EP2622320A1 - Procédé de détection d'un fluide ayant traversé une couche par perméation - Google Patents

Procédé de détection d'un fluide ayant traversé une couche par perméation

Info

Publication number
EP2622320A1
EP2622320A1 EP11764163.9A EP11764163A EP2622320A1 EP 2622320 A1 EP2622320 A1 EP 2622320A1 EP 11764163 A EP11764163 A EP 11764163A EP 2622320 A1 EP2622320 A1 EP 2622320A1
Authority
EP
European Patent Office
Prior art keywords
fluid
cellulose
layer
reactive dye
red
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.)
Withdrawn
Application number
EP11764163.9A
Other languages
German (de)
English (en)
Inventor
Ezio Gandin
Claude Dehennau
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.)
Solvay SA
Original Assignee
Solvay SA
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 Solvay SA filed Critical Solvay SA
Priority to EP11764163.9A priority Critical patent/EP2622320A1/fr
Publication of EP2622320A1 publication Critical patent/EP2622320A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
    • G01N15/082—Investigating permeability by forcing a fluid through a sample
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
    • G01N2015/0846—Investigating permeability, pore-volume, or surface area of porous materials by use of radiation, e.g. transmitted or reflected light
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
    • G01N2015/086—Investigating permeability, pore-volume, or surface area of porous materials of films, membranes or pellicules

Definitions

  • the invention pertains to a method for detecting the permeation of a fluid through a layer, in particular through a polymer layer, and to the use of this method for determining the map of the permeability coefficient of such layer.
  • the permeation phenomenon is related to the penetration and transport of a permeate, i.e. of a fluid such as a liquid, gas, or vapour through a solid, and is related to a material's intrinsic permeability.
  • This intrinsic permeability is strictly related to inherent (micro)structure of the material; in particular, in case of polymer materials, permeability is related to the actual composition of the material (e.g. to the presence of fillers and additives, their amount and distribution), to the nature of polymer chains and their relevant molecular parameters, including crystalline fraction and habits, as well as to the overall layout of the article penetrated by the fluids, i.e. it is sensitive to defects, voids and other ex- processing features.
  • US 2003003589 POTONIC BIOSYSTEMS INC 2/01/2003 discloses a method for detecting and measuring volatile acid or basic components by means of an indicator film having an indicator dye embedded therein, such that said dye undergoes a colour change inducing modification of spectral properties upon exposure to the component to be detected.
  • This method is notably taught as applicable for detecting holes and defects in objects or materials wherein said coating can be applied on one side and the fluid, ammonia, for instance, on the other side.
  • fluorescence measurements are not easy techniques to be used and required the material itself to be submitted to the spectral measurement. This method cannot thus be applied to objects and articles of complex geometry, and or which cannot be easily handled or moved.
  • the present invention pertains to a method for detecting the permeation of a fluid through a layer having a first surface (S1) and a second surface (S2), wherein said fluid is contacted with said first surface (S1) and wherein a coating composition comprising a reactive dye is applied to said second surface (S2) to yield a reactive dye coating onto said surface (S2), wherein said reactive dye coating undergoes a colour change when contacted with said fluid, said method comprising:
  • RGB colour model to said image to determine the red (R ), green (G) and blue (B) coordinates of at least one point of said image
  • Figure 1 shows a calibration curve useful for applying the method in
  • Figure 2 shows the results of a test on how ammonia permeates through a certain PVDF layer : a plot of the concentration of ammonia as a function of time was determined in accordance with the method according to the present invention, wherein in abscissa the time is expressed in hours, while in ordinates, concentration of ammonia in ppm is provided.
  • the method also advantageously enables detecting the permeation of said fluid through selected areas of the layer under investigation.
  • said surface can be divided in 'pixels' of well defined dimensions, each of said pixel being thus possibly associated to a value of concentration of permeating fluid, and hence to a value of permeability coefficient.
  • a mapping of the permeation of the fluid through the layer can be notably advantageously obtained, which can enable, e.g., identification of inhomogeneities in thickness of such layer or other structural local defects.
  • the method can be advantageously used for establishing a map of permeation of the fluid through said layer.
  • polymer layer will be submitted to the method of the invention.
  • polymers whose layers might be submitted to the method of the invention mention can be notably made of elastomeric and thermoplastic polymers, in particular of polyolefins, aromatic and aliphatic polyamides, polyetherketones, polysulphones, halopolymers, including chlorinated polymers (PVC, PVDC) and fluoropolymers (PVDF, PTFE, ECTFE, ETFE, PFA, MFA).
  • the layer may have whichever geometry.
  • the layer might be comprised in articles intended to confine fluids, like, notably, enclosures, bottles, recipients, pipes, tubings and the like, or can be a (part of) a substantially bidimensional article, i.e. a film or a sheet.
  • the method of the invention can be used to determine permeation of
  • hazardous and non hazardous gases such as, notably, ammonia, carbon monoxide, chlorine, arsine, diborane, dimethylamine, fluorine, formaldehyde, hydrogen chloride, hydrogen cyanide, hydrogen fluoride, hydrazine, methylamine, methyl hydrazine, nitric acid, nitrogen dioxide, phosgene, phosphine, sulfur dioxide, trimethylamine hydrogen sulfide (F S) and hydrogen (Kb), and carbon dioxide, water vapour, nitrogen; and hydrocarbon vapours such as benzene, toluene, alkanes, alcohols like methanol, ethanol.
  • hazardous and non hazardous gases such as, notably, ammonia, carbon monoxide, chlorine, arsine, diborane, dimethylamine, fluorine, formaldehyde, hydrogen chloride, hydrogen cyanide, hydrogen fluoride, hydrazine, methylamine, methyl hydrazine, nitric acid, nitrogen dioxide, pho
  • the fluid can be a liquid, preferably a low boiling liquid, such as notably water, hydrogen peroxide, organic solvents, and the like.
  • the reactive dye coating is designed and dimensioned to be gas and liquid permeable so as to allow the fluids to contact the reactive dye held within the coating matrix.
  • the reactive dye comprised in the reactive dye coating is advantageously selected from a group of compounds that change colour perceptibly in response to the presence, interaction with, or binding to the fluid; as a consequence, RGB coordinates of reactive dye in the presence or in the absence of the fluid are modified. It is also understood that the reactive dye might be coloured when kept in the absence of said fluid or can be colourless, in said conditions. Similarly, the reactive dye might be coloured or colourless when in the presence, interaction with or binding to the fluid. As a consequence, the colour change, as above mentioned can be a change from colourless to coloured, from coloured to colourless or may be, more often, a change between two different colours.
  • the reactive dye used can be tailored to the specific environment, the fluid to be detected and other factors, well known to the skilled in the art. Any reactive dye that is known in the industry can be used so long as a colour change occurs in response to the presence, interaction with, or binding to the fluid which permeation should be detected.
  • the group of useful reactive dyes generally comprises: transition metal oxides, permanganate salts such as silver permanganate and potassium permanganate, chromate salts such as sodium dichromate, metal hydroxides, including notably Copper hydroxide, metal carbonates, metal sulfates such as tribasic lead sulfate and copper sulfate, metal chlorides such as cobalt chloride and mercury chloride, cobalt bromide, silver nitrate, tetrephenylporphyrin, a metal complex of tetrephenylporphyrin, lead acetate, uranine, gold complexes, indophenol sodium salt, sodium salt of the leuco sulfuric derivative of Vat Green 1 , phosphomolybdic acid, and organic indicator compounds.
  • transition metal oxides such as silver permanganate and potassium permanganate
  • chromate salts such as sodium dichromate
  • metal hydroxides including notably Copper hydroxide, metal carbonates, metal sul
  • coating are generally selected from the group comprising: scandium oxide, titanium dioxide, chromium(ll) oxide, chromium(IV) oxide, manganese oxide, manganese(IV) oxide, iron(lll) oxide, cobalt(ll) oxide, nickel(lll) oxide, zirconium dioxide, niobium(V) oxide, technetium oxide, ruthenium(IV) oxide, palladium(ll) oxide, silver(ll) oxide, lutetium(lll) oxide, hafnium(IV) oxide, tantalum(V) oxide, rhenium trioxide, rhenium(VII) oxide, osmium tetroxide, vanadium(V) oxide, tungstic oxide, molybdenum oxide, molybdenum dioxide, yttrium oxide, and combinations thereof.
  • the transition metal oxide pigments may also be combined with a catalyst to facilitate the reaction of the metal oxide with hydrogen or hydrogen sulfide.
  • the catalysts may be selected from the group comprising platinum, palladium, rhodium, nickel, combinations of these metals, or alloys of these metals with other metals such as copper, cobalt, iridium,
  • magnesium calcium, barium, strontium, and combinations thereof.
  • anthraquinone dye anthraquinone dye with alkylammonium salts, methyl orange, bromocresol green, methyl red, bromocresol purple, bromothymol blue, phenol red, bromothymol purple, thymol blue, bromophenol blue, methylene red, bromophenol red, bromocresol green, tetraiodophenolphthalein,
  • the reactive dye coating it is generally preferred for the reactive dye coating to possess a
  • the coating composition may further comprise a polymer binder
  • the polymer binder can be notably selected from the group consisting of polytetrafluoroethylene (PTFE), polyvinylidene fluoride (PVDF),
  • ECTFE ethylene/chlorotrifluoroethylene
  • ETFE ethylene/tetrafluoroethylene copolymers
  • polyamides polyacrylamides, polyacrylate, polyalkylacrylates, polystyrenes, polynitriles, polyvinyls, polyvinylchlorides, polyvinyl alcohols, polydienes, polyesters, polycarbonates, polysiloxanes, polyurethanes, polyolefins, polyimides, cellulosic polymers, including ester and ether derivatives, like notably Cellulose triacetate, Cellulose
  • the polymer binder can be selected from thermosetting resins; these resins might be lead to coating
  • thermosetting resins available from renewable sources can be used when limiting environmental impact is required.
  • the selection of the polymer binder will be made also having regards to the chemical nature of the layer to be submitted to the method of the invention.
  • polymer layer it is generally understood that the selection of the polymer binder will be made so as to generally ensure that the polymer binder and the polymer of the layer are compatible with each other; this requirement is considered to advantageously ensure increased adhesion and interaction between the reactive dye coating and the layer.
  • the coating composition may further include other ingredients such as solvents and fillers.
  • Solvents dissolve or disperse constituents of the coating composition, resulting in a liquid mixture that may be applied as a liquid to the surface (S2) as above detailed by standard coating techniques, like casting, spin coating, curtain coating, roll coating, air knife coating, metering rod coating.
  • the solvents are generally selected to have a low boiling point and
  • aromatic solvents like notably benzene, toluene, xylenes
  • alcohols in particular methanol, ethanol, propanols
  • Fillers may also be added, in addition to the other constituents of the
  • Fillers may be selected from the group comprising: glass flake, glass flake coated with silver, hollow glass spheres, solid glass spheres, talc, fibrous talc, lime, calcium carbonate, barite, clay, gypsum, chalk dust, marble dust, fumed silica, amorphous silica, glass fibres, zeolite, and mica.
  • Various other thickeners, stabilizers, emulsifiers, texturizers, adhesion promoters, de-glossing agents and combinations thereof can also be used. Any of a variety of constituents may be used to form the reactive coating composition so long as an adequate coating is formed that can be placed on the surface (S2) with adhesion.
  • the surface (S2) of the layer is preliminary treated for ensuring increased adhesion to the reactive dye coating.
  • the surface (S2) of the layer is preliminary treated for ensuring increased adhesion to the reactive dye coating.
  • the reactive coating composition is deposited onto surface (S2) as a film, with the reactive dye incorporated therein.
  • the method of the invention comprises obtaining an image of at least a portion of said second surface (S2), as above detailed.
  • Said image can be obtained by conventional techniques; either traditional camera or digital camera can be used, being understood that in former case further treatment with suitable software will be required for applying RGB colour model to said image to determine the red (R ), green (G) and blue (B) coordinates of at least one point of said image.
  • RGB colour model may be integrated in data acquisition of the camera itself, so that output of the same can already be a set of RGB coordinates for each section (pixel) of the image, according to the chosen resolution.
  • the RGB coordinates of said at least one point are then compared with the RGB coordinates of a reference colour. This can be achieved by various means for obtaining a quantitative comparison. It may be useful, for instance, to determine the spectral distance between said at least one point having spectral coordinates (R p , G p and B p ) and said reference colour (Rref, Gref, B re f) according to formula:
  • the method of the invention can be notably applied for determining fluids transport coefficients through layers, and more particularly through polymer layers.
  • surface (S2) can provide for the amount Q of fluid actually permeating through the layer from surface (S1) to surface (S2). This amount can be monitored in time (t) as a function of temperature, concentration and/or pressure (p) of the fluid contacting surface (S1).
  • the permeability or permeability coefficient Pe is generally defined as follows:
  • Q is the flux of fluid through the layer
  • I is the thickness of said layer
  • a ⁇ p is the so-called potential difference between both sides of the layer.
  • This potential ⁇ can be a pressure, a mass concentration or a molar concentration.
  • Pe is the permeability coefficient
  • Q is the volume of gas permeated through the layer at time t
  • I is the thickness of the layer
  • A is the diffusion area exposed to said gas, through which the same
  • D diffusion coefficients
  • S solubility coefficient
  • the method also enables determining such coefficients (Pe, D, S) for each of defined area of the layer under investigation, as above detailed.
  • a permeability mapping can thus be established by appropriate
  • a coating composition was prepared by mixing:
  • Said composition was used for coating a film made from SOLEF(R) 1008 VDF homopolymer, commercially available from Solvay Solexis, having a thickness of 16 pm.
  • ammonia was selected, fed through a bubbling system LENZ of inner volume of 100 ml though a metering device Bronkhorst to a measuring cell exposed to a scanner EPSON PERFECTION V750 PRO. Concentration of ammonia was made to vary between 2 ppm and 10 ppm as a function of time; after each pulse of ammonia, enough time was left to the system for desorbing ammonia and recovering initial status of the reactive dye.
  • Figure 1 shows the correlation established between the concentration of ammonia in ppm (in abscissa) and the distance in the RGB space from original point.
  • a vial having an inner volume of 12 ml was filled with 5 ml of a saturated ammonia aqueous solution and was capped by means of the coated PVDF layer as above mentioned, retained by means of aluminium caps, letting a surface of about 0.5 cm 2 exposed.
  • RGB coordinated as a function of time were thus determined and their distance from the reference point (recorded on the coated film before exposure to ammonia) determined.
  • a plot of the concentration of ammonia as a function of time was determined; such plot is reproduced in Figure 2, wherein in abscissa the time is expressed in hours, while in ordinates, concentration of ammonia in ppm is provided. From these data, permeability coefficient can be notably determined by simple correlation, on the basis of calibration data.

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Dispersion Chemistry (AREA)
  • Biophysics (AREA)
  • Molecular Biology (AREA)
  • Paints Or Removers (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)

Abstract

Cette invention concerne un procédé permettant de détecter et de mesurer la perméation d'un fluide à travers une couche ayant une première surface (S1) et une seconde surface (S2). Le fluide est en contact avec ladite première surface (S1) et une composition de revêtement comprenant un colorant réactif est appliquée à ladite seconde surface (S2) pour former un revêtement à base d'un colorant réactif sur ladite surface (S2), ledit revêtement à base d'un colorant réactif subissant un changement de couleur quand il entre en contact avec ledit fluide. Le procédé selon l'invention comprend : - l'obtention d'une image d'au moins une partie de ladite seconde surface (S2); - l'application du modèle de couleur RVB à ladite image pour déterminer les coordonnées du rouge (R), du vert (V) et du bleu (B) d'au moins un point de ladite image; - la comparaison des coordonnées RVB dudit point aux coordonnées RVB d'une couleur de référence; et - la mise en corrélation de ladite comparaison à la concentration du liquide de perméation sur la surface (S2).
EP11764163.9A 2010-10-01 2011-09-29 Procédé de détection d'un fluide ayant traversé une couche par perméation Withdrawn EP2622320A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP11764163.9A EP2622320A1 (fr) 2010-10-01 2011-09-29 Procédé de détection d'un fluide ayant traversé une couche par perméation

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP10185828 2010-10-01
PCT/EP2011/066957 WO2012041945A1 (fr) 2010-10-01 2011-09-29 Procédé de détection d'un fluide ayant traversé une couche par perméation
EP11764163.9A EP2622320A1 (fr) 2010-10-01 2011-09-29 Procédé de détection d'un fluide ayant traversé une couche par perméation

Publications (1)

Publication Number Publication Date
EP2622320A1 true EP2622320A1 (fr) 2013-08-07

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Country Status (3)

Country Link
EP (1) EP2622320A1 (fr)
TW (1) TW201229483A (fr)
WO (1) WO2012041945A1 (fr)

Cited By (1)

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CN112740014A (zh) * 2018-09-03 2021-04-30 五松尖端医疗产业振兴财团 测量水分透过率和透光率的基于图像处理的系统及用该系统测量水分透过率和透光率的方法

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DE102015213974B4 (de) * 2015-07-23 2017-04-06 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Anordnung zur Bestimmung der Permeationsrate einer Probe
CN113237821B (zh) * 2021-04-26 2023-03-10 江西科技师范大学 一种应用于氧化性高温氯腐蚀环境的钇掺杂Inconel625合金的制备及检测方法

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JPH01307635A (ja) * 1988-06-03 1989-12-12 Hamamatsu Photonics Kk 被試験用薄膜の物質透過性能を評価する方法
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CN112740014A (zh) * 2018-09-03 2021-04-30 五松尖端医疗产业振兴财团 测量水分透过率和透光率的基于图像处理的系统及用该系统测量水分透过率和透光率的方法

Also Published As

Publication number Publication date
TW201229483A (en) 2012-07-16
WO2012041945A1 (fr) 2012-04-05

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