EP3586106A1 - Procédé pour quantifier une matière ou un mélange de matières - Google Patents

Procédé pour quantifier une matière ou un mélange de matières

Info

Publication number
EP3586106A1
EP3586106A1 EP18708903.2A EP18708903A EP3586106A1 EP 3586106 A1 EP3586106 A1 EP 3586106A1 EP 18708903 A EP18708903 A EP 18708903A EP 3586106 A1 EP3586106 A1 EP 3586106A1
Authority
EP
European Patent Office
Prior art keywords
fibers
component
coating
products
materials
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Withdrawn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
EP18708903.2A
Other languages
German (de)
English (en)
Inventor
Alex Deitermann
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.)
TAILORLUX GmbH
Original Assignee
TAILORLUX GmbH
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 TAILORLUX GmbH filed Critical TAILORLUX GmbH
Publication of EP3586106A1 publication Critical patent/EP3586106A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G01J3/2823—Imaging spectrometer
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G01J3/44—Raman spectrometry; Scattering spectrometry ; Fluorescence spectrometry
    • G01J3/4406—Fluorescence spectrometry
    • 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
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G01J3/2823—Imaging spectrometer
    • G01J2003/2826—Multispectral imaging, e.g. filter imaging
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G01J3/42—Absorption spectrometry; Double beam spectrometry; Flicker spectrometry; Reflection spectrometry
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G01J3/443—Emission spectrometry
    • 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
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N2021/6439—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" with indicators, stains, dyes, tags, labels, marks
    • 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
    • G01N2021/8444—Fibrous 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
    • G01N21/6408—Fluorescence; Phosphorescence with measurement of decay time, time resolved fluorescence
    • 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
    • G01N21/645—Specially adapted constructive features of fluorimeters
    • G01N21/6456—Spatial resolved fluorescence measurements; Imaging

Definitions

  • the present invention relates to a method for identifying and quantifying a material or a material mixture, wherein the material or the material mixture contains one or more phosphors / markers which are invisible in daylight.
  • the lower quality of the end product is not already noticed in the manufacturing process, but only by the end users.
  • the problem of blending or lengthening high quality raw materials with inferior materials occurs not only in cotton, but also in many other high value and high value fibers such as cashmere, merino wool, and silk, as well as other natural and synthetic fibers used for the production of high-priced branded products.
  • Other materials, for example, offered in the form of bulk materials are stretched by the addition of lower quality products. Examples include natural products such as fruits nuts, cereals, seeds, paints and varnishes, ink and other printed products, as well as plastics and chemicals.
  • the present invention was accordingly an object of the invention to provide a method with which it is possible to mark the starting materials used to recognize by means of suitable metrology, ie identify and determine whether the composition of the material or material mixture of the desired and by the producer given composition (quantification) corresponds.
  • the present invention accordingly provides a method for identifying and quantifying a material or material mixture, the material or the material mixture containing one or more component (s) X which can be identified by means of spectroscopic methods and / or with a hyperspectral camera,
  • the method according to the invention it is possible to identify materials and material mixtures which are used as raw or semi-finished products in the end products and also to determine its quantitative proportion in a product. If, for example, it has been found that the material or material mixture to be identified is contained in a product, it can also be ascertained whether this raw or semi-finished product to be identified is also present in the desired amount or in the amount that was specified or whether other components have been added to the product.
  • the components X should be identifiable by means of spectroscopic methods and / or by means of a hyperspectral camera and / or a photodiode.
  • Spectroscopic methods include emission spectroscopy, absorption spectroscopy, reflection spectroscopy, but also recording and evaluation by means of hyperspectral imaging.
  • a preferred method used in the context of the present invention is emission spectroscopy.
  • one or more signal (s) of the component X is generated by excitation with a radiation source in the range from 280 to 1100 nm.
  • the signals are detected by means of a suitable spectrometer system, a hyperspectral camera or a photodiode. It is possible to detect individual signals, in particular prominent signals (prominent peaks) or also complete spectra of the component X or to record one or more hyperspectral images.
  • the signal or spectrum or hyperspectral image is obtained in response to excitation pulses as a function of time, temperature and / or change in ambient pressure. If the term signal is used below, this is to be understood as meaning a single signal or peak of an emission spectrum, but also a complete spectrum or an image recorded by means of a hyperspectral camera or a signal recorded by a photodiode.
  • the signals or spectra obtained or the recorded images are evaluated in the next method step B.
  • the evaluation takes place in which the obtained signals or spectra or hyperspectral images are compared with the predetermined signals, spectra or hyperspectral images obtained for the component (n) X under the same excitation conditions.
  • the quantitative determination of the component X is carried out by methods known from the prior art.
  • the intensity of a signal changes as a function of the concentration, wherein the change in the intensity of the measured signal or the signals or recorded images at different concentrations also depends on the behavior of the respective component X.
  • the component X should not only be identifiable via the methods used, but also be quantifiable.
  • the signals can be obtained as a function of excitation pulses, as a function of the time, of the temperature and / or the change of the ambient pressure.
  • the change in the intensity of the signal may be linear or not linear.
  • model measurements the changes in the signals and / or images under known conditions and with a known amount of component X contained are measured and graphed, either in tabular form or as a diagram (also by means of suitable software) or transferred to a mathematical model. These model measurements can serve as a basis for the determination of the concentration of the component X in the investigated product.
  • the determination of the existing quantity of the component X can be done manually by means of tables or diagrams created or also by mathematical operations with respect to a determined reference value / ratio / signal / spectrum for the material or mixture of materials or end product to the reference product , From the qualitative and quantitative determination of the component X, it can be determined whether and to what extent the examined material or material mixture was delivered or processed in a product. In this way, it is possible to check in the ongoing production process or in the final product whether the specified materials and material mixtures were actually used and also in the desired quantity.
  • the components X can be selected from any optically and spectroscopically identifiable substances.
  • component X can be incorporated in a separate carrier material which is added to the material or material mixture or incorporated into this material.
  • the component X should be chemically and physically stable both within the material or material mixture or when it is incorporated into a carrier and also not or hardly adversely affect the material properties.
  • Highly suitable substances that can be used as component X include organic complex compounds, organic phosphors and / or inorganic phosphors. These phosphors, also known as luminescent agents or luminescent substances, are already widely used in the identification of objects, for example in banknotes and other value documents.
  • Organic complex compounds and / or phosphors may be selected from organically conjugated systems such as fluorescein derivatives, coumarin derivatives, oxazine derivatives, rhodamine derivatives, lumogens, pyrromethene dye derivatives or others.
  • rare earth complexes with Eu 3+ , Tb 3+ , Sm 2+ , Sm 3+ , Nd 3+ , Ce 3+ , Pr 3+ , Pr 4+ , Dy 3+ , Ho 3+ , Er 3+ , Tm 3+ Yb 2+ or Yb 3+ , but also complex compounds with Ru 3+ , Cr 3+ , Mn 2+ , Mn 3+ , Mn 4+ , Fe 3+ .
  • organically conjugated ligands such as acetylacetone (ACAC), dibenzoylmethane (DBM), 4,4,4-trifluoro-1- (2-naphthyl) -1,3-butanedione (TFNB), thenoyltrifluoroacetone (TTFA), bipyridine derivatives, phenanthroline derivatives or other organic complexing ligands
  • Inorganic phosphors may be selected solid compounds containing one or more luminescent ions from the group: In + , Sn 2+ , Pb 2+ , Sb 3+ , Bi 3+ , Ce 3+ , Pr 3+ , Nd 3+ , Sm 2+ , Sm 3+ , Eu 2+ , Eu 3+ , Gd 3+ , Tb 3+ , Dy 3+ , Ho 3+ , Er 3+ , Tm 2+ , Tm 3+ , Yb 2+ , Yb 3+ , Ti 3+ , Ti 4+ , V 2+ , V 3+ , V 4+ , Cr 3+ , Mn 2+ , Mn 3+ , Mn 4+ , Fe 3+ , Fe 4+ , Fe 5+ , Co 3+ , Co 4+ , Ni 2+ , Cu + , Ru 2+ , Ru 3+ , Pd 2+ , Ag + , Ir 3+ , Pt
  • Preferred inorganic luminescent pigments are binary, ternary or quaternary halides, oxides, oxyhalides, sulfides, oxysulfides, sulfates, oxysulfates, selenides, nitrides, oxynitrides, nitrates, oxynitrates, phosphides, phosphates, carbonates, silicates, oxysilicates, vanadates, molybdate, tungstates, germanates or Oxygermanate of the elements Li, Na, K, Rb, Mg, Ca, Sr, Sc, Ba, Y, La, Ti, Zr, Hf, Nb, Ta, Zn, Gd, Lu, Al, Ga and In.
  • the quantitative determination takes place in the product. For this purpose, it must be ensured that the incorporation of the labeling into the desired product is as homogeneous as possible and does not change over time, so that the reference to the specific and averaged reference continues to exist.
  • the qualitative and quantitative determination of the component X can, as described above, carried out by reference to the given product with the aid of different types of sensors by referencing.
  • the sensor types according to the method comprise in particular the following list:
  • Photodiodes Determination of the (wavelength-dependent) intensity of the emission in response to the excitation by radiation of wavelength 280-1 100 nm by the determination of the current intensity and subsequent metrological adjustment of the sample with pattern and identification of the quantity of the label in the sample.
  • Hyperspectral camera Determination of the spectral emission intensity of individual pixels, intensity of the optical signal (in response to excitation by light) Radiation of wavelength 280-1100 nm and metrological comparison of the sample with pattern and identification of the quantity of label in the sample.
  • Fluorescence spectroscopy Determination of the wavelength-dependent intensity of the radiation emission in response to the excitation by radiation of wavelength 280-1 100 nm and metrological comparison of the sample with pattern and identification of the quantity of the label in the sample.
  • the measurements required to determine the quantity of labeled material can be made manually or automatically for the respective sensor types, ie "offline” or “online”. Furthermore, the measurements required for the determination of the quantity of the marked material can take place both at one and at any desired number of measuring locations and a number from 1 to infinity can be recorded on samples or measured values for collecting emission data.
  • the subsequent concentration determination (quantification) can, as described above, be carried out manually or else by means of mathematical methods and the comparison with a data model developed for the respective component X.
  • suitable mixtures of materials that can be identified are fibers such as vegetable fibers, animal fibers, synthetic fibers or mineral fibers.
  • the fibers may be intermediates, eg. As threads or filaments act as well as products of these threads and filaments.
  • examples of fibers are vegetable fibers such as cotton fibers, kapok, flax, hemp, jute, rami, sisal, coconut, etc., as well as animal fibers, d. H.
  • Protein-based fibers such as sheep wool, goat hair (mohair), cashmere or Vietnamese wool, alpaca, llama, vicuna, camel hair, angora, horsehair and any other animal hair.
  • silk such as mulberry silk or silk silk (Tussah silk).
  • technical fibers such as mineral fibers and synthetic fibers, d. H. from polymers such as polyester fibers, polyamide fibers or aramid fibers, polyvinyl chloride, polyolefin, polyvinylidene chloride, polyvinyl acetate or multipolymerizates such as modacrylic, polyurethanes and elastanes.
  • inorganic based fibers are glass fibers, metal fibers and mineral fibers.
  • any other materials and mixtures of materials, in the form of liquids or bulk solids, may also be treated with a component X to identify these materials and to verify the quality of the material by quantifying the labeled material.
  • these other materials may include chemicals, plastics and plastic products, minerals, liquids, plants, fruits, seeds and animal products, and derived substances and products.
  • the material or material mixture are fiber materials, in particular natural fibers such as cotton.
  • the cotton fibers may contain a defined proportion of aggregates, for example plastic or cellulose, in which one or more component (s) X are incorporated.
  • component X into or onto the material or mixture of materials may be accomplished in any suitable manner, such as incorporation into fibers, incorporation of labeled fibers into unlabelled fibers, coating of fibers, incorporation of markers into filaments (filaments), coating Filaments, "woven” and “non-woven” coating, coating, in particular painting or painting, painting, spin coating, spray painting, thermal spraying, plasticizing, dip coating (anodic or cathodic), hot dipping, enamelling, slot die coating, knife coating , Dip coating, spray coating, roller coating, cascading or curtain coating, sol-gel, thermal spraying, powder coating, tumbling, tumbling, printing on materials, objects and products (integration with printing inks, inks, varnishes, primers or any other means of pressure ) about all printing processes.
  • any suitable manner such as incorporation into fibers, incorporation of labeled fibers into unlabelled fibers, coating of fibers, incorporation of markers into filaments (filaments), coating Filaments, "woven” and
  • textile fibers are marked and textile materials obtained therefrom are identified and their quality in terms of the proportion of labeled fibers is quantitatively verified.
  • Natural fibers are first spun and then further processed into fabrics and knitted fabrics in known processing methods, usually woven or entangled. Frequently, additional fibers are added to the natural fibers to adjust the quality and properties of the finished product accordingly.
  • Other fibers that can be added to natural fibers include, for example, synthetic fibers.
  • synthetic fibers eg cellulose fibers
  • containing a component X are used. The natural fiber is spun together with the synthetic fiber or the synthetic fiber is added to the natural fiber prior to further processing or incorporated in the weaving or knitting process.
  • the resulting product, the spun fiber or the textile material in the form of the fabric or knitted fabric is then further processed into the textile product.
  • the material in the form of a spectrum and / or a hyperspectral image of
  • the component X itself is determined by evaluating the spectrum and / or image obtained and assigning it to a spectrum or image as a component X. From the determined intensities from the spectrum, it is finally possible to increase the amount of component X (quantification) used determine.

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • General Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Immunology (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Optics & Photonics (AREA)
  • Pathology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

L'invention concerne un procédé pour identifier et quantifier une matière ou un mélange de matières, la matière ou le mélange de matières comprenant un ou plusieurs composant(s) X pouvant être identifié(s) au moyen d'un procédé spectroscopique et/ou au moyen d'une caméra hyperspectrale. Le procédé selon l'invention comprend les étapes qui consistent : A. à générer un ou plusieurs signaux par excitation au moyen d'une source de rayonnement selon une gamme comprise entre 280 et 1100 nm et à les enregistrer au moyen d'un système spectrométrique adapté, d'une caméra hyperspectrale ou d'une photodiode, B. à évaluer le signal ou les signaux obtenu(s) et/ou l'image ou les images hyperspectrale(s) et à associer le signal ou les signaux et/ou l'image ou les images hyperspectrale(s) à un composant X, puis à associer le composant X identifié à une matière ou un mélange de matières , C. à effectuer une détermination quantitative de la matière ou du mélange de matières.
EP18708903.2A 2017-02-23 2018-02-23 Procédé pour quantifier une matière ou un mélange de matières Withdrawn EP3586106A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102017103780.2A DE102017103780A1 (de) 2017-02-23 2017-02-23 Verfahren zur Identifizierung eines Materials bzw. Materialgemisches
PCT/DE2018/100161 WO2018153411A1 (fr) 2017-02-23 2018-02-23 Procédé pour quantifier une matière ou un mélange de matières

Publications (1)

Publication Number Publication Date
EP3586106A1 true EP3586106A1 (fr) 2020-01-01

Family

ID=61569006

Family Applications (1)

Application Number Title Priority Date Filing Date
EP18708903.2A Withdrawn EP3586106A1 (fr) 2017-02-23 2018-02-23 Procédé pour quantifier une matière ou un mélange de matières

Country Status (4)

Country Link
US (1) US20200271517A1 (fr)
EP (1) EP3586106A1 (fr)
DE (1) DE102017103780A1 (fr)
WO (1) WO2018153411A1 (fr)

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