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WO2025115168A1 - Liquide d'inspection fluorescent - Google Patents

Liquide d'inspection fluorescent Download PDF

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Publication number
WO2025115168A1
WO2025115168A1 PCT/JP2023/042894 JP2023042894W WO2025115168A1 WO 2025115168 A1 WO2025115168 A1 WO 2025115168A1 JP 2023042894 W JP2023042894 W JP 2023042894W WO 2025115168 A1 WO2025115168 A1 WO 2025115168A1
Authority
WO
WIPO (PCT)
Prior art keywords
fluorescent
fluorescent dye
inspection
parahydroxybenzoate
preservative
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/JP2023/042894
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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/JP2023/042894 priority Critical patent/WO2025115168A1/fr
Priority to PCT/JP2024/040096 priority patent/WO2025115589A1/fr
Publication of WO2025115168A1 publication Critical patent/WO2025115168A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M3/00—Investigating fluid-tightness of structures
    • G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
    • G01M3/04—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point
    • G01M3/20—Investigating 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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/88—Investigating the presence of flaws or contamination
    • G01N21/91—Investigating 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 sometimes performed on equipment or piping facilities that require a certain degree of airtightness.
  • One method of leak inspection is to use a test liquid that contains a fluorescent dye (hereafter referred to as fluorescent test liquid).
  • JP 2018-132305 A describes a system that supplies a mist containing a fluorescent inspection liquid into a pharmaceutical work chamber to inspect the work chamber for leaks.
  • the above document also describes the use of a solution of riboflavin or riboflavin sodium phosphate as the fluorescent inspection liquid.
  • any fluorescent inspection liquid that leaks from the leaking area must be wiped up by an operator with a rag or similar after the inspection, which poses the problem of labor-intensive cleaning work.
  • the present invention aims to solve the above problems.
  • One aspect of the following disclosure is a fluorescent test solution in which a composition containing a fluorescent dye that is easily decomposed by microorganisms, light, or oxygen and a preservative that prevents the fluorescent dye from spoiling is dissolved in water.
  • the fluorescent inspection liquid of the above aspect prevents deterioration of the fluorescent dye during storage, and once released into the environment, the fluorescent dye decomposes and the fluorescence disappears within a few hours to a few days.
  • the fluorescent inspection liquid of the above aspect can simplify the work of adjusting the fluorescent inspection liquid before a leak inspection and the cleaning work after the leak inspection, making it possible to reduce the labor required for leak inspection.
  • FIG. 1 is a table showing example compositions of the first to sixth fluorescent inspection solutions according to the experimental examples, their fluorescent colors, and the evaluation results of the sewage discharge standards.
  • FIG. 2A is a photograph taken by irradiating the leak location with ultraviolet light during a leak inspection
  • FIG. 2B is a photograph taken one week after the photograph of FIG. 2A was taken by irradiating the leak location with ultraviolet light.
  • the fluorescent inspection liquid according to this embodiment is used, for example, to inspect leaks in piping systems in factories.
  • the fluorescent inspection liquid is sprayed as a mist onto compressed air and introduced into the piping system together with the compressed air.
  • the mist of fluorescent inspection liquid travels with the compressed air to reach each part of the piping. For example, if a part such as a pipe joint becomes loose, compressed air will leak from that part.
  • the fluorescent inspection liquid flows out to the outside from the leaking point such as the pipe joint together with the leaking compressed air, and stains the leaking point with a fluorescent dye.
  • the leaking point stained with the fluorescent inspection liquid can be easily detected visually by shining ultraviolet light such as a black light on it.
  • the above example does not limit the use of the fluorescent inspection liquid to piping systems.
  • the fluorescent inspection liquid can also be used to inspect for leaks in water pipes, food manufacturing equipment, building air conditioning ducts, and other equipment that requires airtightness.
  • the fluorescent inspection liquid can also be added to high-pressure air in the form of a mist, or it can be introduced into pipes as a liquid diluted to a specified ratio.
  • the fluorescent inspection liquid of this embodiment is an aqueous solution in which a fluorescent dye and a preservative are dissolved in water as a solvent.
  • the fluorescent dye is made of a substance that is susceptible to decomposition by microorganisms, decomposition by reaction with oxygen in the air, or decomposition by visible light or ultraviolet light in the environment, and is highly safe for the human body.
  • the fluorescent dye for example, food dyes or substances contained in food are selected depending on the application.
  • a substance that is less irritating to contact with the skin is selected depending on the application.
  • blue fluorescent dyes, green fluorescent dyes, and red fluorescent dyes can be used.
  • the blue fluorescent dye is a dye that absorbs ultraviolet light and emits blue fluorescence in the wavelength range of 360 to 500 nm.
  • Examples of blue fluorescent dyes used in the fluorescent test solution of this embodiment include flavin derivatives, quinine, pyrene, anthocyanin, and umbelliferone, which will be described later. These blue fluorescent dyes may be used alone or in combination.
  • a mixture of quinine and a flavin derivative is suitable because it is safe for the human body and emits a bright, highly visible blue fluorescence.
  • Quinine is used as a bittering agent in soft drinks (tonic water), and is highly safe for the human body even when taken orally, and is also highly biodegradable and decomposable in the atmosphere.
  • the flavin derivative of this embodiment is a derivative that uses riboflavin having a flavin skeleton as a starting material.
  • Such a flavin derivative is, for example, a fluorescent dye obtained by photodecomposing riboflavin, and contains formylmethylflavin and lumichrome as main components.
  • the flavin derivative of this embodiment is obtained by irradiating an aqueous solution of riboflavin with a sufficient amount (time) of light, and emits strong blue fluorescence.
  • the photodecomposition product of riboflavin (vitamin B2) is a substance contained in food, is safe when taken orally, and is a substance that is quickly decomposed in the environment.
  • the green fluorescent dye is a dye that absorbs ultraviolet light and emits green fluorescence in the wavelength range of 500 to 570 nm.
  • green fluorescent dyes include riboflavin (vitamin B2), fluorescein, acridine orange, phloxine B (Red No. 104), and lycopene. These green fluorescent dyes may be used alone or in combination.
  • riboflavin is contained in food as vitamin B2, and is highly safe for the human body and has excellent biodegradability and decomposition in the atmosphere, making it ideal for the fluorescent inspection liquid of this embodiment.
  • Red fluorescent dyes are dyes that absorb ultraviolet light and emit red fluorescence in the wavelength range of 590 to 830 nm.
  • red fluorescent dyes include chlorophyll, rhodamine B, acid red (Red No. 106), eosin, cochineal pigment, tannin, phycocyanin (spirulina pigment), carthamin (safflower pigment), phycoerythrin, erythrosine (Red No. 3), and rose bengal (Red No. 105). These red fluorescent dyes may be used alone or in combination.
  • the fluorescent test liquid may be adjusted to emit blue-green fluorescence by including a blue fluorescent dye and a green fluorescent dye.
  • the fluorescent test liquid may also be adjusted to emit orange or yellow fluorescence by combining a green fluorescent dye with a red fluorescent dye.
  • the fluorescent test liquid may be adjusted to emit pink or purple fluorescence by combining a blue fluorescent dye with a red fluorescent dye.
  • the fluorescent test liquid of this embodiment allows for the appropriate selection of a fluorescent color with the best visibility under the test environment.
  • the preservative prevents deterioration of the fluorescent dye contained in the fluorescent test solution due to putrefaction.
  • Paraoxybenzoic acid esters or isothiazolinone derivatives can be used as the preservative.
  • paraoxybenzoic acid esters may be used as preservatives.
  • paraoxybenzoic acid esters that may be used in the fluorescent test solution include methyl paraoxybenzoate (methylparaben), ethyl paraoxybenzoate (ethylparaben), propyl paraoxybenzoate (propylparaben), isopropyl paraoxybenzoate (isopropylparaben), butyl paraoxybenzoate (butylparaben), isobutyl paraoxybenzoate (isobutylparaben), heptyl paraoxybenzoate (heptylparaben), and benzyl paraoxybenzoate (benzylparaben).
  • the preservative one or a combination of the paraoxybenzoic acid esters listed above may be used.
  • an isothiazolinone derivative may be used as the preservative.
  • the isothiazolinone derivative any one of methylisothiazolinone (MI), methylchloroisothiazolinone (MCI), octylisothiazolinone (OI), dichlorooctylisothiazolinone (DOCI), and benzisothiazolinone (BI), or a combination thereof, may be used.
  • the preservative can be used in a concentration range of 10 ppm or less or 100 ppm or less depending on the application.
  • Methylparaben in a concentration range of 10 ppm or less meets the standards acceptable for use as a food additive and is safe for oral ingestion, making it suitable for use in fluorescent inspection solutions for food processing equipment, for example.
  • Preservatives at 100 ppm or less meet the standards acceptable for pharmaceuticals and medical devices, do not irritate the skin when in contact with it, and can provide a highly safe fluorescent inspection solution.
  • the preservative concentration is 100 ppm or less, the rapid decomposition of the fluorescent dye in the environment after use is not hindered.
  • FIG. 1 is a table showing example compositions of the first to sixth fluorescent test solutions according to the experimental example, their fluorescent colors, and the evaluation results of the sewage discharge standards.
  • the first fluorescent test solution is an aqueous solution containing 27 ppm of riboflavin (vitamin B2) as the first fluorescent dye.
  • the first fluorescent test solution contains 100 ppm of methylparaben as a preservative.
  • the first fluorescent test solution emits a pale yellow fluorescence with a slight greenish tinge.
  • the COD (chemical oxygen demand) and BOD (biochemical oxygen demand), which indicate the degree of water pollution, of the first fluorescent test solution were below the standard value of 160 mg/L for discharge as sewage. It was therefore confirmed that the first fluorescent test solution can be flushed down the sewer.
  • the second fluorescent test liquid is an aqueous solution containing 18 ppm of riboflavin as the first fluorescent dye, 6 ppm of quinine, a blue fluorescent dye, as the second fluorescent dye, and 100 ppm of methylparaben as a preservative.
  • the second fluorescent test liquid emits a yellow-green fluorescence. It was confirmed that the second fluorescent test liquid had COD and BOD both below 160 mg/L and could be flushed down the drain.
  • the third fluorescent test liquid is an aqueous solution containing 27 ppm of riboflavin as the first fluorescent dye and 2.7 ppm of the red fluorescent dye acid red as the second fluorescent dye.
  • the third fluorescent test liquid contains 100 ppm of methylparaben as a preservative.
  • the third fluorescent test liquid emits a slightly reddish yellow fluorescence. It was confirmed that the third fluorescent test liquid had COD and BOD both below 160 mg/L and could be flushed down the drain.
  • the fourth fluorescent test liquid is an aqueous solution containing 20 ppm of a flavin derivative, which is a blue fluorescent dye, as the first fluorescent dye, 7 ppm of quinine, which is a blue fluorescent dye, as the second fluorescent dye, and 100 ppm of methylparaben as a preservative.
  • the fourth fluorescent test liquid emits blue fluorescence. It was confirmed that the fourth fluorescent test liquid had COD and BOD both below 160 mg/L and could be flushed down the drain.
  • the fifth fluorescent test liquid contains 123 ppm of the red fluorescent dye rhodamine B as the first fluorescent dye, and 100 ppm of methylparaben as a preservative.
  • the fifth fluorescent test liquid emits orange (yellowish red) fluorescence. Both the COD and BOD of the fifth fluorescent test liquid were below 160 mg/L, and it was confirmed that it can be poured into the sewer.
  • the sixth fluorescent test liquid contains 210 ppm of the red fluorescent dye acid red as the first fluorescent dye, and 100 ppm of methylparaben as a preservative.
  • the sixth fluorescent test liquid emits red fluorescence. Both the COD and BOD of the sixth fluorescent test liquid were below 160 mg/L, and it was confirmed that it can be poured into the sewer.
  • a mist of fluorescent test liquid was supplied along with compressed air to a test pipe with loose joints that could become leak points.
  • a fluorescent test liquid was used that contained riboflavin as the fluorescent dye at a concentration of 5 ppm and methyl paraoxybenzoate as a preservative at a concentration of 10 ppm.
  • fluorescent test liquid is leaking from a pipe joint.
  • Ultraviolet light from a black light is irradiated onto the leaking area.
  • bright fluorescence is emitted from the leaked fluorescent test liquid, making the leaking area easily visible.
  • One aspect of the disclosure is a fluorescent inspection solution obtained by dissolving in water a composition containing a fluorescent dye that is easily decomposed by microorganisms, light or oxygen and a preservative that prevents the fluorescent dye from spoiling.
  • the fluorescent inspection solution can prevent the deterioration of the fluorescent dye during storage.
  • the preservative may contain a paraoxybenzoic acid ester or an isothiazolinone derivative. After this fluorescent inspection liquid is released into the environment, the fluorescent dye is decomposed and the fluorescence disappears within a few hours to a few days.
  • the fluorescent inspection liquid of the above aspect can simplify the adjustment work of the fluorescent inspection liquid before a leak inspection and the cleaning work after the leak inspection, making it possible to reduce the labor required for the leak inspection.
  • the preservative may include at least one of methyl paraoxybenzoate, ethyl paraoxybenzoate, propyl paraoxybenzoate, isopropyl paraoxybenzoate, butyl paraoxybenzoate, isobutyl paraoxybenzoate, heptyl paraoxybenzoate, and benzyl paraoxybenzoate.
  • This fluorescent inspection liquid is excellent in safety to the human body because the preservative is less irritating to the human body.
  • the preservative may include at least one of methylisothiazolinone and methylchloroisothiazolinone.
  • This fluorescent inspection liquid has excellent anti-corrosive properties for the fluorescent dye and is relatively low in irritation to the human body.
  • the fluorescent inspection liquid according to any one of appendices 1 to 4 may contain the preservative at a concentration of 100 ppm or less. This fluorescent inspection liquid is less irritating to human skin, and the preservative does not hinder decomposition of the fluorescent dye in the environment.
  • the fluorescent dye may include at least one of quinine, pyrene, anthocyanin, umbelliferone, and a flavin derivative derived from riboflavin having a flavin skeleton, and may include a blue fluorescent dye that emits blue fluorescence when irradiated with ultraviolet light.
  • This fluorescent test solution can further obtain blue or bluish fluorescence, and can realize various fluorescent colors by mixing with fluorescent dyes of other colors.
  • the fluorescent dye may include at least one of riboflavin, fluorescein, acridine orange, phloxine B, and lycopene, and may include a green fluorescent dye that emits green fluorescence when irradiated with ultraviolet light.
  • This fluorescent inspection liquid can further obtain green or greenish fluorescence, and can realize various fluorescent colors by mixing with fluorescent dyes of other colors.
  • the fluorescent dye includes at least one of chlorophyll, rhodamine B, acid red, eosin, cochineal dye, tannin, phycocyanin, carthamin, phycoerythrin, erythrosine, and rose bengal, and may include a red fluorescent dye that emits red fluorescence when irradiated with ultraviolet light.
  • This fluorescent inspection liquid further provides red or reddish fluorescence, and can realize various fluorescent colors by mixing with fluorescent dyes of other colors.

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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, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Examining Or Testing Airtightness (AREA)

Abstract

Ce liquide d'inspection fluorescent est obtenu par dissolution, dans de l'eau, d'une composition qui contient : un fluorochrome qui est facilement décomposé par des micro-organismes, de la lumière ou de l'oxygène ; et un conservateur qui empêche la putréfaction du fluorochrome. Le conservateur contient un ester d'acide parahydroxybenzoïque ou un dérivé d'isothiazolinone.
PCT/JP2023/042894 2023-11-30 2023-11-30 Liquide d'inspection fluorescent Pending WO2025115168A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PCT/JP2023/042894 WO2025115168A1 (fr) 2023-11-30 2023-11-30 Liquide d'inspection fluorescent
PCT/JP2024/040096 WO2025115589A1 (fr) 2023-11-30 2024-11-12 Liquide d'inspection par fluorescence

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2023/042894 WO2025115168A1 (fr) 2023-11-30 2023-11-30 Liquide d'inspection fluorescent

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WO2025115168A1 true WO2025115168A1 (fr) 2025-06-05

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PCT/JP2024/040096 Pending WO2025115589A1 (fr) 2023-11-30 2024-11-12 Liquide d'inspection par fluorescence

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10221196A (ja) * 1997-02-10 1998-08-21 Tokyo Denki Komusho:Kk 多管形熱交換器の漏洩管の検知方法、多管形熱交換器の漏洩管の検知用布帛、多管形熱交換器の漏洩管の検知用検出剤及び多管形熱交換器の漏洩管の検知用下地
JP2004002358A (ja) * 2002-04-01 2004-01-08 Rohto Pharmaceut Co Ltd 眼科用組成物
JP2007056014A (ja) * 2005-07-29 2007-03-08 Santen Pharmaceut Co Ltd ゲル状組成物を用いた後眼部組織への非侵襲性ドラッグデリバリーシステム
JP2007167266A (ja) * 2005-12-21 2007-07-05 Lion Corp 歯垢検出システムおよび歯垢検出方法
WO2014157703A1 (fr) * 2013-03-29 2014-10-02 国立大学法人三重大学 Tache vitale
JP2020511485A (ja) * 2017-03-20 2020-04-16 トータル・マーケティング・サービシーズ 治療的使用のための炭化水素油

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10197386A (ja) * 1996-12-20 1998-07-31 Fr Des Amortisseurs De Carbon:Soc 加圧された液圧ダンパ管からの流体の漏れを検出する方法
JP2000308669A (ja) * 1999-04-27 2000-11-07 Otsuka Pharmaceut Factory Inc 重炭酸塩含有薬液容器包装体
JP2005220045A (ja) * 2004-02-04 2005-08-18 Konica Minolta Medical & Graphic Inc 蛍光造影剤

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10221196A (ja) * 1997-02-10 1998-08-21 Tokyo Denki Komusho:Kk 多管形熱交換器の漏洩管の検知方法、多管形熱交換器の漏洩管の検知用布帛、多管形熱交換器の漏洩管の検知用検出剤及び多管形熱交換器の漏洩管の検知用下地
JP2004002358A (ja) * 2002-04-01 2004-01-08 Rohto Pharmaceut Co Ltd 眼科用組成物
JP2007056014A (ja) * 2005-07-29 2007-03-08 Santen Pharmaceut Co Ltd ゲル状組成物を用いた後眼部組織への非侵襲性ドラッグデリバリーシステム
JP2007167266A (ja) * 2005-12-21 2007-07-05 Lion Corp 歯垢検出システムおよび歯垢検出方法
WO2014157703A1 (fr) * 2013-03-29 2014-10-02 国立大学法人三重大学 Tache vitale
JP2020511485A (ja) * 2017-03-20 2020-04-16 トータル・マーケティング・サービシーズ 治療的使用のための炭化水素油

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Publication number Publication date
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