Analysis method and composite analysis device

Abstract

The invention provides an analysis method and a composite analysis device. The analysis method is performed in a composite analysis device capable of performing infrared spectroscopic analysis based on an infrared spectroscopic analysis method and LIBS analysis based on a laser-induced breakdown spectroscopy analysis method on a sample. The present invention also relates to a method for analyzing a sample based on the infrared spectroscopic analysis method and a method for analyzing the sample based on the laser-induced breakdown spectroscopy analysis method, and to a method for analyzing the sample based on the laser-induced breakdown spectroscopy analysis method based on the infrared spectroscopic analysis method based on the infrared spectroscopic analysis method. The analysis method comprises the following steps: ST02-ST06, irradiating infrared rays on a sample to perform infrared spectroscopic analysis; steps ST08-ST12 for irradiating the sample with a laser beam to perform LIBS analysis; and a step ST14 for identifying the components of the sample on the basis of the first analysis data obtained by the infrared spectroscopic analysis and the second analysis data obtained by the LIBS analysis. The step of performing the infrared spectroscopic analysis is performed before the step of performing the LIBS analysis.

Description

Technical Field

[0001] The present disclosure relates to an analysis method and a composite analysis device. Background Art

[0002] Infrared spectroscopy is an analytical method that analyzes components in a sample by irradiating infrared light to a sample to be measured and detecting transmitted light or reflected light. Infrared spectroscopy is performed using an infrared spectrophotometer.

[0003] As described in Japanese Patent Application Laid-Open No. 2019-32214, infrared spectroscopy is suitable for analyzing polymer materials and organic substances. Summary of the invention

[0004] Problem that the invention aims to solve

[0005] However, infrared spectroscopy is not the most suitable method for analyzing inorganic substances such as metals. For example, it is known that laser-induced breakdown spectroscopy (LIBS) analysis is suitable for analyzing inorganic substances such as metals.

[0006] Therefore, the user needs to estimate the component to be analyzed in the sample and consider which analysis method to provide to the analysis device, which is time-consuming for the user.

[0007] The present disclosure has been made to solve the above-mentioned problems, and an object of the present disclosure is to provide a system capable of performing comprehensive analysis from organic matter to inorganic matter.

[0008] The first embodiment of the present invention is an analysis method performed in a composite analysis device capable of performing infrared spectroscopy analysis based on infrared spectroscopy and LIBS analysis based on laser-induced breakdown spectroscopy analysis on a sample. The analysis method includes the following steps: irradiating the sample with infrared rays to perform infrared spectroscopy analysis; irradiating the sample with laser to perform LIBS analysis; and identifying the components of the sample based on first analysis data obtained by infrared spectroscopy analysis and second analysis data obtained by LIBS analysis. The step of performing infrared spectroscopy analysis is performed before the step of performing LIBS analysis.

[0009] Another embodiment of the present invention is a composite analysis device having a sample holder, an infrared light source, a detector, a laser light source, a spectrometer, and a control device. A sample is set in the sample holder. The infrared light source generates infrared light to be irradiated onto the sample. The detector detects infrared light emitted from the sample by irradiation of the infrared light. The laser light source generates laser light to be irradiated onto the sample. The spectrometer spectrometers the luminous light generated in the sample by irradiation of the laser light. The control device obtains first analysis data obtained by performing infrared spectroscopy analysis on the infrared light emitted from the sample and second analysis data obtained by performing LIBS analysis on the luminous light generated in the sample. The control device identifies the components of the sample based on the first analysis data and the second analysis data. The control device irradiates the sample with infrared light before irradiating the sample with the laser light.

[0010] The above objects, features, aspects and advantages and other objects, features, aspects and advantages of the present invention will become more apparent from the following detailed description of the present invention when taken in conjunction with the accompanying drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0011] Figure 1 It is a diagram showing the structure of the composite analysis device according to the embodiment and the first optical path during infrared spectrum analysis.

[0012] Figure 2 It is a diagram showing the second optical path during LIBS analysis.

[0013] Figure 3 It is a diagram showing the structure of the analysis device according to Modification 1 and the first optical path during infrared spectrum analysis.

[0014] Figure 4 This is a flowchart showing the processing related to the analysis method according to the embodiment.

[0015] Figure 5 This is a flowchart showing the processing related to the analysis method involved in Modification Example 2. DETAILED DESCRIPTION

[0016] Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. In addition, the same reference numerals are given to the same or corresponding parts in the drawings, and their description will not be repeated.

[0017] [1. Configuration of complex analysis device according to the embodiment]

[0018] Figure 1 1 is a diagram showing the structure of the composite analysis device 100 according to the embodiment and the first optical path 15 during infrared spectrum analysis. Figure 2 25 is a diagram showing the second optical path 25 during LIBS analysis. Figure 1-2The structure of the complex analysis device 100 , the first optical path 15 , and the second optical path 25 will be described.

[0019] The complex analysis device 100 includes a control device 90 and an analysis device 101 .

[0020] The analysis device 101 is a device for analyzing the sample S. The analysis device 101 can perform infrared spectroscopy analysis based on infrared spectroscopy and LIBS analysis based on laser-induced breakdown spectroscopy. In the analysis device 101, LIBS analysis is generally performed after infrared spectroscopy.

[0021] The analysis device 101 includes a sample holder 5 , an infrared light source 10 , a detector 11 , a laser light source 20 , a spectrometer 21 , and a plurality of reflection mirrors 31 to 37 .

[0022] The sample S is placed in the sample holder 5. In one embodiment, the sample S is a solid sample. However, as described later, the sample S may be a liquid sample or a gas sample stored in a container. Figure 1 In the example, the sample holder 5 is a sample stage. In one embodiment, the direction perpendicular to the sample stage is set as the Z axis, and the plane parallel to the sample stage is set as the XY plane. In one embodiment, the sample stage is used in a state where the Z axis is set to be roughly parallel to the gravity direction (vertical direction). Moreover, the sample S is placed on the upper surface of the sample stage. The sample stage is formed, for example, of a material with low transmittance of infrared light (for example, metal). The sample holder 5 can be any mechanism as long as it can fix the position of the sample S during analysis, for example, it can also be a holding mechanism for holding the sample S.

[0023] The infrared light source 10 generates infrared light to be irradiated to the sample S. In one embodiment, the infrared light source 10 includes an interferometer (not shown) and a light source unit (not shown), and the infrared light source 10 generates interfering infrared light for performing spectroscopic measurement. In one embodiment, the infrared light generated from the infrared light source 10 is incident on a specific position S0 of the sample S. The specific position S0 is, for example, an analysis object position of the sample S. In one embodiment, the specific position S0 is a position where LIBS analysis can be performed, and more specifically, the specific position S0 is a position on the surface of the sample S or a position near the surface of the sample S. The infrared light irradiated to the sample S is, for example, an infrared light beam having a specified beam diameter and power density. The beam diameter and power density are set in a manner to have a beam intensity sufficient for infrared spectroscopy analysis.

[0024] The detector 11 is a photodetector that detects infrared light emitted from the sample S by irradiation with infrared light. A light reception signal of the detector 11 is transmitted to the control device 90 .

[0025] The laser light source 20 generates laser light to be irradiated to the sample S. In one embodiment, the laser light source 20 includes a laser oscillator (not shown) and a focusing lens (not shown), and the laser pulse emitted by the laser oscillator is focused by the focusing lens and then irradiated to the sample S. In one embodiment, the laser light generated by the laser light source 20 is incident on a specific position S0 of the sample S. The laser light irradiated to the sample S is set to have a predetermined beam diameter and power density, for example. The beam diameter and power density are set so as to have a beam intensity sufficient for LIBS analysis.

[0026] The spectrometer 21 is an ultraviolet-visible spectrometer that separates the luminescent light generated by the sample S by the irradiation of the laser. The luminescent light is an atomic line and / or an ion line generated when the sample components are atomized and excited (plasmaized) on the surface and / or near the surface of the sample by the irradiation of the laser. A signal indicating the result of the spectral separation of the luminescent light by the spectrometer 21 is sent to the control device 90.

[0027] The positions of the plurality of reflectors 31 to 37 can be Figure 1 The first position shown and Figure 2 The second position is shown. Figure 1-2 In the example of FIG. 1 , the positions of the reflectors 31 and 32 indicated by arrows AR1 and AR2 are different in the first position and the second position, respectively. The reflectors 31 and 32 are movable mirrors configured to be able to change their positions by a reflector drive mechanism (not shown). The reflector drive mechanism can change the position of each of the reflectors 31 and 32 from Figure 1 Move to the position (first position) Figure 2 position (second position), or from Figure 2 Move to the position (second position) Figure 1 The example of the mirror driving mechanism is not limited to this, and for example, it is a rail that slides the positions of the mirrors 31 and 32.

[0028] Reflectors 33 to 37 are fixed mirrors whose positions are fixed. Reflectors 35 to 37 are parabolic mirrors arranged at positions where the focus described later is focused on a specific position S0. On the other hand, each of the reflectors 31, 32, 33, and 34 is arranged at a position where light is incident on the parabolic mirror or where light generated from the parabolic mirror is introduced into the detector 11 or the spectrometer 21.

[0029] When the positions of the plurality of reflectors 31 to 37 are set to the first position, the first optical path 15 is formed. The first optical path 15 includes an optical path 151 and an optical path 152. In the optical path 151, the infrared light generated from the infrared light source 10 is reflected by the reflectors 33, 36, and 35 in sequence, and then enters the specific position S0 of the sample S. In the optical path 152, the infrared light emitted from the specific position S0 is reflected by the reflectors 37, 36, and 34 in sequence, and then enters the detector 11.

[0030] When the positions of the plurality of reflectors 31 to 37 are set to the second position, a second optical path 25 is formed. The second optical path 25 includes an optical path 251 and an optical path 252. In the optical path 251, the laser light generated from the laser light source 20 is reflected by the reflectors 31, 36, and 35 in sequence, and then enters the specific position S0. In the optical path 252, the luminous light generated from the specific position S0 is reflected by the reflectors 37, 36, 34, and 32 in sequence, and then enters the spectrometer 21.

[0031] More specifically, the first positions of the plurality of reflectors 31 to 37 are preferably set so that the intersection (so-called focus) of the center of the incident infrared light 1511 and the center of the emitted infrared light 1521 is located at a specific position S0 of the sample S during infrared spectrum analysis.

[0032] In addition, the second positions of the plurality of reflection mirrors 31 to 37 are preferably set so that the intersection (so-called focus) of the center of the incident laser light 2511 and the center of the emitted light beam 2521 is located at a specific position S0 of the sample S during LIBS analysis.

[0033] exist Figure 1-2 In the example of , the structure is such that when light is incident on the position 361 of the reflector 36 at a predetermined first angle, the focus is focused on a specific position S0 of the sample, and then the light is emitted from the position 362 of the reflector 36 at a predetermined second angle. Moreover, in the first position, it is set that the infrared light 1512 is incident on the position 361 of the reflector 36 at the first angle using the reflector 33, and the infrared light 1522 emitted from the position 362 of the reflector 36 is incident on the detector 11 using the reflector 34. In addition, in the second position, it is set that the laser light 2512 is incident on the position 361 of the reflector 36 at the first angle using the reflector 31, and the luminous light 2522 emitted from the position 362 of the reflector 36 is incident on the spectrometer 21 using the reflectors 34 and 32.

[0034] As described above, in the analysis device 101 , the same position (specific position S0 ) of the sample S can be analyzed in both infrared spectrum analysis and LIBS analysis by a simple configuration and control in which two reflection mirrors are moved to switch the optical path.

[0035] The control device 90 can be constituted by a personal computer or a microcomputer including a CPU (Central Processing Unit) and a memory (not shown).

[0036] The control device 90 controls the analysis device 101. The control device 90 controls the infrared light source 10 and the detector 11 to perform infrared spectroscopy. The control device 90 controls the laser light source 20 and the spectrometer 21 to perform LIBS analysis. When performing infrared spectroscopy, the control device 90 controls the mirror drive unit to configure the positions of the plurality of mirrors 31 to 37 at the first position. When performing LIBS analysis, the control device 90 controls the mirror drive unit to configure the positions of the plurality of mirrors 31 to 37 at the second position. In addition, the movement of the mirrors 31 and 32 may also be configured to be performed manually by the user. However, in order to move the mirrors 31 and 32 to an accurate position for high-precision analysis, it is preferred that the control device 90 controls the positions of the mirrors 31 and 32.

[0037] The control device 90 irradiates infrared light to the sample S to perform infrared spectroscopy analysis before irradiating the sample S with laser light to perform LIBS analysis. Thus, infrared spectroscopy analysis can be performed on the components of the sample S before denaturation due to LIBS analysis. Therefore, both infrared spectroscopy analysis and LIBS analysis can be accurately performed on the same position (specific position S0) of the sample S.

[0038] The control device 90 also performs processing for identifying the components of the sample S based on the signal received from the detector 11 in the infrared spectrum analysis and the signal received from the spectrometer 21 in the LIBS analysis.

[0039] Specifically, the control device 90 first obtains first analysis data obtained by infrared spectrum analysis of infrared light emitted from the sample S and second analysis data obtained by LIBS analysis of luminescent light generated in the sample S. The first analysis data is, for example, an infrared spectrum, and the second analysis data is, for example, a luminescent light spectrum.

[0040] In one embodiment, the control device 90 performs Fourier transform and other processing on the light receiving signal received from the detector 11 to produce an infrared spectrum. In addition, the control device 90 produces a luminous light spectrum based on a signal indicating a spectroscopic result of the luminous light received from the spectroscope 21. However, the infrared spectrum and the luminous light spectrum may be sent to the control device 90 after being produced by the detector 11 and the spectroscope 21, respectively.

[0041] Furthermore, the control device 90 identifies the components of the sample S based on the first analysis data and the second analysis data. Specifically, for example, the control device 90 identifies the components of the specific position S0 based on the peak wavelength of the infrared spectrum, and quantifies the components according to the intensity of the peak wavelength. Also, for example, the control device 90 identifies the components of the specific position S0 based on the peak wavelength of the luminescent light spectrum, and quantifies the components according to the intensity of the peak wavelength.

[0042] According to the composite analysis device 100 described above, it is possible to perform both infrared spectroscopy and LIBS analysis on the sample S. Therefore, when the component to be analyzed in the sample S is an organic substance, the component can be identified with high accuracy based on the first analysis data obtained by infrared spectroscopy. On the other hand, even when the component to be analyzed in the sample S is an inorganic substance, the component can be identified with high accuracy based on the second analysis data obtained by LIBS analysis. Therefore, regardless of whether the component to be analyzed in the sample S is an organic substance or an inorganic substance, the composite analysis device 100 can identify the component with high accuracy. Thus, the user can save the effort of estimating the component to be analyzed in the sample S before starting to analyze the sample S, and considering whether to provide it to an analysis device suitable for organic substances or to an analysis device suitable for inorganic substances. In addition, when the user cannot estimate the component to be analyzed in the sample, the effort of moving the sample is saved compared to the case where the sample is moved to the LIBS analysis device for LIBS analysis after the infrared spectroscopy analysis is performed in the infrared spectroscopy analysis device. Furthermore, the risk of inappropriate analysis, such as performing LIBS analysis first and then performing infrared spectrum analysis on a denatured sample, can be eliminated. As described above, according to the composite analysis device 100, a system capable of performing comprehensive analysis from organic matter to inorganic matter can be provided.

[0043] In particular, the composite analysis device 100 is convenient in that it can easily perform infrared spectroscopy and LIBS analysis on the same position (specific position S0) of the sample S. For example, infrared spectroscopy and LIBS analysis are often used to identify the composition of small foreign matter in the product. The size of the foreign matter is not limited to this, for example, there may be a maximum size of less than 100 μm, and as a more specific example, a case of 10 μm square. After focusing on such a small foreign matter for infrared spectroscopy and analyzing it, it is a very difficult task for the user to refocus on the exact same position for LIBS analysis. In addition, there is also the possibility that the user mistakenly focuses on a foreign matter different from the foreign matter that has been subjected to infrared spectroscopy analysis. However, in the composite analysis device 100, LIBS analysis can be performed on the same position as the infrared spectroscopy analysis by moving the position of the reflectors 31 and 32 after performing infrared spectroscopy analysis. Therefore, for the user, the effort of resetting the focus can be saved. In addition, infrared light analysis and LIBS analysis can be accurately performed on the same position.

[0044] The above mainly describes the case of analyzing solid samples in the composite analysis device 100. However, in the composite analysis device 100, liquid samples or gas samples can also be analyzed in the same manner. For example, in LIBS analysis, no complicated pre-treatment process is performed for samples containing any one of gas, liquid and solid, so that high-speed analysis can be performed. In particular, high-temperature plasma (e.g., 15000K to 30000K) is generated by laser, so not only metal elements can be measured at the order of 1ppm, but also halogens that are difficult to detect in other emission spectrometry analyses can be measured at the order of 1ppm. In other words, in the composite analysis device 100, high-precision LIBS analysis can be performed on all gases, liquids and solids in a short time.

[0045] Furthermore, in the composite analysis device 100 , even for organic matter that is not suitable for LIBS analysis, infrared spectrum analysis suitable for analyzing the organic matter can be performed before the organic matter is denatured by LIBS analysis.

[0046] Therefore, by using the complex analysis device 100 , the user can identify the components contained in the sample with high accuracy regardless of whether the components in the sample are organic or inorganic.

[0047] In addition, since both infrared spectroscopy and LIBS analysis can be performed in one composite analysis device 100, the installation space of the device can be reduced compared to the case where two infrared spectrophotometers dedicated to infrared spectroscopy and two laser induced breakdown spectrometry analysis devices dedicated to LIBS analysis are installed. In addition, since the composite analysis device 100 can share components (such as a control device) required for both infrared spectroscopy and LIBS analysis, the component cost can be reduced compared to the case where two independent devices are manufactured.

[0048] [2. Configuration of Analyzer According to Modification 1]

[0049] The analysis device 101 according to the above-described embodiment is configured to perform infrared spectroscopy analysis on reflected light from the sample S. However, the analysis device 101A according to the first modification is configured to perform infrared spectroscopy analysis on transmitted light from the sample S.

[0050] Figure 3 It is a diagram showing the structure of an analysis device 101A according to Modification 1 and a first optical path during infrared spectrum analysis.

[0051] Reference Figure 3 The position of the infrared light source 10A and the structure of the sample holder 5A of the analysis device 101A involved in the modification 1 are different from those of the analysis device 101. In addition, the reflection mirrors 38 to 40 are added to the analysis device 101A. With the above structural changes, the first optical path 15A of the analysis device 101A during infrared analysis is different from the first optical path 15 of the analysis device 101.

[0052] The sample holder 5A is configured to be able to obtain infrared light transmitted from the sample S placed in the sample holder 5A. Figure 3 In the example of FIG. 5 , the sample holder 5A is a sample stand having a through hole 51A. If the sample holder 5A is used, the sample holder 5A can be moved from a predetermined direction (in Figure 3 The infrared light 1511A, 1511A' passing through the through hole 51A is incident on the sample S. Then, the infrared light 1521A, 1521A' passing through the sample S is directed to the side opposite to the predetermined direction (in the direction of Figure 3 The middle is above) and shoots out.

[0053] The reflecting mirrors 38 to 40 are parabolic mirrors whose positions are fixed.

[0054] The infrared light source 10A is arranged on the side opposite to the sample holder 5A with respect to the reflectors 38 to 40 (at Figure 3 The middle is the lower side).

[0055] In one embodiment, the infrared light source 10A and the reflectors 38 to 40 are configured to focus the intersection point (also referred to as “focus”) of the incident light on a specific position S0A of the sample S. The specific position S0A is, for example, a position on the surface of the sample S or a position near the surface where LIBS analysis can be performed. Figure 3 A more detailed description is given. Infrared light 1512A and infrared light 1512A' are emitted from the infrared light source 10A, infrared light 1512A is reflected by the reflectors 39 and 38 to become infrared light 1511A, and infrared light 1512A' is reflected by the reflectors 39 and 40 to become infrared light 1511A'. Moreover, infrared light 1511A and 1511A' are set so that the intersection is focused at a specific position S0A. Each infrared light in the infrared light 1512A and 1512A' emitted from the infrared light source 10A is, for example, an infrared light beam having a specified beam diameter and power density. The beam diameter and power density are set in a manner to have a beam intensity sufficient for analysis.

[0056] The transmitted light (infrared light 1521A, 1521A′) that has passed through the specific position S0A is reflected by the mirrors 37, 36, 34 and the mirrors 35, 36, 34, respectively, and then enters the detector 11.

[0057] In addition, the infrared light emitted from the infrared light source 10A may be, for example, an infrared light beam having a diameter D. In this case, the light beam is reflected in a left-right split manner at the reflector 39. Then, the two split light beams are respectively reflected by the reflectors 38 and 40, and the intersection is focused at a specific position S0A. Then, the transmitted light of the infrared light that has passed through the specific position S0A is respectively reflected by the reflectors 37, 36, 34 and the reflectors 35, 36, 34, and then incident on the detector 11.

[0058] As described above, by using the analysis device 101A according to the modification 1, infrared spectrum analysis can be performed on the transmitted light of infrared light. Figure 2 Therefore, the analysis device 101A according to the first modification can provide a system capable of performing comprehensive analysis from organic matter to inorganic matter, similarly to the analysis device 101 according to the embodiment.

[0059] In particular, the analysis device 101A involved in the modification example 1 is suitable for analyzing a sample S with a high infrared light transmittance, and can analyze the sample S with a high infrared light transmittance with high precision. On the other hand, the analysis device 101 involved in the embodiment is suitable for analyzing a sample S with a high infrared light reflectance, and can analyze the sample S with a high infrared light reflectance with high precision.

[0060] In addition, the analysis device 101A according to the first modification has the advantage of being able to easily increase the diameter of the infrared light irradiated to the sample S. In the LIBS analysis, the luminous light generated from the components near the sample surface is detected. Therefore, the infrared light is emitted from the sample S on the same side (at the same side) of the XY plane passing through the specific position S0 of the sample S. Figure 2 The structure of setting the laser light source 20 and the beam splitter 21 is simple and preferred (refer to Figure 2 In addition, in order to perform infrared spectroscopy analysis of reflected light of infrared light at the same specific position S0 as LIBS, the infrared light source 10 and the detector 11 are also arranged on the same side as the laser light source 20 and the spectrometer 21 (at Figure 1 The structure of the upper part is simple and preferred (refer to Figure 1 On the other hand, in order to detect the transmitted light of infrared light for infrared spectrum analysis, the infrared light source 10 is set on the side opposite to the detector 11, the laser light source 20 and the spectrometer 21 (at Figure 3 The structure of the bottom is simple and preferred (refer to Figure 3 ). Thus, in the analysis device 101A, unlike the analysis device 101, there is no need to arrange components (e.g., the reflectors 31, 33) other than the reflectors 38 to 40 for focusing on the specific position S0A in the space between the infrared light source 10A and the sample S. Therefore, in the analysis device 101A, it is easy to configure so that infrared light with a large diameter is incident on the sample S. Thus, the amount of infrared light irradiated to the sample S and detected by the detector 11 can be increased, thereby improving the analysis accuracy.

[0061] On the other hand, the analysis device 101 according to the embodiment can use components required for LIBS analysis and / or infrared light detection (eg, mirrors 35 to 36 ) as components required for incident infrared light on the sample S, thereby having the advantage of being able to reduce component costs.

[0062] [3. Processing related to the analysis method involved in the embodiment]

[0063] Figure 4 is a flowchart showing the processing related to the analysis method involved in the embodiment. In one embodiment, Figure 4 The processing is implemented by the control device 90.

[0064] In steps (hereinafter referred to as “ST”) 02 to ST06 , the control device 90 irradiates the sample S with infrared light to perform infrared spectrum analysis.

[0065] In ST02, the control device 90 controls a mirror driving mechanism (not shown) to arrange the plurality of mirrors 31 to 37 at Figure 1 The first position is shown.

[0066] In ST04, the control device 90 irradiates the infrared light generated by the infrared light source 10 to the specific position S0 of the sample S. In one embodiment, the control device 90 first controls the infrared light source 10 to generate infrared light. The infrared light generated by the infrared light source 10 passes through the first optical path 15 formed by the reflector arranged at the first position. More specifically, the infrared light generated by the infrared light source 10 is incident on the specific position S0 of the sample S after being reflected by the reflectors 33, 36, and 35 in sequence. Moreover, the infrared light emitted from the specific position S0 is incident on the detector 11 after being reflected by the reflectors 37, 36, and 34 in sequence. The specific position S0 is the position that becomes the object of analysis. In one embodiment, the specific position S0 corresponds to a small foreign matter in the product discovered by the user through naked eye observation or microscope observation.

[0067] In ST06, the control device 90 performs infrared spectrum analysis on the infrared light emitted from the specific position S0 to obtain first analysis data. The first analysis data is, for example, an infrared spectrum.

[0068] In ST08 to ST12 , the control device 90 irradiates the sample S with laser light to perform LIBS analysis.

[0069] In ST08 , the control device 90 controls a mirror driving mechanism (not shown) to arrange the plurality of mirrors at a second position different from the first position.

[0070] In ST10, the control device 90 irradiates the laser light generated by the laser light source 20 to the specific position S0. In one embodiment, the control device 90 first controls the laser light source 20 to generate the laser light. The laser light generated by the laser light source 20 passes through the second optical path 25 formed by the reflector arranged at the second position. More specifically, the laser light generated by the laser light source 20 is incident on the specific position S0 of the sample S after being reflected by the reflectors 31, 36, and 35 in sequence. Then, the luminous light emitted from the specific position S0 is incident on the spectrometer 21 after being reflected by the reflectors 37, 36, 34, and 32 in sequence.

[0071] In ST12, the control device 90 obtains second analysis data obtained by performing LIBS analysis on the luminescent light generated at the specific position S0. The second analysis data is, for example, a spectrum of the luminescent light.

[0072] In ST14, the control device 90 identifies the components of the specific position S0 based on the first analysis data obtained by infrared spectrum analysis and the second analysis data obtained by LIBS analysis. Thus, for example, the components of foreign matter in the product can be identified. For example, the organic component corresponding to the peak of the infrared spectrum can be identified with high precision. On the other hand, the inorganic component corresponding to the peak of the luminescent light spectrum can be identified with high precision.

[0073] As mentioned above, in Figure 4 In the process of LIBS analysis, infrared spectroscopy analysis is performed before LIBS analysis. Therefore, infrared spectroscopy analysis can be performed on the components before denaturation due to LIBS analysis. As a result, whether the components to be analyzed are organic, inorganic, or both organic and inorganic, accurate component identification can be easily performed. Therefore, a system capable of performing comprehensive analysis from organic to inorganic substances can be provided.

[0074] In addition, Figure 4 In ST02 to ST06 of FIG. 1 , the control device 90 performs infrared spectroscopy analysis on the reflected light emitted from the sample S. However, this process may be replaced by the control device 90 performing infrared spectroscopy analysis on the transmitted light emitted from the sample S.

[0075] [4. Processing Related to the Analysis Method According to Modification 2]

[0076] The analysis method according to Modification 2 includes a process in which, when the control device 90 has information on the component to be analyzed, the control device 90 determines to execute one of the infrared spectroscopic analysis and the LIBS analysis, or to execute both the infrared spectroscopic analysis and the LIBS analysis based on the information.

[0077] Figure 5 FIG. 1 is a flowchart showing the processing related to the analysis method involved in Modification Example 2. In one embodiment, Figure 5 The processing is implemented by the control device 90.

[0078] In ST010, the control device 90 acquires information related to the component to be analyzed. The information related to the component to be analyzed is, for example, the name of a substance that is a candidate for the component to be analyzed. For example, a user operates an input device (not shown) of the control device 90 to input information related to the component to be analyzed, and the control device 90 acquires the information inputted through the input device.

[0079] In ST011, the control device 90 determines whether the component to be analyzed may contain an organic substance based on the input information. Specifically, for example, the control device 90 determines whether the candidate substance names of the component to be analyzed include a substance name corresponding to an organic substance. The substance name corresponding to an organic substance refers to a substance name indicating that the substance is an organic substance, for example, the name of an organic substance.

[0080] When the component to be analyzed may contain organic matter ( ST011 : YES), the control device 90 advances the process to ST02 . Figure 5 The processing of ST02~ST06 and Figure 4 The processing of ST02 to ST06 is the same.

[0081] Following the processing of ST06 or when the component to be analyzed cannot contain organic matter (ST011: "No"), in ST07, the control device 90 determines whether the component to be analyzed can contain inorganic matter based on the input information. Specifically, for example, the control device 90 determines whether the name of a substance corresponding to an inorganic substance is included in the candidate names of the component to be analyzed. The name of a substance corresponding to an inorganic substance refers to a name of a substance indicating that the substance is an inorganic substance, for example, the name of an inorganic substance.

[0082] When the component to be analyzed may contain an inorganic substance ( ST07 : YES), the control device 90 advances the process to ST08 . Figure 5 The processing of ST08 to ST12 Figure 4 The processing of ST08 to ST12 is the same.

[0083] Following the processing in ST12 or when the component to be analyzed is unlikely to contain inorganic substances (ST07: No), in ST14A, the control device 90 identifies the component at the specific position S0 based on the analysis data obtained in ST06 and / or ST12.

[0084] As mentioned above, Figure 5 The processing includes steps ST010, ST011, and ST07 of determining whether to perform one of steps ST02 to ST06 for infrared spectroscopy and steps ST08 to ST12 for LIBS analysis, or both steps ST02 to ST06 for infrared spectroscopy and steps ST08 to ST12 for LIBS analysis, based on information related to the components of the sample to be analyzed. Thus, the user can shorten the time for performing obviously unnecessary analysis. Therefore, in a system capable of performing comprehensive analysis from organic matter to inorganic matter, it is expected that the efficiency of analysis can be further improved.

[0085] Furthermore, in ST010 , when the user does not input a substance name as a candidate for the component to be analyzed, it may be determined that the component to be analyzed may include both organic and inorganic substances, and infrared spectrum analysis and LIBS analysis may be performed.

[0086] In addition, the user can also more directly input information on whether the component to be analyzed may contain organic matter or inorganic matter. Similarly, the user can also input instructions on whether to perform infrared spectroscopy analysis or LIBS analysis. Furthermore, in the case where the component to be analyzed is determined for each type of sample, the user can also input the type of the sample.

[0087] [Way]

[0088] It will be understood by those skilled in the art that the above-described multiple exemplary embodiments are specific examples of the following aspects.

[0089] (Item 1) An analysis method according to one embodiment is an analysis method performed in a composite analysis device capable of performing infrared spectroscopy analysis based on infrared spectroscopy and LIBS analysis based on laser-induced breakdown spectroscopy analysis on a sample. The analysis method includes the following steps: irradiating the sample with infrared rays to perform infrared spectroscopy analysis; irradiating the sample with laser to perform LIBS analysis; and identifying the components of the sample based on first analysis data obtained by infrared spectroscopy analysis and second analysis data obtained by LIBS analysis. The step of performing infrared spectroscopy analysis is performed before the step of performing LIBS analysis.

[0090] According to the analysis method described in the first item, infrared spectroscopy is performed before LIBS analysis. Therefore, infrared spectroscopy can be performed on components before denaturation due to LIBS analysis. Thus, whether the components to be analyzed are organic, inorganic, or both organic and inorganic, accurate component identification can be easily performed. Therefore, a system capable of performing comprehensive analysis from organic to inorganic can be provided.

[0091] (Item 2) In the analysis method described in Item 1, the step of performing infrared spectroscopy analysis includes the step of irradiating infrared light generated by an infrared light source to a specific position of the sample. The step of performing LIBS analysis includes the step of irradiating laser light generated by a laser light source to a specific position.

[0092] According to the analysis method described in the second item, it is easy to analyze the same position (specific position) of the sample in the infrared spectrum analysis and the LIBS analysis.

[0093] (Item 3) In the analysis method described in Item 2, the composite analysis device further includes a plurality of reflectors. The step of performing infrared spectroscopy analysis also includes the step of configuring the plurality of reflectors at a first position. The step of performing LIBS analysis also includes the step of configuring the plurality of reflectors at a second position different from the first position. A first optical path is formed at the first position. In the first optical path, infrared light generated from an infrared light source is incident on a specific position, and infrared light emitted from the specific position is incident on a detector. A second optical path is formed at the second position. In the second optical path, laser light generated from a laser light source is incident on a specific position, and luminous light generated at the specific position is incident on a spectrometer.

[0094] According to the analysis method described in the third aspect, the same position (specific position) of the sample can be analyzed in infrared spectrum analysis and LIBS analysis by a simple configuration and control in which the reflection mirror is moved to switch the optical path.

[0095] (Item 4) In the analysis method described in any one of Items 1 to 3, the step of performing infrared spectroscopy includes the step of performing infrared spectroscopy of reflected light from the sample or the step of performing infrared spectroscopy of transmitted light from the sample.

[0096] In the case where the analysis method described in the fourth item includes the step of performing infrared spectroscopy analysis of reflected light, samples with high reflectivity of infrared light can be analyzed with high precision. In addition, in that the components required for LIBS analysis and / or detection of infrared light can be used as components required for incident infrared light on the sample, the cost of components can be reduced. On the other hand, in the case where the analysis method described in the fourth item includes the step of performing infrared spectroscopy analysis of transmitted light, samples with high transmittance of infrared light can be analyzed with high precision. In addition, it is easy to make the diameter of the infrared light irradiated to the sample large.

[0097] (Fifth Item) In the analysis method described in any one of Items 1 to 4, the following steps are also included: based on information related to the component of the sample that becomes the analysis object, determining to execute one of the steps of performing infrared spectroscopy analysis and the steps of performing LIBS analysis, or to execute both the steps of performing infrared spectroscopy analysis and the steps of performing LIBS analysis.

[0098] According to the analysis method described in the fifth item, in a system capable of performing comprehensive analysis from organic matter to inorganic matter, further improvement in analysis efficiency can be expected.

[0099] (Item 6) Another embodiment of the composite analysis device is a composite analysis device including a sample holder, an infrared light source, a detector, a laser light source, a spectrometer, and a control device. A sample is set in the sample holder. The infrared light source generates infrared light to be irradiated onto the sample. The detector detects infrared light emitted from the sample by irradiation with the infrared light. The laser light source generates laser light to be irradiated onto the sample. The spectrometer spectrometers the luminous light generated in the sample by irradiation with the laser light. The control device obtains first analysis data obtained by performing infrared spectroscopy analysis on the infrared light emitted from the sample and second analysis data obtained by performing LIBS analysis on the luminous light generated in the sample. The control device identifies the components of the sample based on the first analysis data and the second analysis data. The control device irradiates the sample with infrared light before irradiating the sample with the laser light.

[0100] According to the composite analysis device described in the sixth item, when the component to be analyzed in the sample is an organic substance, the component can be identified with high precision based on the first analysis data obtained by infrared spectroscopy. On the other hand, even when the component to be analyzed in the sample is an inorganic substance, the component can be identified with high precision based on the second analysis data obtained by LIBS analysis. Thus, the user can save the effort of estimating the component to be analyzed in the sample before starting to analyze the sample and considering whether to provide it to an analysis device suitable for organic substances or to an analysis device suitable for inorganic substances. In addition, the risk of inappropriate analysis such as performing LIBS analysis first and then performing infrared spectroscopy analysis on the denatured sample can be eliminated. As described above, a system capable of performing comprehensive analysis from organic to inorganic substances can be provided.

[0101] (Item 7) In the composite analysis device described in Item 6, the composite analysis device further includes a plurality of reflectors. The positions of the plurality of reflectors can be a first position and a second position. A first optical path is formed in the first position. In the first optical path, infrared light generated from an infrared light source is incident on a specific position, and infrared light emitted from the specific position is incident on a detector. A second optical path is formed in the second position. In the second optical path, laser light generated from a laser light source is incident on a specific position, and the luminous light generated at the specific position is incident on a spectrometer.

[0102] According to the composite analysis device described in the seventh item, LIBS analysis can be performed on the same position as infrared spectroscopy analysis by moving the position of the reflector after infrared spectroscopy analysis. Therefore, for the user, the time of resetting the focus can be saved. In addition, infrared light analysis and LIBS analysis can be accurately performed on the same position.

[0103] Although the embodiments of the present invention have been described, the embodiments disclosed this time should be considered to be illustrative in all aspects and not restrictive. The scope of the present invention is indicated by the claims, and is intended to include all modifications within the meaning and scope equivalent to the claims.

Claims

1. An analysis method is performed in a composite analysis device capable of performing infrared spectroscopy analysis based on infrared spectroscopy and laser induced breakdown spectroscopy analysis based on laser induced breakdown spectroscopy on a sample, comprising the following steps: irradiating the sample with infrared rays to perform the infrared spectrum analysis; irradiating the sample with laser light to perform the laser induced breakdown spectroscopy analysis; and identifying the components of the sample based on the first analysis data obtained by the infrared spectrum analysis and the second analysis data obtained by the laser induced breakdown spectroscopy analysis, Wherein, the step of performing the infrared spectrum analysis is performed before the step of performing the laser induced breakdown spectrum analysis.

2. The analysis method according to claim 1, wherein The step of performing the infrared spectrum analysis includes the step of irradiating infrared light generated by an infrared light source to a specific position of the sample, The step of performing the laser induced breakdown spectroscopy includes the step of irradiating laser light generated from a laser light source to the specific position.

3. The analysis method according to claim 2, wherein: The composite analysis device further comprises a plurality of reflecting mirrors. The step of performing the infrared spectrum analysis further includes the step of configuring the plurality of reflectors at a first position, The step of performing the laser induced breakdown spectroscopy analysis further includes the step of configuring the plurality of reflectors at a second position different from the first position, When in the first position, a first optical path is formed, In the first optical path, the infrared light generated by the infrared light source is incident on the specific position, and the infrared light emitted from the specific position is incident on the detector. In the second position, a second optical path is formed. In the second optical path, the laser light generated from the laser light source is incident on the specific position, and the luminous light generated at the specific position is incident on the spectrometer.

4. The analysis method according to any one of claims 1 to 3, wherein The step of performing the infrared spectrum analysis includes the step of performing the infrared spectrum analysis of the reflected light from the sample or the step of performing the infrared spectrum analysis of the transmitted light from the sample.

5. The analysis method according to any one of claims 1 to 3, wherein The following steps are also included: Based on information about the component to be analyzed of the sample, it is determined whether to perform either the infrared spectroscopic analysis or the laser induced breakdown spectroscopic analysis, or whether to perform both the infrared spectroscopic analysis and the laser induced breakdown spectroscopic analysis.

6. A composite analysis device comprising: A sample holder for setting the sample; an infrared light source that generates infrared light to irradiate the sample; a detector that detects infrared light emitted from the sample by the irradiation of the infrared light; a laser light source that generates laser light to irradiate the sample; A spectrometer for splitting the luminescent light generated on the sample by the irradiation of the laser light; and Control device, in, The control device performs the following actions: Acquiring first analysis data obtained by performing infrared spectrum analysis on the infrared light emitted from the sample and second analysis data obtained by performing laser induced breakdown spectrum analysis on the luminescent light generated in the sample; and Based on the first analysis data and the second analysis data, the components of the sample are identified, and the control device irradiates the sample with infrared light before irradiating the sample with laser light.

7. The composite analysis device according to claim 6, wherein: The composite analysis device further comprises a plurality of reflecting mirrors. The positions of the plurality of reflectors can adopt a first position and a second position, When in the first position, a first optical path is formed, In the first optical path, the infrared light generated by the infrared light source is incident on a specific position, and the infrared light emitted from the specific position is incident on the detector. In the second position, a second optical path is formed. In the second optical path, the laser light generated from the laser light source is incident on the specific position, and the luminous light generated at the specific position is incident on the spectrometer.

Images