%, respectively. Except for the above, under the same conditions as in Example 1, a comparative washable water-based fluorescent permeation solution in which the respective materials were mixed and dissolved to form a single phase was prepared. The mixing ratio of water to EDGAC in the permeation solution is 1: 4.3.

ここに得られた比較用水洗性水ベース蛍光浸透液は、液温を100℃まで上昇させても二相に分離せず、引火点はなく、探傷性能評価結果は、約20℃の水を使用した場合にはきず深さ100μmの試験片については「×」、きず深さ150μmの試験片については「△」、きず深さ200μmの試験片については「○」であり、約65℃の温水を使用した場合にはきず深さ100μmの試験片ときず深さ150μmの試験片についてはいずれも「×」、きず深さ200μmの試験片については「△」であった。   The comparative washable water-based fluorescent penetrant obtained here does not separate into two phases even when the liquid temperature is raised to 100 ° C, there is no flash point, and the flaw detection performance evaluation result is about 20 ° C water. When used, it is “×” for a specimen having a flaw depth of 100 μm, “△” for a specimen having a flaw depth of 150 μm, and “◯” for a specimen having a flaw depth of 200 μm. When hot water was used, the test piece with a scratch depth of 100 μm and the test piece with a depth of 150 μm were both “x”, and the test piece with a crack depth of 200 μm was “Δ”.

比較例2:PMA31.0重量%をEDGAC39.2重量%に、水の割合を58.8重量%に、それぞれ代え、界面活性剤とBDGを用いなかった以外は、実施例4と同一条件にて、当該各材料が混和・溶解して単一相の状態となっている比較用水洗性水ベース赤色浸透液を調製した。なお、当該浸透液のEDGACに対する水の混合割合は1:1.5である。   Comparative Example 2: PMA 31.0% by weight EDGAC 39.2% by weight, water ratio 58.8% by weight, respectively, except that surfactant and BDG were not used, under the same conditions as Example 4 A comparative washable water-based red penetrant in which each material was mixed and dissolved to form a single phase was prepared. In addition, the mixing ratio of water with respect to EDGAC of the said permeate is 1: 1.5.

ここに得られた比較用水洗性水ベース赤色浸透液の分離温度は43℃であり、引火点はなく、探傷性能評価結果は、約20℃の水を使用した場合にはきず深さ100μmの試験片については「×」、きず深さ150μmの試験片ときず深さ200μmの試験片については、いずれも「△」であり、約65℃の温水を使用した場合にはきず深さ100μmの試験片については「×」、きず深さ150μmの試験片については「△」、きず深さ200μmの試験片については「○」であった。   The separation temperature of the comparative washable water-based red penetrant obtained here is 43 ° C, there is no flash point, and the flaw detection performance evaluation result is a flaw depth of 100μm when using water at about 20 ° C. “×” for the test piece, “△” for both the test piece with a depth of 150 μm and the test piece with a depth of 200 μm, and when the hot water of about 65 ° C. is used, the depth is 100 μm. The test piece was “x”, the test piece having a flaw depth of 150 μm was “Δ”, and the test piece having a flaw depth of 200 μm was “◯”.

比較例3:水46.5重量%、ノニオン系界面活性剤(同上)5.0重量%、BDG46.5重量%及び油溶性蛍光染料(同上)2重量%とし、EDGAを用いなかった以外は、実施例1と同一条件にて、当該各材料が混和・溶解して単一相の状態となっている比較用水洗性水ベース蛍光浸透液を調製した。   Comparative Example 3 Example 1 except that 46.5% by weight of water, 5.0% by weight of a nonionic surfactant (same as above), 46.5% by weight of BDG and 2% by weight of an oil-soluble fluorescent dye (same as above) were used, and EDGA was not used. A comparative washable water-based fluorescent permeation solution in which each material was mixed and dissolved in a single phase under the same conditions was prepared.

ここに得られた比較用水洗性水ベース蛍光浸透液は液温を100℃まで上昇させても二相に分離せず、引火点はなく、探傷性能評価結果は、約20℃の水を使用した場合にはきず深さ100μmの試験片ときず深さ150μmの試験片についてはいずれも「△」、きず深さ200μmの試験片については「○」であり、約65℃の温水を使用した場合にはきず深さ100μmの試験片については「×」、きず深さ150μmの試験片については「△」、きず深さ200μmの試験片については「○」であった。   The comparative washable water-based fluorescent penetrant obtained here does not separate into two phases even when the liquid temperature is raised to 100 ° C, there is no flash point, and the flaw detection performance evaluation results use water of about 20 ° C In this case, the test piece with a scratch depth of 100 μm and the test piece with a depth of 150 μm are both “△”, and the test piece with a crack depth of 200 μm is “◯”, using hot water of about 65 ° C. In this case, the test piece having a scratch depth of 100 μm was “×”, the test piece having a scratch depth of 150 μm was “Δ”, and the test piece having a scratch depth of 200 μm was “◯”.

比較例4:EDGAC46.5重量%、非水溶性有機溶剤(カクタスノルマルパラフィンN-12:商品名:ノルマルパラフィン:株式会社ジャパンエナジー)40.0重量%、ノニオン系界面活性剤(同上)5.0重量%、BDG6.5重量%、油溶性蛍光染料(同上)2.0重量%とし、水を用いなかった以外は、実施例1と同一条件にて、当該各材料が混和・溶解して単一相の状態となっている比較用水洗性油ベース蛍光浸透液を調製した。   Comparative Example 4: EDGAC 46.5% by weight, water-insoluble organic solvent (Cactus normal paraffin N-12: trade name: normal paraffin: Japan Energy Co., Ltd.) 40.0% by weight, nonionic surfactant (same as above) 5.0% by weight, BDG 6.5% by weight, oil-soluble fluorescent dye (same as above) 2.0% by weight, except that water was not used, each material was mixed and dissolved in a single phase under the same conditions as in Example 1. A comparative washable oil-based fluorescent penetrant was prepared.

ここに得られた比較用水洗性油ベース蛍光浸透液は、液温を100℃まで上昇させても二相に分離せず、引火点は89℃であり、探傷性能評価結果は、約20℃の水を使用した場合及び約65℃の温水を使用した場合ともに、きず深さ100μmの試験片については「△」、きず深さ150μmの試験片ときず深さ200μmの試験片についてはいずれも「○」であった。   The comparative washable oil-based fluorescent penetrant obtained here does not separate into two phases even when the liquid temperature is raised to 100 ° C, the flash point is 89 ° C, and the flaw detection performance evaluation result is about 20 ° C. In the case of using water of approximately 65 ° C and in the case of using hot water of about 65 ° C, △ is indicated for specimens with a scratch depth of 100 μm, and specimens with a depth of 150 μm and specimens with a depth of 200 μm are both used. It was “○”.

本発明によれば、周知浸透探傷試験を引火点のない水洗性水ベース浸透液を用いて実施でき、その余剰浸透液の除去に当たって過洗浄の発生を可及的に抑制して高精度をもって被検査物表面に存在する微細な開口欠陥部が探傷できるので、浸透液の大量使用・貯蔵と高精度の欠陥検出性能とを必要としている自動車工場などにおける浸透探傷試験現場の要求を満たすことができるから、本発明に産業利用性は大きいといえる。   According to the present invention, a well-known penetrant flaw detection test can be performed using a flushable water-based penetrant having no flash point, and the occurrence of overwashing is suppressed as much as possible in removing the surplus penetrant so that the test can be performed with high accuracy. Since fine opening defects on the surface of the inspection object can be inspected, it can meet the demands of the penetration inspection field in automobile factories that require large-scale use / storage of penetrant and high-accuracy defect detection performance. Therefore, it can be said that the present invention has great industrial applicability.

Claims (1)

有機溶剤と水とを該有機溶剤が該水に溶解して単一相になっている状態と該有機溶剤が該水から分離して二相になっている状態との二つの相状態間を温度変化によって可逆的に変化すると共に引火点を有しない割合にて混合してなる主溶剤と該有機溶剤に溶解する油溶性赤色染料又は油溶性蛍光染料と界面活性剤とが配合されている浸透探傷試験用水洗性水ベース浸透液を、当該浸透液の相状態が前記単一相になっている状態で被検査物表面に付着させ、当該浸透液を被検査物表面の開口欠陥部に浸透させた後、当該浸透液の相状態が前記二相に変化する温度以上の温水によって当該被検査物表面を洗浄して開口欠陥部内に浸透せずに被検査物表面に残留している余剰浸透液を除去し、次いで開口欠陥部内に浸透している浸透液によって開口欠陥部の存在を探傷することを特徴とする浸透探傷試験方法。 An organic solvent and water are dissolved in the water to form a single phase, and the organic solvent is separated from the water into a two-phase state. Penetration in which a main solvent mixed reversibly with a temperature change and having a flash point and an oil-soluble red dye or oil-soluble fluorescent dye dissolved in the organic solvent and a surfactant are blended A washable water-based penetrant for flaw detection tests is attached to the surface of the inspection object in a state in which the phase of the permeation liquid is the single phase, and the permeation liquid penetrates into an opening defect portion on the surface of the inspection object. Then, excess permeation that remains on the surface of the inspection object without being infiltrated into the opening defect by washing the surface of the inspection object with warm water at a temperature equal to or higher than the temperature at which the phase state of the permeation liquid changes to the two phases. Remove the liquid and then open it with the permeate that has penetrated into the opening defect Penetrant method characterized by testing for the presence of Recessed portion.
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