WO2023093922A1 - Equipment for chemical analyses to detect the presence and determine the content of elements in a sample and the measurement method using this equipment - Google Patents

Equipment for chemical analyses to detect the presence and determine the content of elements in a sample and the measurement method using this equipment Download PDF

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Publication number
WO2023093922A1
WO2023093922A1 PCT/CZ2022/000047 CZ2022000047W WO2023093922A1 WO 2023093922 A1 WO2023093922 A1 WO 2023093922A1 CZ 2022000047 W CZ2022000047 W CZ 2022000047W WO 2023093922 A1 WO2023093922 A1 WO 2023093922A1
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Prior art keywords
sample
equipment
test sample
housing
focusing lens
Prior art date
Application number
PCT/CZ2022/000047
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French (fr)
Inventor
Tomáš Janeček
Drahoslav CAGAŇ
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AtomTrace a.s.
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 AtomTrace a.s. filed Critical AtomTrace a.s.
Publication of WO2023093922A1 publication Critical patent/WO2023093922A1/en

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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
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/718—Laser microanalysis, i.e. with formation of sample plasma
    • 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
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/39—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using tunable lasers
    • 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
    • G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00—Features of devices classified in G01N21/00
    • G01N2201/02—Mechanical
    • G01N2201/022—Casings
    • G01N2201/0221—Portable; cableless; compact; hand-held

Definitions

  • Equipment for chemical analyses to detect the presence and determine the content of elements in a sample and the measurement method using this equipment. field of the invention
  • the invention falls within the field of measurement methods used in various domains of human activity and deals with the new design of the equipment for chemical analyses to detect the presence and determine the content of elements in a sample, using the LIBS method, and the method of measurement using this equipment.
  • the chemical composition of materials needs to be checked in various domains, where there is a need to know the material specification of products, to verify the quality of materials, to guarantee that no materials are confused and/or to detect the presence of elements in materials or human or plant tissue.
  • AES atomic emission spectrometry
  • LIBS laser-induced breakdown spectroscopy
  • laser is used as the inducing source for the excitation of atoms in a sample.
  • a laser beam pulse is sent to the analysed sample, and its high energy concentrated in one spot causes the rapid and massive heating of the sample over a small area of between 30 and 100 ⁇ m in diameter, causing laser ablation and the formation of microplasma.
  • the microplasma loses heat and also energy, which is emitted as electromagnetic radiation.
  • the emitted radiation is detected and evaluated by a spectrometer with a detector and, because the wavelengths of the emitted radiation are different for each element, it is possible to determine the elemental composition of the sample or to determine whether sample contain the element of interest. Depending on the intensity of radiation, the concentrations of the individual elements in the sample can then be determined after the creation of a calibration curve.
  • a number of designs of analytical equipment using UBS methods for chemical analyses are known, both in the form of laboratory kits and mobile portable devices.
  • the laser beam before each shot is fired, the laser beam must first be moved in the horizontal “x” or “y” axis, then the correct distance in the “z” axis must be measured, and only then the shot must be fired.
  • the disadvantage of this procedure is that tuning the correct distance of the measured sample point for the laser beam impact can take several seconds, which for multiple shots significantly increases the duration of the measurement.
  • An example is the device described in ON 106680019, consisting of a handling unit which moves in the “x :: , “y” and “z” axes but not automatically and, in addition, the measurement distance in the “z” axis does not change and so it has to be readjusted. Prior to the measurement, the device needs to adjust the measured object, namely coal, which considerably increases the overall time for the evaluation of the checked elements.
  • the object of the present invention is to provide a new method of performing the chemical analyses of elements and the corresponding equipment, thanks to which the measurement time would be considerably reduced while preserving the quality, without significantly increasing the design complexity of the equipment, the requirements for the operation of the device and the overall production costs.
  • the invention is equipment for chemical analyses to detect the presence and determine the content of elements in a sample formed by a housing with an infrared interaction chamber embedded in part of the inner space, and containing a laser radiation source, a laser beam guide assembly featuring a focusing iens, a handling pad for storing a test sample, a spectrometer equipped with a detector, a radiation collection optical assembly, an evaluation unit comprising a PC and a height gauge for checking and determining the correct vertical distance of the focusing lens from a selected location on the test sample surface, wherein the essence of the invention is that the handling pad is automatically adjustable in the interactive chamber in the direction of the two horizontal “x” and “y” axes and also in the direction of the vertical “z” axis.
  • a power supply battery is placed inside the housing and provided with a power connection leading outside the housing.
  • analyses can be performed at the sampling location such as mining areas or environmental inspection sites.
  • the test specimen is first set on a handling pad, then the surface of the test specimen is measured using a height gauge and this is followed by the determination of the coordinates of the points to which the laser beam is to be directed while maintaining the focusing distance of the focusing lens for individual laser shots and the formation of the microplasma with the required characteristics, and then a specified number of measurements is carried out while moving the handling pad in the “x” and “y” and “z” axes: the measured values are transferred to the controlling unit using the spectrometer detector and a conclusion is made whether the test sample contains the chemical element of interest.
  • the effect of the invention is new and better compared to the known solutions in that, by simply complementing the LIBS assembly, the overall chemical analysis time is significantly reduced and the possibilities of the operational use for measuring different samples are extended without the need to change the setup or arrangement of the individual functional members of the assembly, Depending on the size of the analysed area, the measurement time reduction can be expressed as between several and hundreds of minutes. Furthermore, the new invention allows the surfaces of larger areas to be analysed without the need for alignment.
  • Fig. 1 is the layout of the basic arrangement of the equipment in a compact form, with the laser source and the spectrometer featuring a detector located inside the housing and Fig. 2 is the layout of the alternative arrangement of the equipment in an external regime, with the laser source and the spectrometer featuring a detector located outside the housing.
  • the equipment for chemical analysis in the basic embodiment shown in Fig. 1 , consists of compact housing 1. provided with a handling member (not shown), such as a handle or bracket.
  • An interaction chamber 101 is incorporated in part of the interior of the housing 1 in order to separate the dusty test area from the surrounding space; maintaining cleanliness is desirable and necessary to ensure perfect operation of the measuring and evaluation equipment.
  • the apparatus consists of a laser radiation source 2, a laser beam guide assembly 3 equipped with a laser beam focusing tens 31, a handling pad 4 for storing a test sample 5, a spectrometer 6 provided with a detector (not shown), a radiation optical collection assembly 7 consisting preferably of a lens or objective or a parabolic mirror, a height gauge 8, a controlling and evaluation unit 9, preferably consisting of a PC, and a power supply battery 10 provided with a power connection.
  • the housing 1 is provided with a handling door 102 for inserting and removing the test sample 5 and at least one passage 103 for allowing the functional members of the equipment to be connected to the space outside the housing.
  • the laser radiation source 2 is arranged so that the radiation is directed to the laser beam guide assembly 3, which is directed to the selected point of the test specimen 5 via the focusing lens 31.
  • the optical collection assembly 7 is also focused on the selected point of the test sample 5 and is connected to the spectrometer detector, from which the presence or absence of the selected chemical element can be determined in the connected controlling and evaluation unit 9 using the measured radiation wavelengths.
  • the handling pad 4 can be adjusted in the direction of two horizontal “x” and “y” axes and also in the direction of vertical “z” axis, and the height gauge 8, for example a micro-laser distance sensor, checks and determines the correct focusing distance of the focusing lens 31 from the selected location of the test specimen 5 surface.
  • the optical collection assembly 3 is further connected to the spectrometer 2 detector using optical fibre 11.
  • the laser source 2 and the spectrometer 6 are located outside the housing 1. and the test sample 5 has a top face ground flat.
  • the housing 1. may be shaped according to the users requirements user or according to the domain and location of use.
  • the test specimen 5 is first set up on the handling pad 4 and then the test specimen 5 surface is measured with the height gauge 8 and the coordinates of the points where the laser beam is to be directed while maintaining the focusing distance of the focusing lens 31 for the individual laser shots and the formation of the microplasma of the necessary characteristics are determined. Subsequently, a specified number of measurements are taken while moving the handling pad 4 in the "x" and “y” and “z” axes, and the measured values are transferred by the spectrometer 6 detector to the controlling unit 9, i.e. the PC, and it is evaluated whether the test sample 5 contains the chemical element of interest.
  • the controlling unit 9 i.e. the PC
  • the equipment according to the invention is intended for use in various industries and domains, for exampie in engineering, construction, for research into the composition of minerals or archaeological finds, or for the analysis of plant, animal or human tissues. It can be used both in laboratories and as a mobile instrument for collecting data outside of laboratories.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • General Physics & Mathematics (AREA)
  • Pathology (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Immunology (AREA)
  • Chemical & Material Sciences (AREA)
  • Optics & Photonics (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

Equipment for chemical analyses to detect the presence and determine the content of elements in a sample formed by a housing (1) with an infrared interaction chamber (101) embedded in part of the inner space, and containing a laser radiation source (2), a laser beam guide assembly (3) featuring a focusing lens (31), a handling pad (4) for storing a test sample (5), a spectrometer (6) equipped with a detector, a radiation optical collection assembly 7, an evaluation unit (9) comprising a PC and a height gauge (8) for checking and determining the correct vertical distance of the focusing lens (31) from a selected location on the test sample surface (5), where the nature of the invention is that the handling pad (4) is automatically adjustable in the interactive chamber (101) in the direction of the two horizontal "x" and "y" axes and also in the direction of the vertical "z" axis.

Description

Equipment for chemical analyses to detect the presence and determine the content of elements in a sample and the measurement method using this equipment. field of the invention
The invention falls within the field of measurement methods used in various domains of human activity and deals with the new design of the equipment for chemical analyses to detect the presence and determine the content of elements in a sample, using the LIBS method, and the method of measurement using this equipment.
Background of the invention
The chemical composition of materials needs to be checked in various domains, where there is a need to know the material specification of products, to verify the quality of materials, to guarantee that no materials are confused and/or to detect the presence of elements in materials or human or plant tissue. Recently, a new method of analytical chemistry based on the principle of atomic emission spectrometry (AES) has often been used for this purpose. In laser-induced breakdown spectroscopy (LIBS), laser is used as the inducing source for the excitation of atoms in a sample. A laser beam pulse is sent to the analysed sample, and its high energy concentrated in one spot causes the rapid and massive heating of the sample over a small area of between 30 and 100 μm in diameter, causing laser ablation and the formation of microplasma. After the laser pulse ends, the microplasma loses heat and also energy, which is emitted as electromagnetic radiation. The emitted radiation is detected and evaluated by a spectrometer with a detector and, because the wavelengths of the emitted radiation are different for each element, it is possible to determine the elemental composition of the sample or to determine whether sample contain the element of interest. Depending on the intensity of radiation, the concentrations of the individual elements in the sample can then be determined after the creation of a calibration curve. A number of designs of analytical equipment using UBS methods for chemical analyses are known, both in the form of laboratory kits and mobile portable devices. Laboratory equipment (such as SciTrace from AtomTrace, published at https://www.atomtrace.com/products/sci-trace/) is usually large and heavy and makes moving to other locations very complicated. The advantage is in modularity, allowing the replacement of the type of the UBS assembly, such as laser or spectrometer, etc. Mobile devices (e.g. handhelds from SciAps described at https://sciaps.com/libs-handheld-laser-analyzers/z-300/) are handheld compact devices that can be carried freely and used in various locations, not only indoors, but also outdoors, such as within building sites, in quarries, etc. The disadvantage is in their precisely defined compact design, which complicates the replacement of individual components, and so they are in reality single-use devices.
Nowadays, we see an increasing use of analytical devices that allow to detect samples from more locations than by a single laser shot, i.e. to use laser shots over a larger surface area of the sample by deflecting the beam to various locations or by moving the sample. Due to the fact that in order to obtain microplasma with the necessary characteristics, it is necessary to maintain a standard distance of the laser beam focusing lens from the sample, then in order to obtain relevant information, it is necessary to either resharpen and flatten the surface of the sample or, if it is impossible to flatten the sample surface, to move the sample also along the vertical !’z” axis, which is identical to the direction of the laser beam, so that the sample is always within its working distance. In known methods, before each shot is fired, the laser beam must first be moved in the horizontal “x” or “y” axis, then the correct distance in the “z” axis must be measured, and only then the shot must be fired. The disadvantage of this procedure is that tuning the correct distance of the measured sample point for the laser beam impact can take several seconds, which for multiple shots significantly increases the duration of the measurement. An example is the device described in ON 106680019, consisting of a handling unit which moves in the “x::, “y" and “z” axes but not automatically and, in addition, the measurement distance in the “z” axis does not change and so it has to be readjusted. Prior to the measurement, the device needs to adjust the measured object, namely coal, which considerably increases the overall time for the evaluation of the checked elements.
The object of the present invention is to provide a new method of performing the chemical analyses of elements and the corresponding equipment, thanks to which the measurement time would be considerably reduced while preserving the quality, without significantly increasing the design complexity of the equipment, the requirements for the operation of the device and the overall production costs.
Summary of the invention
The stated objective is achieved by the invention, which is equipment for chemical analyses to detect the presence and determine the content of elements in a sample formed by a housing with an infrared interaction chamber embedded in part of the inner space, and containing a laser radiation source, a laser beam guide assembly featuring a focusing iens, a handling pad for storing a test sample, a spectrometer equipped with a detector, a radiation collection optical assembly, an evaluation unit comprising a PC and a height gauge for checking and determining the correct vertical distance of the focusing lens from a selected location on the test sample surface, wherein the essence of the invention is that the handling pad is automatically adjustable in the interactive chamber in the direction of the two horizontal “x” and “y" axes and also in the direction of the vertical “z” axis.
In a preferred embodiment, in addition to the interaction chamber, a power supply battery is placed inside the housing and provided with a power connection leading outside the housing. Thus, analyses can be performed at the sampling location such as mining areas or environmental inspection sites.
Further, it is an essential feature of the invention that during measurements the test specimen is first set on a handling pad, then the surface of the test specimen is measured using a height gauge and this is followed by the determination of the coordinates of the points to which the laser beam is to be directed while maintaining the focusing distance of the focusing lens for individual laser shots and the formation of the microplasma with the required characteristics, and then a specified number of measurements is carried out while moving the handling pad in the “x” and “y” and “z” axes: the measured values are transferred to the controlling unit using the spectrometer detector and a conclusion is made whether the test sample contains the chemical element of interest.
The effect of the invention is new and better compared to the known solutions in that, by simply complementing the LIBS assembly, the overall chemical analysis time is significantly reduced and the possibilities of the operational use for measuring different samples are extended without the need to change the setup or arrangement of the individual functional members of the assembly, Depending on the size of the analysed area, the measurement time reduction can be expressed as between several and hundreds of minutes. Furthermore, the new invention allows the surfaces of larger areas to be analysed without the need for alignment.
Explanation for images
Specific examples of the invention embodiments are shown in the accompanying drawings, where
Fig. 1 is the layout of the basic arrangement of the equipment in a compact form, with the laser source and the spectrometer featuring a detector located inside the housing and Fig. 2 is the layout of the alternative arrangement of the equipment in an external regime, with the laser source and the spectrometer featuring a detector located outside the housing.
The drawings illustrating the presented invention and the following examples of particular embodiments do not in any way limit the scope of protection stipulated in the definition, but merely illustrate the principle of the invention. Examples of the invention designs
The equipment for chemical analysis, in the basic embodiment shown in Fig. 1 , consists of compact housing 1. provided with a handling member (not shown), such as a handle or bracket. An interaction chamber 101 is incorporated in part of the interior of the housing 1 in order to separate the dusty test area from the surrounding space; maintaining cleanliness is desirable and necessary to ensure perfect operation of the measuring and evaluation equipment. The apparatus consists of a laser radiation source 2, a laser beam guide assembly 3 equipped with a laser beam focusing tens 31, a handling pad 4 for storing a test sample 5, a spectrometer 6 provided with a detector (not shown), a radiation optical collection assembly 7 consisting preferably of a lens or objective or a parabolic mirror, a height gauge 8, a controlling and evaluation unit 9, preferably consisting of a PC, and a power supply battery 10 provided with a power connection. The housing 1 is provided with a handling door 102 for inserting and removing the test sample 5 and at least one passage 103 for allowing the functional members of the equipment to be connected to the space outside the housing. The laser radiation source 2 is arranged so that the radiation is directed to the laser beam guide assembly 3, which is directed to the selected point of the test specimen 5 via the focusing lens 31. The optical collection assembly 7 is also focused on the selected point of the test sample 5 and is connected to the spectrometer detector, from which the presence or absence of the selected chemical element can be determined in the connected controlling and evaluation unit 9 using the measured radiation wavelengths. The handling pad 4 can be adjusted in the direction of two horizontal “x” and “y” axes and also in the direction of vertical “z” axis, and the height gauge 8, for example a micro-laser distance sensor, checks and determines the correct focusing distance of the focusing lens 31 from the selected location of the test specimen 5 surface. The optical collection assembly 3 is further connected to the spectrometer 2 detector using optical fibre 11. In the alternative embodiment of the equipment according to Fig. 2, the laser source 2 and the spectrometer 6 are located outside the housing 1. and the test sample 5 has a top face ground flat. The described and illustrated examples are not the only possible embodiments according to the invention; for example, the housing 1. may be shaped according to the users requirements user or according to the domain and location of use.
During the analysis, i.e. during the measurement, the test specimen 5 is first set up on the handling pad 4 and then the test specimen 5 surface is measured with the height gauge 8 and the coordinates of the points where the laser beam is to be directed while maintaining the focusing distance of the focusing lens 31 for the individual laser shots and the formation of the microplasma of the necessary characteristics are determined. Subsequently, a specified number of measurements are taken while moving the handling pad 4 in the "x" and “y” and "z" axes, and the measured values are transferred by the spectrometer 6 detector to the controlling unit 9, i.e. the PC, and it is evaluated whether the test sample 5 contains the chemical element of interest.
Industrial applicability
The equipment according to the invention is intended for use in various industries and domains, for exampie in engineering, construction, for research into the composition of minerals or archaeological finds, or for the analysis of plant, animal or human tissues. It can be used both in laboratories and as a mobile instrument for collecting data outside of laboratories.

Claims

PATENT CLAIMS
1, Equipment for chemical analyses to detect the presence and determine the content of elements in a sample formed by a housing (1) with an infrared interaction chamber (101) embedded in part of the inner space, and containing a laser radiation source (2), a laser beam guide assembly (3) featuring a focusing lens (31), a handling pad (4) for storing a test sample (5), a spectrometer (6) equipped with a detector, a radiation optical collection assembly 7, an evaluation unit (9) comprising a PC and a height gauge (8) for checking and determining the correct vertical distance of the focusing lens (31) from a selected location on the test sample surface (5), characterized in that the handling pad (4) is automatically adjustable in the interactive chamber (101) in the direction of the two horizontal “x” and “y” axes and also in the direction of the vertical “z” axis.
2. Equipment according to claim 1, characterized in that in addition to the interaction chamber (101), a power supply battery (10) is placed inside the housing (1) and provided with a power connection leading outside the housing (1).
3. Method of performing the chemical analysis for the presence and determination of the content of elements in a sample using equipment according to claim 1 , characterized in that the test sample (5) is first set up on a handling pad (4), then the surface of the test sample (5) is measured using a height gauge (8) and the coordinates of the points are determined, where the laser beam is to be directed while maintaining the focusing distance of the focusing lens (31) for the individual laser shots and the formation of the microplasma of the required characteristics, and then a specified number of measurements are taken while moving the handling pad (4) In the “x” and “y" and “z” axes, and the measured values are transferred to the controlling unit (9) by the spectrometer (6) detector and are evaluated to determine whether the test sample (5) contains the chemical element of interest.
PCT/CZ2022/000047 2021-11-26 2022-11-22 Equipment for chemical analyses to detect the presence and determine the content of elements in a sample and the measurement method using this equipment WO2023093922A1 (en)

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CZPV2021-540 2021-11-26
CZ2021-540A CZ2021540A3 (en) 2021-11-26 2021-11-26 Equipment for chemical analysis of the presence and determining the content of elements in a sample and measuring with this equipment

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111610179A (en) * 2020-05-20 2020-09-01 北京科技大学 System and method for quickly detecting components LIBS of high-temperature sample in front of furnace
CN113109273A (en) * 2021-04-25 2021-07-13 中国科学院合肥物质科学研究院 High-performance portable LIBS analysis system
US20210341392A1 (en) * 2008-05-05 2021-11-04 Applied Spectra, Inc. Laser ablation analysis

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20210341392A1 (en) * 2008-05-05 2021-11-04 Applied Spectra, Inc. Laser ablation analysis
CN111610179A (en) * 2020-05-20 2020-09-01 北京科技大学 System and method for quickly detecting components LIBS of high-temperature sample in front of furnace
CN113109273A (en) * 2021-04-25 2021-07-13 中国科学院合肥物质科学研究院 High-performance portable LIBS analysis system

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