EP1828750A1 - Dispositif pour detecter au moins un constituant chimique - Google Patents

Dispositif pour detecter au moins un constituant chimique

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Publication number
EP1828750A1
EP1828750A1 EP05823844A EP05823844A EP1828750A1 EP 1828750 A1 EP1828750 A1 EP 1828750A1 EP 05823844 A EP05823844 A EP 05823844A EP 05823844 A EP05823844 A EP 05823844A EP 1828750 A1 EP1828750 A1 EP 1828750A1
Authority
EP
European Patent Office
Prior art keywords
detection layer
detected
component
layer
polyacrylic acid
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Withdrawn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
EP05823844A
Other languages
German (de)
English (en)
Inventor
Stefan Dick
Mandy Erdmann
Inge KRÄMER
Michael Haubs
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.)
Sued Chemie AG
Original Assignee
Sued Chemie AG
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 Sued Chemie AG filed Critical Sued Chemie AG
Publication of EP1828750A1 publication Critical patent/EP1828750A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • 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
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • 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
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • G01N21/81—Indicating humidity
    • 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
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
    • G01N21/45—Refractivity; Phase-affecting properties, e.g. optical path length using interferometric methods; using Schlieren methods
    • 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

Definitions

  • the invention relates to a device for detecting at least one chemical component, in particular of water or water vapor, wherein a component which swells in the presence of the chemical component to be detected is used in a detection layer.
  • the capacitive sensors are based on dielectric change of thin layers in the case of water vapor absorption.
  • the properties of these sensors are determined by the hygroscopic material and the electrode geometry.
  • a layer arrangement has proven itself.
  • a sequence of layers arranged on one another is located on a substrate surface, consisting of a base electrode, a layer sensitive to water vapor, and a cover electrode.
  • Resistance humidity sensors are devices that display humidity in impedance changes. This can be measured with current, voltage or resistance. Ceramic materials are particularly well suited because they have very good properties in terms of their mechanical adhesion, reproducibility, durability, ease of handling and resistance to environmental influences. Disadvantages of ceramic moisture sensors are the effects of hysteresis and atmospheric phenomena, especially at high moisture concentrations.
  • An electrolytic humidity sensor is essentially a moisture meter that works on the basis of lithium chloride probes. It uses two properties of LiCl. On the one hand, LiCl is hygroscopic, that is, it adsorbs water molecules, and on the other hand, the resulting saline solution is an electrolyte that conducts the electric current.
  • LiCl-based electrolyte humidity sensors A major disadvantage of LiCl-based electrolyte humidity sensors is their relatively slow response time. But also they should not be used in a very humid environment as this will negatively affect the precision and lifetime of the sensor. Particularly disadvantageous here are the aging effects of the sensor due to the crystal formation of the LiCl.
  • the most common gravimetric humidity sensor is the Quartz Crystal Microbalance (QCM). Piezoelectric quartz thin plates have resonance frequencies (thickness and / or shear mode) in the MHz range. Coated with a hygroscopic layer, the frequency change is used to measure the humidity. When using a non-coated reference resonator, the lateral sensitivity of pressure and temperature can be minimized.
  • QCM Quartz Crystal Microbalance
  • the physical background of the optical humidity sensor is a harmonic electromagnetic wave with the amplitude E 0 , the frequency ⁇ and the phase ⁇ :
  • Humidity information can be obtained by the amplitude, polarization, frequency or phase of the wave.
  • Another possibility of use makes use of the absorption wavelength of water: when light passes through gas, the absorption of certain wavelengths provides information about the composition.
  • Color hygrometers consist of a series of different scale plates of cellulose pulp mixed with salts of, for example, cobalt (II) compounds, copper sulfate, copper chloride or nickel chloride are drunk.
  • salts of, for example, cobalt (II) compounds, copper sulfate, copper chloride or nickel chloride are drunk.
  • a major disadvantage of these color hygrometers is the use of heavy metal salts.
  • the present invention thus relates in one aspect to an apparatus for detecting at least one chemical component comprising a light-reflecting substrate or a light-reflecting background and an overlying detection layer comprising at least one component swellable in the presence of the component to be detected, wherein. the chemical component to be detected comes into contact with the detection layer and the detection layer can change its layer thickness by interaction with the chemical components to be detected, whereby the color of the detection ons Mrs changes in the reflected light.
  • the chemical component to be detected is particularly preferably water or water vapor. It has thus been found that the devices described herein are particularly suitable for the detection of water or water vapor. "Water or water vapor" is intended to encompass both liquid water or water in liquid media, and in particular water in the gaseous state or in gaseous media such as air.
  • the detection layer contains on the one hand at least one component which can swell in the presence of the chemical component to be detected, but on the other hand not as described by Kleinfeld and Ferguson (loc. Cit.), consists of an inhomogeneous material.
  • This result was all the more surprising since in the above reference by Kleinfeld and Ferguson the synthetic exfoliated hectorite arranged in layers or layers is described as an essential element of the swellable detection layer.
  • the use of a homogeneous material as a detection layer both the response times, i. the delay to a detectable color change, the color intensity, and / or the Nachquellzeit the detection layer positively influences.
  • a homogeneous material is thus particularly preferred as the detection layer.
  • a homogeneous material is understood as meaning a material which either contains only one component or, if two or more components are contained, these are distributed or mixed uniformly (homogeneously) in the layer. This should be the same over the entire layer thickness Refractive index of the detection layer can be ensured.
  • a homogeneous distribution can be ensured in a conventional manner, for example by intensive mixing of the components prior to the generation of the detection layer.
  • a multi-layered structure of the detection layer of layers with different refractive index and different composition as Kleinfeld and Ferguson (loc. Cit.) Is deliberately avoided. It has been found that both the response times, the color intensity and the after-swelling time of the detection layer can be positively influenced.
  • the detection layer further contains no platelet-shaped layer silicates. It is believed, without the invention being limited to the correctness of this assumption, that the presence of platelet-shaped substances, such as synthetic hedetite, prolongs the diffusion paths for the substance to be detected into the detection layer or within the detection layer. Flake-form phyllosilicates as such are familiar to the person skilled in the art and need not be explained in more detail here. In other words, it is believed that the platelet-shaped layered silicate particles constitute (diffusion) barriers for the substance to be detected, so that the homogeneous swelling of the detection layer is impeded or retarded upon accommodation of the component to be detected.
  • both the response time of the detection layer until reaching a detectable color change and the time delay until a defined final swelling has been reached under certain conditions can be extended. Accordingly, the time is extended until a final color change, which can not be changed by a subsequent swelling of the layer, can be read off. It is also possible that the subsequent redistribution of the detected chemical component between the platelike phyllosilicate (synthetic hectorite) and the polyelectrolyte (PDDA) is followed by a subsequent change in the layer thickness under constant environmental conditions. Since such a subsequent change in the layer thickness in turn impedes or delays the readability of a definitive color change at a certain concentration of the chemical component to be detected in the environment, this is disadvantageous. According to a preferred embodiment, therefore, the detection layer or the layers arranged on the light-reflecting substrate do not contain platelet-shaped layer silicates such as hectorite or the like.
  • the detection layers or devices without synthetic hectorite without platelet-shaped phyllosilicates according to the invention enable a rapid and homogeneous uptake of the chemical component to be detected into the detection layer.
  • the detection layer generally contains no particulate components, since the best results have been achieved. Especially, particulate components, even if they have no platelet shape, often have a negative impact on the achievable response and NachquellZeiten and the color intensities.
  • the detection layer and / or the device as a whole also contains no dye (dye), in particular no so-called "bronzing dye”.
  • the detection layer contains at least one component which can swell in the presence of the component to be detected (detection component), wherein the detection layer can change its layer thickness by interaction with the chemical components to be detected, so that the color of the detection layer changes in the reflected light.
  • detection component component which can swell in the presence of the component to be detected
  • the detection layer can change its layer thickness by interaction with the chemical components to be detected, so that the color of the detection layer changes in the reflected light.
  • detection component which are able to absorb the chemical component to be detected and thereby to change their volume, ie to sources.
  • the "uptake” can take place, for example, by adsorption, absorption or other physical or chemical mechanisms of uptake / storage.
  • the suitability of substances as detection substances in the context of the present invention can easily be routinely determined on the basis of the absorption or swelling capacity of the substance.
  • 5 g of the substance to be examined are weighed into a Petri dish.
  • the samples are dried at room temperature in a vacuum drying cabinet (100 mbar, membrane pump) to constant mass.
  • the drying temperature can be increased depending on the detection component (for example in the case of polyacrylic acid to about 70 ° C.), as long as this does not lead to the destruction of the detection component.
  • the Petri dishes with the dried substance are then transferred into a climatic chamber at 25 ° C., 40% relative humidity or 40% saturation with the component to be detected in the gas phase and the weight increase (adsorption of the component to be detected) is determined (to constant mass). , This results in a percentage absorption capacity for the component to be detected in% by weight based on the detection component.
  • the detection layer accordingly contains at least one component which swells in the presence of the component to be detected and has a capacity for the component to be detected (as determined above) of from 10 to 30% by weight, in particular from 15 to 27% by weight. %, preferably from 18 to 25 wt .-% based on the amount used.
  • a capacity for the component to be detected (as determined above) of from 10 to 30% by weight, in particular from 15 to 27% by weight. %, preferably from 18 to 25 wt .-% based on the amount used.
  • the at least one component swellable in the presence of the chemical component to be detected comprises at least one salt of a polyacid or polymeric acid.
  • polyacid or polymeric acid is familiar to the person skilled in the art.
  • polyacid or “polymeric acid” is meant any polymer comprising monomer units having at least one acid function, in particular at least one carboxylic acid group.
  • Such polyacids or polymeric acids can be used particularly well in the form of their salts for highly sensitive devices for the detection of water or water vapor.
  • the polymer contains more than 10, in particular more than 50, more preferably more than 100 monomer units.
  • the hydrophilicity of the detection layer can be optimally adjusted.
  • a particularly good swelling capability is provided.
  • Very thin detection layers are advantageously made possible which respond very sensitively and rapidly even to low moisture contents of a gaseous medium.
  • the salts of the polyacids are particularly preferably alkali metal salts. As alkali ions Na + , K + and / or Li + are particularly preferred.
  • the molar ratio of alkali metal ions to polyacid (or polymeric acid) is between 50 and 6500, in particular between 150 and 6500, more preferably between 300 and 6500.
  • the at least one component swellable in the presence of the chemical component to be detected consists essentially or completely of at least one salt of at least one polyacid, preferably at least one polyacrylic acid, in particular at least one alkali metal salt of at least one polyacrylic acid. It is particularly preferred that the at least one swellable in the presence of the chemical component to be detected component or the detection layer itself to more than 50 wt .-%, preferably more than 75 wt .-%, more preferably more than 90 wt - preferably more than 95% by weight, more preferably more than 98 or even 99% by weight or more, of at least one salt of at least one polyacid, preferably at least one polyacrylic acid.
  • the at least one salt of a polyacrylic acid is a completely or partially neutralized polyacrylic acid.
  • the degree of neutralization can be easily determined by titration and the creation of titration curves. Preference is given in particular to polyacrylic acids which are partly or completely neutralized with the aid of alkali metal hydroxides or alkali metal carbonates, preferably from 5 to 70%, more preferably from 10 to 60%, in particular from 15 to 50%.
  • the polyacid used (in particular polyacrylic acid) or its salt has a pH of between about 3 and 7, in particular between about 5 and 7.
  • the determination of the pH can be carried out in the usual way on the basis of the solution of the polyacid salt used for the preparation of the detection layer, for example as described in more detail below using an aqueous solution with a pH meter.
  • the following substances have proven to be particularly suitable detection components: salts of polyacids such as methacrylic acid, glutamic acid, polyacrylic acid, or salts of amine-containing polymers such as polyethyleneamine. But also substances such as water glass, polyphosphates, proteins, copolymers such as block copolymers (eg PO / EO block polymers), graft copolymers (such as PO-G-PEO) as well as random or alternating copolymers (as literature to Copmmermeren which can be tested for their suitability in the context of the present invention by means of routine experiments can be referred, for example, to: Houben-Weyl, Methods of Organic Chemistry, 4th edition, ed.: Eugen Müller, Chapter 1); sulfonated polystyrene, polyvinyl caprolactam or cellulose acetate have proven to be suitable. It has proved to be particularly advantageous if the detection layer consists essentially or completely of the detection component. Also mixtures of
  • hydrophilic polymers preferably selected from the polyacrylic acids and their salts
  • hydrophilic polymers are particularly suitable detection components for the detection layer. and lead to devices with very high color intensities, low response and Nachquell consultants. Also, good adherent films can be produced on most light-reflecting substrates.
  • Polyacrylic acids as such and their salts are familiar to the person skilled in the art. These are, for example, in the radical polymerization of acrylic acid resulting polymers of the formula
  • Polyacrylic acids are also to be understood as those which have been synthesized by crosslinking copolymerization of acrylic acids with bifunctional or polyfunctional monomers or by partial crosslinking with polyvalent ions.
  • the use of the polyacrylic acids or salts thereof makes it possible to generate reversibly responsive detection layers particularly rapidly to changes in the concentration of the chemical components to be detected, whereby particularly intense dyeings or Allow color changes in the light reflected against the reflective surface produce.
  • the device according to the invention initially comprises a light-reflecting substrate or a light-reflecting background.
  • the light-reflecting substrate or the background serves as a reflective background and should therefore at least partially, in particular as completely as possible. Dere reflection of the light wavelength (s) used for detection allow.
  • the light-reflecting substrate or the light-reflecting background is a metal, in particular Al, Au, Ag, Cr or Si, whereby the use in the form of a metal foil or a metal-coated or coated foil or layer is also advantageous is possible.
  • the light-reflecting substrate or the background consists of a composite material or a two- or multi-layered film, in particular of a polymer film with a metallized layer, silvered glass or paper with a metal layer. Both flexible and rigid substrates are possible.
  • the light-reflecting substrate or the light-reflecting background may be permeable or impermeable to the chemical component to be detected.
  • a substrate or background permeable to the chemical component to be detected may be useful if the environment to be monitored is located on the side of the light-reflecting substrate opposite the detection layer. In such a case, e.g. on the side of the reflection layer opposite the light-reflecting substrate, a layer impermeable to the chemical component to be detected is applied.
  • polyacrylic acid (salt) offers the further advantage that it is very can be easily prepared in various concentrations as a solution and applied to various materials with good adhesion.
  • a solution (in particular an aqueous solution) of a polyacrylic acid or one of its salts is first prepared and then applied to the reflective background or the light-reflecting substrate.
  • the thickness of the detection layer is less than 10 ⁇ m, in particular less than 2 ⁇ m, more preferably less than 0.2 ⁇ m.
  • the thickness of the detection layer is preferably in the range from 1 nm to 10 .mu.m, in particular in the range from 1 nm to 2 .mu.m, more preferably in the range from 10 nm to 1 .mu.m, particularly preferably in the range from 50 nm to 700 nm, more preferably between 50 nm and 500 nm.
  • layer thicknesses between 100 and 600 nm, in particular between 200 and 500 nm. This ensures rapid and uniform absorption of the substance to be detected, in particular of water vapor, into the detection layer.
  • This change in the layer thickness can in turn be perceived or measured against the light-reflecting substrate or the light-reflecting background as a color change in the reflected light.
  • the detection layer is a lithium, sodium, Potassium and / or ammonium salt of at least one polyacrylic acid used.
  • the best results are achieved with lithium salts of polyacrylic acid, so that they are particularly preferred.
  • the molecular weight of the polyacrylic acid or its salt used is between about 5,000 and 500,000, in particular about 25,000 to 250,000, more preferably 50,000 and 100,000. Furthermore, it was surprisingly found that the reproducibility of the color change of the detection layer depending on the humidity of the environment to be monitored can be further increased when the polyacrylic acid is present in the detection layer in partially or completely neutralized form, preferably alkali metal hydroxides and alkali metal carbonates can be used.
  • the pH of the polyacrylic acid or salt solution used for the preparation of the detection layer is between about 2 and 7, in particular between about 3 and 7, more preferably between about 5 and 7.
  • the pH can, for example, at 23 0 C in a 10% strength by weight aqueous solution with a pH meter (inoLab, pH level 1, WTWijnlich-Technische Werkmaschinen GmbH, Weilheim, the device is calibrated according to the manufacturer's instructions with buffer solutions).
  • the degree of neutralization of the polyacrylic acids used is thus preferably about 5 to 70%, more preferably about 10 to 60%, in particular about 15 to 50%.
  • the neutralization is preferably carried out with an alkali metal hydroxide or an alkali metal carbonate.
  • the device according to the invention can also be used according to a further embodiment for the detection of further chemical components.
  • these are other volatile solvents, such as acetone or ethanol, these examples are not to be considered as limiting.
  • the respective color change, which results with the aid of the device according to the invention as a function of the concentration of the chemical component to be detected in the environment to be monitored, can be determined by the skilled person in each case with the aid of a few routine experiments.
  • the device according to the invention can easily be set in defined environments, each with a different (known) concentration of the chemical component to be detected, and the respective color or color change determined.
  • the chemical components to be detected are gaseous components, and in the environment to be monitored preferably a gaseous medium, eg air.
  • a gaseous medium eg air.
  • An example here is the monitoring of the relative humidity in the air contained in a container for a moisture-sensitive product.
  • the salt of the polyacrylic acid contains organic cations.
  • organic cations are ammonium, sulfonium or phosphonium ions. Preference is given to quaternary ammonium ions of the formula
  • radicals R 1 , R 2 , R 3 and R 4 are each independently hydrogen, an aliphatic radical having one to 18 carbon atoms (Cl to C18), an aromatic radical preferably with six Kohlenst ⁇ ffatomen, an aliphatic (Cl to C18) / aromatic (C6) radical or a heterocyclic radical containing N, O, S or P.
  • Crosslinked polyacrylic acids can also be used.
  • the at least one detection component is furthermore preferred for the at least one detection component to be homogeneously distributed in the detection layer on the light-reflecting background or the light-reflecting substrate.
  • the detection layer is present as a homogeneous monolayer.
  • two or more detection layers are possible instead of just one detection layer.
  • cover layers in addition to the at least one detection layer, further layers are contained in the device, in particular layers serving as color filters or polymerization filters. It is also possible to use cover layers, in particular to prevent damage or mechanical abrasion of the detection layer. Correspondingly, such cover layers will be mounted outwardly relative to the detection layer in order to enable efficient protection when using the detection device according to the invention.
  • Suitable materials are, for example, polyamide (PA), polyacrylonitrile (PAN) and polyethylene terephthalate (PET).
  • the device in addition to the reflective substrate or background and the detection layer, also comprises a layer, in particular a partially reflecting (semireflecting) layer of at least a metal such as gold, aluminum, chromium, nickel, silver or silicon or a metal oxide such as chromium oxide or titanium oxide.
  • a layer is advantageously mounted on the side of the detection layer opposite the reflective substrate or background, for example as an outer cover layer on the detection layer.
  • the layer should preferably be permeable to the chemical component to be detected.
  • it should preferably be at least partially transmissive (semireflecting, ie not completely permeable or fully reflecting), at least for the light used for detection. It is preferably a layer applied by metal vapor deposition or by sputter coating.
  • the layers overlying the light-reflecting substrate or background are at least partially transparent, as far as possible, for the wavelength of light used to detect the color change. transparent, to be.
  • the light pauses will be in the visible range.
  • wavelengths in the infrared or ultraviolet range can also be used when using suitable detection devices.
  • the device according to the invention is therefore preferably an optical indicator or detection element.
  • each layer lying between the detection layer and the environment to be monitored must also have a corresponding permeability to the chemical component to be detected.
  • the chemical component to be detected is water or water vapor
  • the detection layer can be applied to the reflective background or the light-reflecting substrate by all methods known to the person skilled in the art, including spin coating, dip coating, spray coating, kiss coating, screen printing and the like. It has proven to be particularly advantageous and favorable with regard to the generation of a uniform layer thickness of the detection layer, if the application takes place with the aid of spin coating, screen printing or dipcoating. These methods are known in the art as such, conventional devices can be used.
  • the viscosity of the detection component used can be influenced, for example, by changing the concentration or the solvent or suspending agent.
  • the viscosity of the polyacrylic acid (salt) solution used for the application can also be influenced by its molecular weight.
  • water is used as the solvent.
  • other solvents such as ethanol or aqueous-ethanolic solutions are possible.
  • concentration of the polyacrylic acid or its salt in the solution used for application between about 0.5 and 30 wt .-%, in particular between about 1 and 20 wt .-%, particularly preferably between about 2 and 10 wt .-% lies.
  • the viscosity is preferably in the range of 1 to 1500 mPas.
  • the viscosity was measured according to DIN 53015.
  • the surface tension is preferably in the range of 30 to 90, preferably 45 to 85 ⁇ nN / m.
  • the surface tension was determined according to DIN 53914.
  • the surface tension or viscosity can also be influenced by the addition of wetting agents or the like.
  • a non-limiting example of a suitable wetting agent is N, N-dimethyl-N-hexadecyl-N- (3-sulfopropyl) ammonium betaine (e.g., from Raschig, trade name RALUFON DP).
  • This wetting agent can be used, for example, in an amount of 0.01 to 1 wt .-%, in particular of about 0.1 wt .-%.
  • an unexpected advantage of using polyacrylic acid or its salts in the detection layer is also the ability to easily create a well-adhered uniform detection layer.
  • conventional treatment roughening, compatibilization
  • these methods are known to the person skilled in the art.
  • the device described above is an optically readable indicator element, in particular a so-called indicator card.
  • indicator card With the aid of such an indicator card, the presence or concentration of the chemical component to be detected in an environment to be monitored can be easily determined.
  • Indicator cards as such are the skilled worker and need not be further described here.
  • suitable indicator elements of several layers are known for example from US 5,224,373, US 4,034,609 and EP 1 305 621. Their disclosure in this respect with regard to the construction of an indicator element of a plurality of layers or parts is hereby expressly incorporated by reference into the present description.
  • a further aspect of the invention relates to a packaging of any kind, for example for a pharmaceutical product having a device or an indicator element as described above.
  • the device or the indicator element may preferably be arranged as an integral part of the packaging.
  • the device or the indicator element is positioned so that it is easily accessible or visible for a reading.
  • the device according to the invention can also be used (alone or in addition) for decorative purposes or as a decorative element on / in products such as consumer goods.
  • An example of a particular embodiment of the present invention is a blister pack for a pharmaceutical product conventionally consisting of a clear plastic film and a sealable aluminum foil bonded thereto.
  • the sealable aluminum foil can now serve as a reflective substrate onto which the detection layer according to the invention is applied.
  • the transparent plastic film it can be determined by means of the color or color shift of the detection layer in the light reflected against the sealable aluminum foil, to what extent the relative Moisture inside the blister pack is still in the acceptable range and thus the blister pack has no damage, could occur through the humidity.
  • a further aspect of the present invention relates to a dry agent-containing product in which the device according to the invention or the indicator element described above for checking the moisture content in the desiccant-containing product is used.
  • An example here is a container for a pharmaceutical product (e.g., tablets) in which a desiccant bag or canister is also placed.
  • a container for a pharmaceutical product e.g., tablets
  • a desiccant bag or canister is also placed.
  • About the attachment of the device according to the invention or the indicator element in the container interior can now, for.
  • the closed container for example, via a viewing window or a transparent area
  • the extent to which the acceptable relative humidity was not exceeded there and the desiccant used is still sufficiently effective.
  • another aspect of the present invention relates to a method for detecting at least one chemical component, wherein the chemical component to be detected is brought into contact with at least one detection layer as described herein, for example containing a polyacrylic acid or one of its salts, and wherein the detection layer changes its layer thickness in interaction with the component to be detected, so that the color of the detection layer, in particular with respect to a reflective surface behind it, changes in the reflected light.
  • a device as described above or, for example, a detection layer containing the inventive polyacrylic acid or one of its salts for qualitative or quantitative Determination of the detected chemical compound, in particular the humidity can be used.
  • optical measuring elements are not essential. However, it may be convenient in many cases to use known optical measuring elements, which allow an accurate determination of the wavelength of the reflected light over a wide range, in order to accurately detect the color or color change of the reflected light, both qualitatively and quantitatively. According to a preferred embodiment, an automated measuring and reading system, as used in other photospectrometric measurements, can be used for this purpose.
  • a quantitative determination of the chemical component to be detected by means of the devices according to the invention is possible by first determining these in surroundings with known concentrations of the detecting chemicals. Mix component brought and the staining is read. On the basis of this "calibration" then unknown concentrations of the chemical component to be detected of the corresponding coloration can be assigned.
  • the solution is adjusted Before spin coating, the pH of 5 and filtered using a membrane filter (CHROMAFIL ®).
  • CHROMAFIL ® membrane filter
  • the molar ratio of alkali ions to polyacrylic acid in the solution used was between 300 and 6500.
  • the sample is dried for three minutes and then shows a specific color (blue). After drying in a drying oven or treatment in a climate chamber, the sample has a different color, which depends on the respective humidity.
  • 0.4 g of water glass (Na 2 O 8.15% and SiO 2 27.06%) is applied to a Si wafer (Fa. Finders, polished on one side, diameter 50.8 mm, orientation [100] +/- 1 ° , Type P / boron, specific resistance 1 - 2 ohmcm, thickness 275 +/- 25 ⁇ m, without secondary phase) by means of spin-coating (70 rps) applied.
  • the sample is dried for 3 minutes and then shows a blue color. After drying in a dry cabinet or treatment in the climate chamber, the sample has a different color, which is dependent on the respective humidity.
  • 0.4 g of a 7.5% strength by weight polyvinylcaprolactam solution (solvent: ethanol) (BASF, Luviskol Plus, 40% strength solution in ethanol) is applied to a Si wafer (Fa. Seekers, as indicated in the preceding example ) by means of spin coating (70 rps).
  • the solution is filtered prior to the spin coating with a membrane filter (CHROMAFIL ®).
  • CHROMAFIL ® membrane filter
  • the sample is dried for 3 minutes and then shows a blue color. After drying in a drying oven or treatment in a climate chamber, the sample has a different color, which depends on the respective air humidity.
  • a multilayer film of alternating layers of synthetic hectorite and the polyelectrolyte poly (diallyldimethylammonium chloride) (PDDA) according to the Kleinfeld and Ferguson publications (supra) was formed on respective silicone wafers and with a corresponding layer thickness as in Example 1.
  • PDDA polyelectrolyte poly (diallyldimethylammonium chloride)
  • the Nachquell of the devices was determined according to Examples 1 to 6, namely the change in the color after a change from 40% relative humidity (25 ° C) to 10% relative humidity (25 ° C). Attention was paid to the time delay until the color of the sample did not change in the reflected light. This criterion can serve as an indication of how quickly equilibrium has been established with respect to the absorption of water vapor from the environment, so that no more swelling of the layer occurs and a stable color reading is possible.
  • This polymer solution is then applied to a Si wafer by means of spin coater (70 rps). The samples were dried and the intensity of the color obtained visually evaluated.

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Abstract

L'invention concerne un dispositif servant à détecter au moins un constituant chimique et comprenant un substrat ou un arrière-plan réfléchissant la lumière, ainsi qu'une couche de détection placée sur ce substrat ou cet arrière-plan et contenant au moins un constituant apte au gonflement en présence du constituant à détecter. Selon l'invention, la couche de détection est constituée d'un matériau homogène et le constituant à détecter est l'eau.
EP05823844A 2004-12-22 2005-12-21 Dispositif pour detecter au moins un constituant chimique Withdrawn EP1828750A1 (fr)

Applications Claiming Priority (2)

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DE102004061927 2004-12-22
PCT/EP2005/013791 WO2006069702A1 (fr) 2004-12-22 2005-12-21 Dispositif pour detecter au moins un constituant chimique

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EP1828750A1 true EP1828750A1 (fr) 2007-09-05

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US (1) US20090301191A1 (fr)
EP (1) EP1828750A1 (fr)
JP (1) JP2008524612A (fr)
KR (1) KR20070093976A (fr)
WO (1) WO2006069702A1 (fr)

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US7682530B2 (en) * 2007-02-07 2010-03-23 Sean Purdy Crystalline colloidal arrays responsive to an activator
US8582194B2 (en) 2010-04-29 2013-11-12 Ppg Industries Ohio, Inc. Thermally responsive crystalline colloidal arrays
US9022648B2 (en) 2010-11-11 2015-05-05 Prc-Desoto International, Inc. Temperature sensitive composite for photonic crystals
US8641933B2 (en) 2011-09-23 2014-02-04 Ppg Industries Ohio, Inc Composite crystal colloidal array with photochromic member
US20130077169A1 (en) 2011-09-23 2013-03-28 Ppg Industries Ohio, Inc. Hollow particle crystalline colloidal arrays
KR101477341B1 (ko) * 2012-05-11 2015-01-06 포항공과대학교 산학협력단 발색 습도 센서
KR101925467B1 (ko) * 2017-06-27 2018-12-05 주식회사 엘지화학 장식 부재 및 이의 제조방법
CN114414509B (zh) * 2021-12-30 2023-12-12 通标标准技术服务（天津）有限公司 食品中重金属铬的检测方法

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Also Published As

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WO2006069702A1 (fr) 2006-07-06
JP2008524612A (ja) 2008-07-10
KR20070093976A (ko) 2007-09-19
US20090301191A1 (en) 2009-12-10

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