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WO2025115169A1 - Liquide d'inspection fluorescent - Google Patents

Liquide d'inspection fluorescent Download PDF

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Publication number
WO2025115169A1
WO2025115169A1 PCT/JP2023/042895 JP2023042895W WO2025115169A1 WO 2025115169 A1 WO2025115169 A1 WO 2025115169A1 JP 2023042895 W JP2023042895 W JP 2023042895W WO 2025115169 A1 WO2025115169 A1 WO 2025115169A1
Authority
WO
WIPO (PCT)
Prior art keywords
fluorescent
blue
fluorescent dye
quinine
ppm
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/JP2023/042895
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English (en)
Japanese (ja)
Inventor
川村陽一
奥平宏行
吉田安徳
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SMC Corp
Original Assignee
SMC Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by SMC Corp filed Critical SMC Corp
Priority to PCT/JP2023/042895 priority Critical patent/WO2025115169A1/fr
Priority to TW113144465A priority patent/TW202536140A/zh
Publication of WO2025115169A1 publication Critical patent/WO2025115169A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01MTESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M3/00Investigating fluid-tightness of structures
    • G01M3/02Investigating fluid-tightness of structures by using fluid or vacuum
    • G01M3/04Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point
    • G01M3/20Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84Systems specially adapted for particular applications
    • G01N21/88Investigating the presence of flaws or contamination
    • G01N21/91Investigating the presence of flaws or contamination using penetration of dyes, e.g. fluorescent ink

Definitions

  • the present invention relates to a fluorescent inspection liquid used for leak inspection.
  • Leak inspections are carried out on equipment that requires airtightness and on piping systems in factories, etc.
  • One type of leak inspection is the fluorescent leak inspection method, which uses an inspection liquid containing a fluorescent dye (fluorescent inspection liquid).
  • JP 10-221196 A describes the use of food additives (Food Red No. 2, Food Red No. 106, Food Blue No. 1, Food Green No. 3) as the fluorescent agents in the fluorescent inspection liquid.
  • a blue fluorescent agent is a coumarin derivative.
  • coumarin derivatives are toxic to the human body, and therefore are avoided for use in, for example, food equipment.
  • Another example of a substance that emits blue fluorescence is quinine.
  • Quinine is used as a bittering agent in soft drinks (tonic water), and is a substance that is safe for the human body.
  • Quinine's fluorescence is a deep blue color.
  • quinine's fluorescence is not bright enough, and it is difficult to distinguish it from the external light that enters the measurement location and the blue-purple light emitted from a black light as an ultraviolet light source, resulting in poor visibility during leak inspections.
  • the inventors of this application therefore felt that a fluorescent testing liquid that emits a blue color and is both safe for the human body and highly visible in leak testing is needed.
  • the present invention aims to solve the above problems.
  • a fluorescent test solution that includes water as a solvent, a first blue fluorescent dye selected from any one of a flavin derivative, quinine, pyrene, and anthocyanin, and a second blue fluorescent dye selected from any one of the flavin derivative, quinine, pyrene, and anthocyanin excluding the first blue fluorescent dye, where the flavin derivative has a flavin skeleton and is a derivative that uses riboflavin as a starting material.
  • the fluorescent inspection liquid described above has a relatively low toxicity to the human body, and compared to the use of a single blue fluorescent dye, the saturation of the fluorescent color is improved, resulting in excellent visibility during leak inspection.
  • FIG. 1 shows photographs of an aqueous solution of a flavin derivative, an aqueous solution of quinine, an aqueous solution of pyrene, and an aqueous solution of anthocyanin (each having a concentration of 10 ppm) irradiated with ultraviolet light in a dark room.
  • FIG. 2A is a photograph of a first fluorescent test solution containing a flavin derivative and quinine (both at a concentration of 10 ppm) irradiated with ultraviolet light in a dark room
  • FIG. 2B is a photograph of a second fluorescent test solution containing a flavin derivative and pyrene (both at a concentration of 10 ppm) irradiated with ultraviolet light in a dark room.
  • FIG. 1 shows photographs of an aqueous solution of a flavin derivative, an aqueous solution of quinine, an aqueous solution of pyrene, and an aqueous solution of anthocyanin (each having a concentration
  • FIG. 3A is a photograph of a third fluorescent test solution containing a flavin derivative and anthocyanin (both at a concentration of 10 ppm) irradiated with ultraviolet light in a dark room
  • FIG. 3B is a photograph of a fourth fluorescent test solution containing quinine and pyrene (both at a concentration of 10 ppm) irradiated with ultraviolet light in a dark room
  • FIG. 4A is a photograph of the fifth fluorescent test solution containing quinine and anthocyanin (both at a concentration of 10 ppm) irradiated with ultraviolet light in a dark room
  • FIG. 4B is a photograph of the sixth fluorescent test solution containing pyrene and anthocyanin (both at a concentration of 10 ppm) irradiated with ultraviolet light in a dark room.
  • the fluorescent inspection liquid of this embodiment is used for leak inspection of equipment or piping that requires a certain degree of airtightness.
  • the fluorescent inspection liquid is sprayed as a mist into compressed air and introduced into the inside of the target equipment. If there is a leak in the object being inspected, the fluorescent inspection liquid will leak out from the leak site and stain the leak site with a blue fluorescent dye.
  • ultraviolet light is then shone on the object being inspected from outside using a light source such as a black light, the fluorescent inspection liquid will emit blue fluorescence at the leak site, making it possible to visually detect the leak site.
  • the fluorescent test solution of this embodiment is composed of a composition in which a blue fluorescent dye is dissolved in water as a solvent.
  • the blue fluorescent dye is a dye that is excited by irradiation with ultraviolet light and emits blue fluorescence (wavelength 360 to 500 nm).
  • the fluorescent test solution of this embodiment contains two types of blue fluorescent dyes selected from flavin derivatives, quinine, pyrene, and anthocyanin.
  • the fluorescent test solution contains a first blue fluorescent dye and a second blue fluorescent dye.
  • the fluorescent test solution may further contain a third blue fluorescent dye.
  • the flavin derivative is a derivative that starts from riboflavin (vitamin B2) that has a flavin skeleton.
  • the fluorescent test solution may contain at least one of the flavin derivatives, for example formylmethylflavin and lumichrome, as a main component.
  • lumichrome (7,8-dimethylalloxazine) absorbs ultraviolet light and emits blue fluorescence with a fluorescent emission peak at 450 to 480 nm.
  • the flavin derivative of this embodiment is obtained by irradiating an aqueous solution of riboflavin with a sufficient amount (time) of light, and emits blue fluorescence.
  • flavin derivatives are substances that are generated in the body as metabolic products of riboflavin, and if ingested in excess, they will be excreted from the body through the same metabolic mechanism as riboflavin. Flavin derivatives are also contained in food as photodecomposition products of riboflavin, and are ingested on a daily basis. Therefore, fluorescent test solutions containing flavin derivatives are considered to have relatively low toxicity to the human body and excellent safety.
  • Quinine absorbs ultraviolet light and emits a deep blue fluorescence with a peak emission wavelength of 440-490 nm. Quinine is used as a bittering agent in soft drinks (tonic water) and as a treatment for malaria, and has extremely low toxicity to the human body.
  • Pyrene absorbs ultraviolet light and emits a bright blue fluorescence with a peak emission wavelength of 450-500 nm.
  • Anthocyanin is a pigment found in plant pigments that absorbs ultraviolet light and emits deep blue fluorescence. Anthocyanin is also found in food and is considered to be highly safe when ingested orally.
  • the total concentration of the blue fluorescent dye contained in the fluorescent test solution of this embodiment is set within a range that satisfies the standard values of COD (Chemical Oxygen Demand) and BOD (Biochemical Oxygen Demand) that are permissible for discharge into sewage.
  • the standard values of COD and BOD in Japan are 160 mg/L.
  • the total concentration of the blue fluorescent dye satisfies the above-mentioned COD and BOD standard values, and from this perspective, it is preferable that the total concentration of the blue fluorescent dye be, for example, 30 ppm or less.
  • the blue fluorescent dye used in the fluorescent inspection liquid of this embodiment is a substance that is easily decomposed (putrefied) by microorganisms
  • a preservative may be included to prevent deterioration due to putrefaction during transportation and storage.
  • a paraoxybenzoic acid ester such as butylparaben, isopropylparaben, propylparaben, ethylparaben, or methylparaben, or an isothiazolinone derivative such as methylisothiazolinone can be used.
  • the preservative concentration can be set appropriately depending on the application. If the preservative concentration is in the range of 10 ppm or less, it is within the range approved for use as a food additive. Therefore, a fluorescent inspection liquid containing 100 ppm or less of a preservative can be used more safely in equipment that handles food. Furthermore, if the preservative concentration is in the range of 100 ppm or less, it is within the range approved for medical equipment that comes into contact with the human body. Therefore, if the preservative concentration is 100 ppm or less, it is thought that there will be almost no irritation to the user's skin even if the fluorescent inspection liquid is exposed to the skin.
  • the fluorescent inspection liquid of this embodiment includes the following six types based on the combination of blue fluorescent dyes.
  • First fluorescent test solution Flavin derivative and quinine
  • Second fluorescent test solution Flavin derivative and pyrene
  • Third fluorescent test solution Flavin derivative and anthocyanin
  • Fourth fluorescent test solution Quinine and pyrene
  • Fifth fluorescent test solution Quinine and anthocyanin
  • Sixth fluorescent test solution Pyrene and anthocyanin
  • the first fluorescent test solution containing a flavin derivative and quinine is safe even if taken orally, has a high saturation S, and emits bright fluorescence, so it is also excellent in visibility. For this reason, the first fluorescent test solution is suitable for leak testing.
  • the first fluorescent test solution contains a flavin derivative at a concentration of 5 ppm to 20 ppm and quinine at a concentration of 1 ppm to 10 ppm, and has an excellent balance of hue H, saturation S, and brightness V, and has good visibility. If the concentration of the flavin derivative falls below the above range, the brightness of the fluorescence decreases, making it difficult to use in leak testing.
  • the concentration of quinine falls below 1 ppm, bright blue fluorescence cannot be obtained.
  • a quinine concentration of 10 ppm is close to the upper limit of quinine's solubility in water at room temperature.
  • the first fluorescent inspection liquid with this concentration meets the sewage discharge standard of 160 mg/L or less for COD and BOD, and is easy to dispose of after use. Furthermore, the first fluorescent inspection liquid is decomposed in the atmosphere in a relatively short time, about a few hours to a few days. Therefore, the impact on the environment can be reduced.
  • the amount of fluorescent light emitted by the first to sixth fluorescent test solutions when irradiated with ultraviolet light was investigated.
  • an increase in the amount of fluorescent light of about 1.1 to 1.5 times was observed in the first, second and third fluorescent test solutions compared to the blue fluorescent dye alone.
  • no increase in the amount of fluorescent light was observed in the third, fifth and sixth fluorescent test solutions, which contain anthocyanin.
  • Anthocyanin absorbs light with a wavelength of around 500 nm, so it is thought that it does not contribute much to the increase in the amount of light.
  • the hue H, saturation S and value V were investigated.
  • An aqueous solution of flavin derivative with a concentration of 10 ppm had a hue H of 208°, saturation S of 74%, and brightness V of 31%.
  • An aqueous solution of quinine with a concentration of 10 ppm had a hue H of 233°, saturation S of 81%, and brightness V of 20%.
  • An aqueous solution of pyrene with a concentration of 10 ppm had a hue H of 212°, saturation S of 75%, and brightness V of 23%.
  • An aqueous solution of anthocyanin had a hue H of 231°, saturation S of 75%, and brightness V of 10%.
  • the first fluorescent test solution shown in Figure 2A is an aqueous solution containing a flavin derivative with a concentration of 10 ppm and quinine with a concentration of 10 ppm.
  • the first fluorescent test solution had a hue H of 215°, a saturation S of 85%, and a brightness V of 29%. From these results, it was confirmed that the saturation S value of the first fluorescent test solution, 85%, is higher than the saturation S value of the flavin derivative aqueous solution, 74%, and the saturation S value of the quinine aqueous solution, 81%, improving visibility.
  • the second fluorescent test liquid in Figure 2B is an aqueous solution containing a flavin derivative with a concentration of 10 ppm and pyrene with a concentration of 10 ppm.
  • the second fluorescent test liquid had a hue H of 212°, a saturation S of 92%, and a brightness V of 45%.
  • the saturation S value of 92% for the second fluorescent test liquid is higher than the saturation S value of the aqueous solution of the flavin derivative (74%) and the saturation S value of the aqueous solution of pyrene (75%), confirming that improved visibility is due to improved saturation S.
  • the third fluorescent test solution in Figure 3A is an aqueous solution containing a flavin derivative at a concentration of 10 ppm and anthocyanin at a concentration of 10 ppm.
  • the third fluorescent test solution had a hue H of 209°, a saturation S of 82%, and a brightness V of 28%.
  • the saturation S value of 82% for the third fluorescent test solution is higher than the saturation S value of the flavin derivative aqueous solution (74%) and the saturation S value of the anthocyanin aqueous solution (75%), confirming that visibility is improved.
  • the fourth fluorescent test solution in Figure 3B is an aqueous solution containing quinine at a concentration of 10 ppm and pyrene at a concentration of 10 ppm.
  • the fourth fluorescent test solution had a hue H of 225°, a saturation S of 92%, and a brightness V of 36%.
  • the saturation S value of 92% for the fourth fluorescent test solution is higher than the saturation S value of 81% for the quinine aqueous solution and the saturation S value of 75% for the pyrene aqueous solution, confirming that visibility is improved.
  • the fifth fluorescent test solution in Figure 4A is an aqueous solution containing quinine at a concentration of 10 ppm and anthocyanin at a concentration of 10 ppm.
  • the fifth fluorescent test solution had a hue H of 235°, a saturation S of 97%, and a brightness V of 13%.
  • the saturation S value of 97% for the fifth fluorescent test solution is higher than the saturation S value of 81% for the quinine aqueous solution and the saturation S value of 75% for the anthocyanin aqueous solution, confirming that visibility is improved.
  • the sixth fluorescent test solution in Figure 4B is an aqueous solution containing pyrene at a concentration of 10 ppm and anthocyanin at a concentration of 10 ppm.
  • the sixth fluorescent test solution had a hue H of 217°, saturation S of 88%, and brightness V of 23%.
  • the saturation S value of 88% for the sixth fluorescent test solution is higher than the saturation S value of 75% for the pyrene aqueous solution and the saturation S value of 75% for the anthocyanin aqueous solution, confirming that visibility is improved.
  • a fluorescent inspection liquid that emits blue fluorescence with high saturation S can be obtained, improving visibility during leak inspections. Furthermore, the fluorescent inspection liquid of the embodiment has little impact on the human body and the environment, and can be used for a variety of purposes.
  • the present invention is not limited to the above disclosure, and various configurations may be adopted without departing from the gist of the present invention.
  • the following notes are further disclosed in relation to the above disclosure.
  • One aspect is a fluorescent test solution comprising water as a solvent, a first blue fluorescent dye selected from any one of a flavin derivative, quinine, pyrene, and anthocyanin, and a second blue fluorescent dye selected from any one of the flavin derivative, quinine, pyrene, and anthocyanin excluding the first blue fluorescent dye, the flavin derivative having a flavin skeleton and using riboflavin as a starting material.
  • a fluorescent test solution is excellent in safety, and furthermore, has a higher saturation and is excellent in visibility in leakage test compared to an aqueous solution of the first blue fluorescent dye or the second blue fluorescent dye alone.
  • the first blue fluorescent dye may be the flavin derivative, and the second blue fluorescent dye may be quinine.
  • the fluorescent inspection liquid is excellent in safety even when orally ingested, since the blue fluorescent dye is a substance contained in food. Therefore, the fluorescent inspection liquid can be suitably used for leak inspection of food equipment, etc., where safety is required.
  • the fluorescent inspection liquid described in Appendix 2 may contain the flavin derivative as the first blue fluorescent dye at a concentration of 5 ppm to 20 ppm, and may contain quinine as the second blue fluorescent dye at a concentration of 1 ppm to 7 ppm.
  • This fluorescent inspection liquid exhibits vivid blue fluorescence and has COD and BOD values below the sewage discharge standard of 160 mg/L, so that it can be discharged into the sewer, and waste liquid after inspection can be discharged into the sewer.
  • the first blue fluorescent dye may be the flavin derivative
  • the second blue fluorescent dye may be pyrene.
  • Such a fluorescent inspection solution has higher saturation and is excellent in visibility in leakage inspection, compared with an aqueous solution of the first blue fluorescent dye or the second blue fluorescent dye alone.
  • the first blue fluorescent dye may be the flavin derivative
  • the second blue fluorescent dye may be anthocyanin.
  • Such a fluorescent inspection solution has higher saturation and is excellent in visibility in leakage inspection, compared with an aqueous solution of the first blue fluorescent dye or the second blue fluorescent dye alone.
  • the first blue fluorescent dye may be quinine and the second blue fluorescent dye may be pyrene.
  • Such a fluorescent test solution has higher saturation and is excellent in visibility in leak testing, compared to an aqueous solution of the first blue fluorescent dye or the second blue fluorescent dye alone.
  • the first blue fluorescent dye may be quinine
  • the second blue fluorescent dye may be anthocyanin.
  • Such a fluorescent test solution has higher saturation and is excellent in visibility in leakage test, compared with an aqueous solution of the first blue fluorescent dye or the second blue fluorescent dye alone.
  • the first blue fluorescent dye may be pyrene and the second blue fluorescent dye may be anthocyanin.
  • Such a fluorescent inspection solution has higher saturation and is excellent in visibility in leakage inspection, compared with an aqueous solution of the first blue fluorescent dye or the second blue fluorescent dye alone.
  • the fluorescent inspection solution according to any one of appendices 1 to 8 may contain at least one of formylmethylflavin and lumichrome as a main component as the flavin derivative. This fluorescent inspection solution is safe and reduces the burden on the environment, and also exhibits blue fluorescence with excellent visibility, making it suitable for leak inspection.

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  • Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Biochemistry (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Examining Or Testing Airtightness (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)

Abstract

La présente invention concerne un liquide d'inspection fluorescent qui est très sûr pour un corps humain et émet une fluorescence bleue ayant une visibilité élevée dans l'inspection de fuite. Le liquide d'inspection fluorescent contient de l'eau en tant que solvant et deux colorants fluorescents bleus choisis parmi un dérivé de flavine, la quinine, le pyrène et l'anthocyanine. Le dérivé de flavine est un dérivé ayant un squelette de flavine et obtenu à partir d'un matériau de départ, la riboflavine.
PCT/JP2023/042895 2023-11-30 2023-11-30 Liquide d'inspection fluorescent Pending WO2025115169A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PCT/JP2023/042895 WO2025115169A1 (fr) 2023-11-30 2023-11-30 Liquide d'inspection fluorescent
TW113144465A TW202536140A (zh) 2023-11-30 2024-11-19 螢光檢測液

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2023/042895 WO2025115169A1 (fr) 2023-11-30 2023-11-30 Liquide d'inspection fluorescent

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WO2025115169A1 true WO2025115169A1 (fr) 2025-06-05

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007006709A (ja) * 2005-06-28 2007-01-18 Matsushita Electric Ind Co Ltd 発光物の判別方法
JP2011513213A (ja) * 2008-02-25 2011-04-28 ロレアル 皮膚および/または髪の外観を改善するための、光線とリパーゼにより生物学的に変換可能な化合物との組合せ
JP2017513820A (ja) * 2014-03-28 2017-06-01 カールスルーエ インスティテュート フュア テクノロジ 無機有機ハイブリッド化合物
JP2021172607A (ja) * 2020-04-23 2021-11-01 株式会社 資生堂 紫外線波長変換物質、炭化水素油及び/又は直鎖シリコーン油、並びに粉末を含有する肌用組成物

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007006709A (ja) * 2005-06-28 2007-01-18 Matsushita Electric Ind Co Ltd 発光物の判別方法
JP2011513213A (ja) * 2008-02-25 2011-04-28 ロレアル 皮膚および/または髪の外観を改善するための、光線とリパーゼにより生物学的に変換可能な化合物との組合せ
JP2017513820A (ja) * 2014-03-28 2017-06-01 カールスルーエ インスティテュート フュア テクノロジ 無機有機ハイブリッド化合物
JP2021172607A (ja) * 2020-04-23 2021-11-01 株式会社 資生堂 紫外線波長変換物質、炭化水素油及び/又は直鎖シリコーン油、並びに粉末を含有する肌用組成物

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