CN119780138A - Analytical testing system and analytical testing method - Google Patents
Analytical testing system and analytical testing method Download PDFInfo
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- CN119780138A CN119780138A CN202411798832.2A CN202411798832A CN119780138A CN 119780138 A CN119780138 A CN 119780138A CN 202411798832 A CN202411798832 A CN 202411798832A CN 119780138 A CN119780138 A CN 119780138A
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Abstract
The embodiment of the application relates to the technical field of testing the chemical properties of materials, in particular to an analysis and test system and an analysis and test method, which are suitable for analyzing and testing samples, wherein the analysis and test system comprises a laser-induced breakdown spectroscopy analysis module, a laser-induced breakdown spectroscopy analysis module and a laser-induced breakdown spectroscopy analysis module, wherein the laser-induced breakdown spectroscopy analysis module is used for determining the elemental composition and the content of the sample; the laser-induced breakdown spectroscopy analysis module and the X-ray fluorescence analysis module are respectively and fixedly connected with the analysis test system body. According to the embodiment of the application, the laser-induced breakdown spectroscopy analysis module and the X-ray fluorescence analysis module are respectively and fixedly connected with the analysis test system body, so that the laser-induced breakdown spectroscopy analysis and the X-ray fluorescence analysis can be respectively carried out on the same sample in the same cavity on a single device, the elemental composition, the content and the chemical attribute of the sample are determined, and the accuracy and the efficiency of the analysis test result of the sample are improved.
Description
Technical Field
The application relates to the technical field of testing material chemical properties, in particular to an analysis and test system and an analysis and test method.
Background
This section is merely provided for background information related to the present application and does not necessarily constitute prior art.
Analysis and testing of samples is required in various fields of industrial production, chemical research, biological medicine and the like. In performing analytical testing, it is necessary to test the elemental composition of the sample and its content. In general, the use of the analytical testing procedure described above requires the elemental composition of the sample and its content to be accurately determined. In the prior art, the analysis and test of the element content of the sample has the defects of inaccurate test results and low analysis efficiency.
Disclosure of Invention
The following presents a simplified summary of the application in order to provide a basic understanding of some aspects of the application. It should be understood that this summary is not an exhaustive overview of the application. It is not intended to identify key or critical elements of the application or to delineate the scope of the application. Its purpose is to present some concepts in a simplified form as a prelude to the more detailed description that is discussed later.
In a first aspect, embodiments of the present application provide an analytical test system adapted for analytical testing of a sample, the analytical test system comprising a laser induced breakdown spectroscopy module configured to determine elemental composition of the sample and its content, an X-ray fluorescence analysis module configured to determine chemical properties of the sample, an analytical test system body forming a sample test cavity in which the sample is disposed and in which the sample is capable of changing position, wherein laser light emitted by the laser induced breakdown spectroscopy module irradiates the sample in the sample test cavity and collects light emitted by the sample that generates a high temperature plasma after irradiation and transmits the light emitted by the sample to the laser induced breakdown spectroscopy module for detection thereby determining elemental composition of the sample and its content, and X-rays emitted by the X-ray fluorescence analysis module irradiate the sample in the sample test cavity and detect fluorescent X-rays generated after irradiation thereby determining chemical properties of the sample.
According to the embodiment of the application, the laser-induced breakdown spectroscopy analysis module and the X-ray fluorescence analysis module are respectively and fixedly connected with the analysis test system body, so that the laser-induced breakdown spectroscopy analysis and the X-ray fluorescence analysis are respectively carried out on the same sample in the same cavity on a single device, and the position of the sample can be adjusted in the same cavity in the test process, so that the sample does not need to be put in again when the laser-induced breakdown spectroscopy analysis module and the X-ray fluorescence analysis module are respectively used, the influence on the analysis result of the sample due to different test environments is avoided, the analysis test flow is simplified, and the accuracy of the analysis result and the analysis test efficiency are improved.
In a second aspect, an embodiment of the present application provides an analytical test method, which is suitable for analyzing and testing a sample, and the analytical test system provided by the first aspect of the present application is used for the analytical test method, and the analytical test method includes the steps of S1, obtaining a laser-induced breakdown spectroscopy spectrogram of the sample by using a laser-induced breakdown spectroscopy analysis module, S2, obtaining an X-ray fluorescence spectroscopy spectrogram of the sample by using an X-ray fluorescence analysis module, and S3, determining properties of the sample according to the laser-induced breakdown spectroscopy spectrogram and the X-ray fluorescence spectroscopy spectrogram.
According to the embodiment of the application, the analysis and test method is provided, the laser-induced breakdown spectroscopy analysis and the X-ray fluorescence analysis are respectively carried out on the same sample, and the element composition, the element content and the chemical attribute of the sample are determined by combining the analysis results of the two methods, so that the accuracy of the analysis results is improved.
Drawings
To further clarify the above and other advantages and features of the present application, a more particular description of the application will be rendered by reference to the appended drawings. The accompanying drawings are incorporated in and form a part of this specification, along with the detailed description that follows. Elements having the same function and structure are denoted by the same reference numerals. It is appreciated that these drawings depict only typical examples of the application and are therefore not to be considered limiting of its scope.
FIG. 1 is a schematic diagram of an analytical test system according to one embodiment of the present application;
FIG. 2 is a side view of an analytical test system according to one embodiment of the present application;
FIG. 3 is a partial cross-sectional view of an analytical test system according to one embodiment of the present application;
FIG. 4 is an enlarged schematic view of a portion of an analytical test system according to one embodiment of the present application;
FIG. 5 is a flow chart of an analytical test method according to one embodiment of the present application.
It should be noted that the drawings are not necessarily to scale, but are merely shown in a schematic manner that does not affect the reader's understanding.
Reference numerals illustrate:
1. analyzing the test system;
10. A laser-induced breakdown spectroscopy analysis module; 11, a laser emitter, 12, a spectrometer, 13, a light guide piece, 14, a first light condensation piece;
20. the X-ray fluorescence analysis module, the 21, the X-ray source, the 22, the X-ray energy detector;
30. analyzing a test system body; 31, a sample testing cavity, 32, a structure for projecting light;
40. A light path channel 41, a horizontal channel;
50. a first fixing member;
60. a second fixing member;
70. an optical fiber;
80. 81, support columns 82, support body;
90. stage 91, supporting part 92, rod part;
100. Coordinate platform, 101, first platform, 102, second platform, 1021, coordinate adjusting component, 10211, transverse coordinate adjusting piece, 10212, longitudinal coordinate adjusting piece, 10213, normal coordinate adjusting piece, 102131, extension part, 102132, adjusting part, 103, protruding part, 104, platform connecting piece;
110. A bellows;
120. a vacuum module;
130. A purge module;
140. and a measurement and control system.
Detailed Description
Exemplary embodiments of the present application will be described hereinafter with reference to the accompanying drawings. In the interest of clarity and conciseness, not all features of an actual implementation are described in this specification. It will of course be appreciated that in the development of any such actual embodiment, numerous implementation-specific decisions must be made in order to achieve the developer's specific goals, such as compliance with system-and business-related constraints, and that these constraints will vary from one implementation to another. Moreover, it will be appreciated that such a development effort might be complex and time-consuming, but would nevertheless be a routine undertaking for those of ordinary skill in the art having the benefit of this disclosure.
It should be noted here that, in order to avoid obscuring the present application due to unnecessary details, only the device structures and/or processing steps closely related to the solution according to the present application are shown in the drawings, while other details not greatly related to the present application are omitted.
It is to be noted that unless otherwise defined, technical or scientific terms used herein should be taken in a general sense as understood by one of ordinary skill in the art to which the present application belongs.
In the description of the embodiments of the present application, the meaning of "plurality" is at least two, for example, two, three, etc., unless explicitly defined otherwise.
In various fields such as industrial production, chemical research, and biological medicine, analysis and test of a sample are required, and the elemental composition and the content of the sample are required to be accurately determined through the analysis and test.
The inventor of the application discovers that the device for analyzing and testing the element content of the sample can only realize single and specific analysis and test on the sample, and has the defects of inaccurate analysis and test results and low analysis efficiency.
Based on this, an embodiment of the present application provides an analytical test system suitable for analytical testing of a sample, FIG. 1 is a schematic diagram of an analytical test system according to one embodiment of the present application. FIG. 2 is a side view of an analytical test system according to one embodiment of the present application. As shown in fig. 1 and 2, the analysis test system 1 comprises a laser-induced breakdown spectroscopy module 10 configured to determine the elemental composition of a sample and the content thereof, an X-ray fluorescence spectroscopy module 20 configured to determine the chemical properties of the sample, an analysis test system body 30 configured to form a sample test cavity 31, the sample being disposed in the sample test cavity 31 and capable of changing position within the sample test cavity 31, wherein the laser-induced breakdown spectroscopy module 10 and the X-ray fluorescence spectroscopy module 20 are configured to be fixedly connected with the analysis test system body 30, respectively, the laser emitted by the laser-induced breakdown spectroscopy module 10 irradiates the sample within the sample test cavity 31 and collects the emitted light of the sample that generates a high temperature plasma after the sample is irradiated and transmits the emitted light to the laser-induced breakdown spectroscopy module 10 for detection thereof to determine the elemental composition of the sample and the content thereof, and the X-ray emitted by the X-ray fluorescence spectroscopy module 20 irradiates the sample within the sample test cavity 31 and detects the sample that generates fluorescent X-rays after the sample is irradiated to determine the chemical properties of the sample.
According to the embodiment of the application, the laser-induced breakdown spectroscopy analysis module and the X-ray fluorescence analysis module are respectively and fixedly connected with the analysis test system body, so that the laser-induced breakdown spectroscopy analysis and the X-ray fluorescence analysis are respectively carried out on the same sample in the same cavity on a single device, and the position of the sample can be adjusted in the same cavity in the test process, so that the sample does not need to be put in again when the laser-induced breakdown spectroscopy analysis module and the X-ray fluorescence analysis module are respectively used, the influence on the analysis result of the sample due to different test environments is avoided, the analysis test flow is simplified, and the accuracy of the analysis result and the analysis test efficiency are improved.
Fig. 3 is a partial cross-sectional view of an analytical test system 1 according to one embodiment of the present application. As shown in fig. 1 and 3, in some embodiments, the analysis test system body 30 includes a plurality of walls that form the sample test cavity 31, and a portion of the laser-induced breakdown spectroscopy module 10 and a portion of the X-ray fluorescence analysis module 20 are fixedly connected to different ones of the plurality of walls, respectively, so as to avoid the laser-induced breakdown spectroscopy module 10 from contacting the X-ray fluorescence analysis module 20 during the analysis test, which may interfere with the laser-induced breakdown spectroscopy and the X-ray fluorescence analysis of the sample.
As shown in fig. 3, in some embodiments, analytical test system 1 also includes an optical path channel 40, a first mount 50, a second mount 60, and an optical fiber 70. The analytical test system body 30 includes a plurality of walls that form a sample test cavity 31. The optical path channel 40 is provided in fixed connection with one of the walls and a structure 32 for projecting light is provided at the wall so that laser light emitted from the laser-induced breakdown spectroscopy module 10 can irradiate the sample provided in the sample test cavity 31. The first fixing member 50 is provided in fixed connection with one of the walls and in fixed connection with a portion of the X-ray fluorescence analysis module 20 so that X-rays emitted from the X-ray fluorescence analysis module 20 can be irradiated into a sample provided in the sample test cavity 31. A portion of the X-ray fluorescence analysis module 20 is fixedly disposed on one of the plurality of walls opposite to one of the plurality of walls on which the first fixture 50 is disposed. The second fixture 60 is fixedly disposed on one of the plurality of walls and is configured to secure the optical fiber 70 such that the optical fiber 70 receives light reflected from the sample by the laser light and transmits it to the laser induced breakdown spectroscopy module 10. By arranging the optical path channel 40, the first fixing member 50 and the second fixing member 60 on one of the different walls of the analysis and test system body 30, the cross mutual interference of the optical paths of the laser light, the X-ray light and the light reflected by the laser light is avoided, so that the irradiation of the laser light and the X-ray light to the sample in the sample test cavity 31 and the transmission of the reflected light of the laser light are ensured.
In some embodiments, the structure 32 that projects light may be a quartz window for introducing laser light into the cavity from the atmospheric side.
In some embodiments, a second mount 60 communicates with the sample testing cavity 31, the second mount 60 being configured to mount the optical fiber 70 such that the optical fiber 70 enters the sample testing cavity 31 through the second mount 60. In some embodiments, the second securing member 60 may be a through flange.
In some embodiments, the fiber 70 species may be a silica fiber.
As shown in fig. 1 and 3, in some embodiments, the analytical test system 1 further includes a support 80, the support 80 being juxtaposed with the analytical test system body 30. The laser-induced breakdown spectroscopy module 10 comprises a laser emitter 11, a spectrometer 12 and a light guide member 13, wherein the laser emitter 11 is arranged on a support member 80, the light guide member 13 is arranged in a light path channel 40, the spectrometer 12 is arranged outside an analysis and test system body 30, laser emitted by the laser emitter 11 irradiates the light guide member 13, irradiates a sample after being conducted by the light guide member 13, reflects the sample to an optical fiber 70, is conducted to the spectrometer 12 by the optical fiber 70, and is detected by the spectrometer 12. Specifically, by arranging the supporting member 80 in parallel with the analysis and test system body 30, the laser emitted by the laser emitter 11 arranged on the supporting member 80 can be emitted into the optical path channel 40 of the analysis and test system body 30, and the laser path is changed by the light guide member 13 arranged in the optical path channel 40, so that the laser irradiates the sample, the composition of the emitted light generated by the sample after the laser irradiation is detected by the spectrometer 12, the elemental composition and content of the sample are obtained, and the laser-induced breakdown spectroscopy analysis of the sample is completed.
In some embodiments, the support 80 is provided with a plurality of support posts 81 and a support body 82, the plurality of support posts 81 are used to support the support body 82, the support body 82 is provided with a plurality of walls, and the laser transmitter 11 is disposed on the wall of the support body 82 opposite to the analytical test system body 30. In some embodiments, a horizontal channel 41 is formed in the opposite wall of the light path channel 40 from the support body 82 in communication with the light path channel 40. The horizontal channel 41 is juxtaposed with the laser transmitter 11, and the laser outlet of the laser transmitter 11 is collinear with the center of the horizontal channel 41. The laser light emitted from the laser emitter 11 can enter the optical path channel 40 through the horizontal channel 41.
In some embodiments, the laser transmitter 11 outputs laser light with a wavelength of 1064nm, 532nm or other shorter wavelength (e.g., 256 nm), and the laser power may be selected to be 20-300 mJ for providing a high-energy monochromatic excitation light source.
In some embodiments, the light guide 13 is disposed upstream of the structure 32 that projects light, with the center of the light guide 13 collinear with the laser light outlet of the laser transmitter 11 and the center of the horizontal channel 41. Specifically, the laser light is irradiated to the light guide 13 through the horizontal channel 41, and the laser light path emitted from the laser emitter 11 is changed by the light guide 13 so that the laser light is irradiated to the sample.
In some embodiments, the light guide 13 may be a 45 degree mirror, and the 45 degree mirror is disposed at the light path channel 40 with a 45 degree angle, and reflects the horizontal laser light emitted from the laser emitter 11 into the vertical laser light, so that the laser light is irradiated to the sample.
In some embodiments, the laser-induced breakdown spectroscopy module 10 further includes a first light-focusing element 14, where the first light-focusing element 14 is disposed between the light-guiding element 13 and the light-projecting structure 32, so that the laser light passes through the light-projecting structure 32 and is focused on the sample surface inside the cavity. Unnecessary loss of laser energy is prevented, thereby ensuring effective irradiation of the sample by the laser. Specifically, the first condensing member 14 may be a convex lens.
In some embodiments, the laser-induced breakdown spectroscopy module 10 further includes a second light collector for collecting the emitted light generated by the laser irradiation at the sample surface and transmitting the emitted light to the optical fiber 70.
In some embodiments, the wavelength monitoring range of the spectrometer 12 may be selected based on the composition of the sample, avoiding interference with other wavelength ranges, and improving the analysis efficiency of the spectrometer 12.
As shown in fig. 1, in some embodiments, the X-ray fluorescence analysis module 20 includes an X-ray source 21 and an X-ray energy detector 22, the X-ray source 21 being disposed on one of the plurality of walls by a first mount 50, the X-ray energy detector 22 being fixedly disposed on one of the plurality of walls opposite the one of the plurality of walls on which the first mount 50 is disposed, the X-rays emitted by the X-ray source 21 illuminating the sample, and the X-rays reflected from the sample being detected by the X-ray energy detector 22. By arranging the X-ray source 21 and the X-ray energy detector 22 on one of the walls respectively, the X-ray source 21 and the X-ray energy detector 22 are prevented from contacting each other during the analysis and test, the normal operation of the X-ray source 21 and the X-ray energy detector 22 is disturbed, and the two walls respectively arranged are opposite to each other, so that the X-rays reflected by the sample can be detected by the X-ray energy detector 22 after the sample is irradiated by the X-rays.
In some embodiments, the first fixture 50 may be a flange interface for enabling a secure connection of the X-ray source 21 to one of the plurality of walls of the analytical test system body 30.
In some embodiments, the excitation voltage of the X-ray source 21 may be 20kV to 50kV, for example, 30kV.
In some embodiments, the X-ray energy detector 22 is used to detect the reflected X-ray composition of the sample, and obtain the chemical properties of the sample.
In some embodiments, the material of the detector of the X-ray source 21 may be selected according to the test requirements, for example, rhodium, silver, tungsten, etc.
As shown in fig. 3, in some embodiments, the X-ray source 21 and the X-ray energy detector 22 are disposed with their central extension at a predetermined angle and converge on the surface of the sample. The X-ray fluorescence spectrum analysis device is used for limiting the X-ray to irradiate the sample and the light path of the X-ray reflected by the sample, and preventing the interference to the accuracy of the X-ray fluorescence spectrum analysis of the sample due to the fact that the light path of the X-ray and the light path of the reflected X-ray are too close or too far.
In some embodiments, the X-ray source 21 forms an angle with the X-ray energy detector 22 in the range of 30-90, such as 45.
Fig. 4 is an enlarged schematic view of a portion of an analytical test system 1 according to one embodiment of the present application. As shown in fig. 3 and 4, in some embodiments, the analytical test system 1 further includes a stage 90, the sample being disposed on the stage 90, the stage 90 being disposed in sealing connection with the cavity and being capable of adjusting the position in three directions, transverse, longitudinal, and perpendicular to the transverse and longitudinal directions. The sample can be moved to the corresponding test position by the stage 90 when switching between laser induced spectroscopy and X-ray fluorescence spectroscopy.
As shown in fig. 3 and 4, in some embodiments, the stage 90 is formed with a support portion 91 and a lever portion 92, the support portion 91 being disposed directly above the lever portion 92, the lever portion 92 being for supporting the support portion 91. Wherein the support portion 91 and a portion of the stem portion 92 are disposed within the sample testing cavity 31, and the sample is disposed on the support portion 91.
As shown in fig. 4, in some embodiments, the analytical test system 1 further includes a coordinate platform 100 and a coordinate adjustment assembly 1021. The coordinate platform 100 comprises a first platform 101 and a second platform 102, the first platform 101 is arranged above the second platform 102, the horizontal relative positions of the first platform 101 and the second platform 102 are fixed, and the distance between the first platform 101 and the second platform 102 is adjustable. The coordinate adjusting assembly 1021 is disposed on the second platform 102, and is configured to move the sample in the sample testing chamber 31 without breaking the vacuum state of the chamber.
In some embodiments, the analytical test system body 30 is disposed on a first platform 101, and the first platform 101 and a second platform 102 are each formed with a through hole. Wherein, the first platform 101 through hole is communicated with the sample testing cavity 31, the second platform 102 through hole is larger than the first platform 101 through hole, and the rod 92 of the objective table 90 penetrates through the through holes of the first platform 101 and the second platform 102. Specifically, a protruding portion 103 is disposed below the through hole of the second platform 102, the vertical relative position of the protruding portion 103 and the second platform 102 is fixed, the horizontal relative position is adjustable, and the rod portion 92 of the stage 90 is fixed at the center of the bottom surface of the protruding portion 103.
In some embodiments, coordinate adjustment assembly 1021 includes lateral coordinate adjustment member 10211, longitudinal coordinate adjustment member 10212, and normal coordinate adjustment member 10213. The lateral coordinate adjusting member 10211 is disposed in the lateral direction of the boss 103, and the lateral coordinate adjusting member 10211 is configured to effect movement of the boss 103 in the lateral direction, and further effect movement of the lever 92 of the stage 90 in the lateral direction. The longitudinal coordinate regulating member 10212 is provided in the longitudinal direction of the boss 103 for effecting movement of the boss 103 in the longitudinal direction, and further effecting movement of the lever portion 92 of the stage 90 in the longitudinal direction. Normal coordinate adjusting member 10213 includes an extension 102131 and an adjustment portion 102132. The upper end of the extension part 102131 is fixedly connected with the first platform 101, the lower end part of the extension part 102131 extends into the adjusting part 102132, the upper end of the adjusting part 102132 is fixedly connected with the lower part of the second platform 102, and the adjusting part 102132 is used for adjusting the length of the extension part 102131 extending into the adjusting part 102132. Movement of the lever portion 92 of the stage 90 in the transverse and longitudinal vertical directions is achieved by varying the length of the extension 102131 extending into the adjustment portion 102132, thereby varying the height of the gap between the first stage 101 and the second stage 102. Movement of the stem 92 of the stage 90 in the three directions transverse, longitudinal and perpendicular to the transverse and longitudinal directions is achieved by the transverse coordinate adjustment member 10211, the longitudinal coordinate adjustment member 10212 and the normal coordinate adjustment member 10213, thereby achieving movement of the sample in the three directions transverse, longitudinal and perpendicular to the transverse and longitudinal directions.
In some embodiments, the coordinate platform 100 further includes a plurality of platform connectors 104, wherein the plurality of platform connectors 104 extend through the first platform 101 and the second platform 102 for improving stability of the coordinate platform 100.
As shown in fig. 1 and 3, in some embodiments, the analytical test system 1 further includes a bellows 110, where two ends of the bellows 110 are respectively connected with the stage 90 and the cavity in a sealing manner, so that the vacuum state in the cavity is maintained when the stage 90 adjusts the position of the sample. By arranging the bellows 110 in sealing connection with the stage 90 and the sample testing cavity 31, the stage 90 is arranged in the sample testing cavity 31 in airtight vacuum, so that the movement of the sample in the sample testing cavity 31 can be realized under the condition that the vacuum state of the sample testing cavity 31 is not damaged.
As shown in fig. 1, in some embodiments, the bellows 110 has an outer diameter dimension smaller than the through-hole of the second platform 102, preventing the bellows 110 from colliding with the second platform 102 when the distance between the first platform 101 and the second platform 102 is reduced.
As shown in fig. 1 and 3, in some embodiments, the analytical test system 1 further includes a vacuum module 120, the vacuum module 120 being configured to be fixedly connected to the analytical test system body 30 and configured to maintain the vacuum level of the sample test cavity 31 when tested with the laser induced breakdown spectroscopy module 10 to provide a vacuum environment required for performing laser induced breakdown spectroscopy analysis.
In some embodiments, a vacuum module 120 is disposed on one of the walls of the analytical test system body 30 and communicates with the sample test cavity 31 to regulate the vacuum of the sample test cavity 31.
In some embodiments, the vacuum module 120 may include a vacuum pump set, vacuum piping, vacuum gauges, solenoid valves, and the like. The vacuum pump unit is used for vacuumizing the sample testing cavity 31, the vacuum pipeline is connected with the vacuum pump unit and used for discharging gas pumped by the vacuum pump unit, the vacuum gauge is connected with the vacuum pipeline and used for measuring the vacuum degree of the sample testing cavity 31, and the electromagnetic valve is connected with the vacuum pipeline and used for controlling the opening and closing of the vacuum pipeline.
As shown in fig. 3, in some embodiments, the analysis test system 1 further includes a purge module 130, where the purge module 130 is fixedly connected to the analysis test system body 30, and is configured to purge the sample surface to remove impurities remaining on the sample surface when tested by the laser-induced breakdown spectroscopy analysis module 10, so as to avoid affecting the analysis result.
In some embodiments, the purge module 130 may include a gas source, piping, flow regulating valves, and sample nozzles. The device comprises a gas source, a pipeline, a flow regulating valve, a sample nozzle and a sample nozzle, wherein the gas source is used for providing purge gas, the pipeline is connected with the gas source and used for transmitting the purge gas provided by the gas source, the flow regulating valve is connected with the pipeline and used for controlling the flow of the purge gas in the pipeline so as to purge samples at different flow rates, and the sample nozzle is connected with the pipeline and aims at the sample surface so as to purge the sample surface.
As shown in fig. 1, in some embodiments, the analysis test system 1 further includes a measurement and control system 140, where the measurement and control system 140 can implement measurement and control of the laser-induced breakdown spectroscopy module 10, the X-ray fluorescence analysis module 20, the optical path channel 40, the coordinate platform 100, the sample test cavity 31, the vacuum module 120, and the purge module 130 in a communication manner.
In some embodiments, when performing laser induced spectroscopy, the measurement and control system 140 may control the coordinate adjustment assembly 1021 to move the sample in the sample testing chamber 31 synchronously along a predetermined path until the end of the laser induced spectroscopy process.
In some embodiments, when performing laser induced spectroscopy, the measurement and control system 140 may control the power switch of the vacuum pump assembly to start and stop the vacuum pump assembly, thereby implementing the vacuum state of the sample testing cavity 31.
In some embodiments, the measurement and control system 140 may synchronize the purging of the sample with the purge gas by controlling the flow regulating valve when performing laser-induced spectroscopy.
FIG. 5 is a flow chart of an analytical test method according to one embodiment of the present application. As shown in FIG. 5, an embodiment of the present application provides an analytical test method suitable for analytical testing of a sample, the analytical test method using the analytical test system 1 of any embodiment of the present application, the analytical test method comprising the steps of S1 obtaining a laser induced breakdown spectroscopy spectrogram of the sample using the laser induced breakdown spectroscopy module 10, S2 obtaining an X-ray fluorescence spectroscopy spectrogram of the sample using the X-ray fluorescence spectroscopy module 20, and S3 determining properties of the sample according to the laser induced breakdown spectroscopy spectrogram and the X-ray fluorescence spectroscopy spectrogram.
According to the analysis and test method provided by the embodiment of the application, the laser-induced breakdown spectroscopy analysis and the X-ray fluorescence analysis are respectively carried out on the same sample, and the element composition, the element content and the chemical attribute of the sample are determined by combining the analysis results of the two analysis methods, so that the accuracy of the analysis results is improved.
In some embodiments, the order of steps S1 and S2 may be adjusted according to the test requirements.
In some embodiments, after the step S3, the analysis results of the X-ray fluorescence analysis and the laser-induced breakdown spectroscopy analysis may be referred to each other and compared, so as to avoid a situation that an analysis result error is large when one of the methods fails, thereby improving the accuracy of the analysis result.
The embodiment of the application also provides an analysis and test method which is suitable for analyzing and testing the element beryllium in the rock, and comprises the following steps:
And S10, preparing a sample of the rock, wherein the sample comprises the element beryllium and the reference element.
S20, preparing a standard sample of rock with known composition, wherein the standard sample comprises reference elements and element beryllium, and the concentration of the reference elements and the element beryllium in the standard sample is known.
S30, acquiring an X-ray fluorescence spectrum of the standard sample, and determining the relation between the concentration of the reference element and the signal intensity of an X-ray peak according to the X-ray fluorescence spectrum.
And S40, acquiring an X-ray fluorescence spectrogram of the sample, and determining the concentration of the reference element in the sample according to the relationship determined in the step S30.
S50, obtaining a laser-induced breakdown spectrum of the standard sample, and determining sensitivity coefficients of the reference element and the element beryllium according to the laser-induced breakdown spectrum and the concentrations of the reference element and the element beryllium in the standard sample.
S60, obtaining a laser-induced breakdown spectrum of the sample, and determining the concentration of the element beryllium in the sample according to the laser-induced breakdown spectrum and the sensitivity coefficient of the reference element and the element beryllium determined in the step S50 and the concentration of the reference element in the sample.
The embodiment of the application respectively performs X-ray fluorescence spectrum analysis and laser-induced breakdown spectrum analysis on the sample containing the element beryllium and the reference element and the standard sample. The sensitivity coefficients of the reference element and the element beryllium are determined according to the analysis results of the two analysis methods, and the concentration of the element beryllium in the sample is corrected through the sensitivity coefficients of the reference element and the element beryllium, so that the accuracy of the analysis results is improved.
In some embodiments, in step S30, the concentration of the reference element in the standard sample as a function of its X-ray peak signal intensity corresponds to the following expression:
(1)。
In the formula, X-ray peak signal intensity representing a reference element in a standard sample; representing the concentration of the reference element in the standard sample; Representing a constant; Representing a constant. To determine the relationship of the X-ray peak signal intensity of the reference element in the standard sample to the concentration of the reference element in the standard sample.
In some embodiments, in step S40, the concentration of the reference element in the sample as a function of its X-ray peak signal intensity corresponds to the following expression:
(2)。
In the formula, An X-ray peak signal intensity representing a reference element in the sample; Representing the concentration of the reference element in the sample; Representing a constant; Representing a constant. To determine the concentration of the reference element of the sample by the X-ray peak signal intensity of the expression (2) and the reference element of the sample.
In some embodiments, the reference element may be selected according to the composition of the sample. In some embodiments, the reference element may be elemental calcium and elemental iron.
In some embodiments, in step S50, the sensitivity coefficient of the element beryllium corresponds to the following expression:
(3)。
wherein R LIBS (i/j) represents the sensitivity coefficient of the reference element and the element beryllium, A LIBS (j) represents the laser ray peak signal intensity of the element beryllium in the standard sample, A LIBS (i) represents the laser ray peak signal intensity of the reference element in the standard sample, C Representing the concentration of the reference element in the standard sample CIndicating the concentration of elemental beryllium in the standard sample. The concentration of the element beryllium in the sample is corrected through the sensitivity coefficient of the reference element and the element beryllium, so that the accuracy of the analysis and test result of the element beryllium in the sample is improved.
In some embodiments, in step S60, the concentration of elemental beryllium in the sample versus the sensitivity coefficient of the reference element to elemental beryllium corresponds to the following expression:
(4)。
Wherein, C LIBS (j) represents the concentration of the element beryllium in the sample, R LIBS (i/j) represents the sensitivity coefficient of the reference element and the element beryllium, A LIBS (j) represents the laser ray peak signal intensity of the element beryllium in the sample, and A LIBS (i) represents the laser ray peak signal intensity of the reference element in the sample; Indicating the concentration of the reference element in the sample. The concentration of the element beryllium in the sample can be determined by the expression (4) and the laser ray peak signal intensities of the element beryllium and the reference element in the sample, the concentration of the reference element and the sensitivity coefficients of the reference element and the element beryllium.
In some embodiments, in step S10, the method further comprises the steps of:
S11, preparing rock into powder.
The powder was formed into a round plate shape to obtain a sample S12.
To obtain a sample suitable for performing X-ray fluorescence spectroscopy and laser-induced breakdown spectroscopy.
In some embodiments, the rock sample is crushed into a powder having a particle size in the range of 20-70 μm, which may be 20 μm, for example.
In some embodiments, the powder may be pressed into a regular round tablet shape with a flat face by a tablet press.
In some embodiments, in step S30, the method further comprises the steps of:
s31, obtaining X-ray fluorescence spectrograms of a plurality of standard samples, and determining the X-ray peak signal intensity of reference elements in the plurality of standard samples.
S32, determining a curve of the relation between the X-ray peak signal intensity and the reference element according to the intensities of the plurality of standard samples and the concentrations of the reference element in the plurality of standard samples.
S33, determining an expression of the X-ray peak signal intensity and the concentration of the reference element according to the curve determined in the step S32.
And establishing a curve of the relation between the X-ray peak signal intensity and the reference element according to a plurality of standard samples with different reference element concentrations, reducing accidental errors of the test, and determining an accurate expression of the X-ray peak signal intensity and the reference element concentration, thereby ensuring the reliability of the expression of the X-ray peak signal intensity and the reference element concentration.
In some embodiments, the X-ray peak signal intensity versus reference element curve is a straight line. Wherein the intercept and slope of the relation curve of the X-ray peak signal intensity and the reference element are constants in the expression (1) and the expression (2), respectivelyAnd constant (constant)。
In some embodiments, the X-ray peak signal intensity may be an X-ray peak area or an X-ray peak height in an X-ray fluorescence spectrogram, as the case may be.
In some embodiments, the excitation voltage of the X-ray fluorescence spectroscopy is greater than or equal to 50kV, which may be, for example, 100kV, and the maximum current is 1mA, which may be, for example, 0.7mA.
In some embodiments, in step S50, the method further comprises the steps of:
And S51, determining the characteristic wavelength of the laser rays according to the reference element and the element beryllium.
S52, determining the laser ray peak signal intensity of the reference element and the element beryllium in the laser-induced breakdown spectrogram according to the characteristic wavelength of the laser rays.
The laser ray characteristic wavelengths of the reference element and the element beryllium are determined, so that the laser ray peaks of the reference element and the element beryllium and the corresponding signal intensities thereof can be rapidly and accurately determined in the laser-induced breakdown spectrogram of the standard sample.
Specifically, different elements have corresponding laser ray characteristic wavelengths, and by means of the corresponding laser ray characteristic wavelengths, a laser ray peak corresponding to the element can be determined in a laser induced breakdown spectrogram.
In some embodiments, the laser-ray characteristic wavelength of beryllium may be 313nm.
In some embodiments, in step S60, the method further comprises the steps of:
and S61, determining the characteristic wavelength of the laser rays according to the reference element and the element beryllium.
S62, determining the laser ray peak signal intensity of the reference element and the element beryllium in the laser-induced breakdown spectrogram according to the characteristic wavelength of the laser rays.
The laser ray characteristic wavelengths of the reference element and the element beryllium are determined, so that the laser ray peaks of the reference element and the element beryllium and the corresponding signal intensities thereof can be rapidly and accurately determined in a laser-induced breakdown spectrogram of the sample.
In some embodiments, the method is implemented with an analytical test system 1 that combines X-ray fluorescence spectroscopy and laser-induced breakdown spectroscopy, the analytical test system 1 further comprising a laser emitter 11, the method further comprising the step of adjusting the distance of the laser light emitted by the laser emitter 11 from the sample to focus the laser light on the surface of the sample. So as to realize the effective irradiation of the laser to the sample, thereby ensuring the accuracy of the experimental result.
In some embodiments, the laser transmitter 11 emits laser light having a wavelength less than 1064nm, which may be 532nm, for example.
In some embodiments, the laser energy emitted by the laser emitter 11 may be adjusted according to practical situations, and the laser energy range may be 20-300 mJ, for example, 100mJ.
The process of analytical testing of elemental beryllium in rock using the method of the present invention is further described in the following with specific examples.
Example 1
The rock sample was crushed to a powder with a particle size of about 70 μm and prepared by a tablet press into regular round tablets with a flat surface. A plurality of rock standard samples containing different concentrations of reference element calcium were prepared.
And adjusting the X-ray fluorescence spectrum device to an optimal working state, and performing X-ray fluorescence spectrum analysis on a plurality of rock standard samples containing elemental calcium to obtain a plurality of X-ray fluorescence spectrum diagrams. And obtaining a plurality of X-ray peak signal intensities of the elemental calcium according to the plurality of X-ray fluorescence spectrograms. Combining the X-ray peak signal intensity of the element calcium in the plurality of standard samples with the corresponding element calcium content, establishing a relation curve of the X-ray peak signal intensity of the element calcium in the standard samples with the element calcium content, and obtaining the slope and intercept of the relation curve. And according to the slope and intercept of the relation curve, obtaining an expression (1) of the X-ray peak signal intensity of the element calcium in the standard sample and the content of the corresponding element calcium.
And similarly, performing X-ray fluorescence spectrum analysis on the rock sample to obtain an X-ray fluorescence spectrum chart and the X-ray peak signal intensity of the elemental calcium. The X-ray peak signal intensity of elemental calcium of the rock sample is brought into expression (1), and expression (2) and the content of elemental calcium in the rock sample are obtained.
The laser transmitter 11 and the spectrometer 12 are adjusted to an ideal working state, a disc-shaped rock sample is placed on a coordinate platform, and the focus of the laser is adjusted to the surface of the rock sample.
Adjusting the distance between the optical lens and the rock sample, setting the integration time, the working wavelength and the triggering mode of the spectrometer 12, and setting the synchronous triggering signal to enable the spectrometer 12 and the laser transmitter 11 to be in the same-frequency working mode. 313nm is selected as the characteristic wavelength of the laser ray of the element beryllium, and 272nm is selected as the characteristic wavelength of the laser ray of the element calcium.
And carrying out laser-induced breakdown spectroscopy analysis on the rock sample to obtain a laser-induced breakdown spectrogram. The signal intensity of the 313nm laser ray peak in the laser induced breakdown spectrum is recorded as the signal intensity of the element beryllium laser ray peak in the rock sample, and the signal intensity of the 272nm laser ray peak is recorded as the signal intensity of the element calcium laser ray peak in the rock sample.
And similarly, performing laser-induced breakdown spectroscopy analysis on the rock standard sample to obtain the signal intensity of the laser ray peak of the element beryllium in the rock standard sample and the signal intensity of the laser ray peak of the element calcium in the rock standard sample.
And obtaining an expression (3) and sensitivity coefficients of the element calcium and the element beryllium according to the laser ray peak signal intensity of the element beryllium and the element calcium in the rock sample and the concentration of the element calcium and the beryllium element in the rock standard sample.
And obtaining an expression (4) and the concentration of the element beryllium in the rock sample according to the laser ray peak signal intensity of the element beryllium and the element calcium in the rock sample, the concentration of the element calcium in the rock sample and the sensitivity coefficient of the element calcium and the element beryllium.
Example 2
The rock sample was crushed into a powder having a particle size of about 20 μm and prepared into a regular round tablet shape with a flat surface by a tablet press. A plurality of rock standard samples containing different concentrations of reference elemental iron were prepared.
And adjusting the X-ray fluorescence spectrum device to an optimal working state, and performing X-ray fluorescence spectrum analysis on a plurality of rock standard samples containing elemental iron to obtain a plurality of X-ray fluorescence spectrum diagrams. And obtaining a plurality of X-ray peak signal intensities of the elemental iron according to the plurality of X-ray fluorescence spectrograms. Combining the X-ray peak signal intensity of the element iron in the plurality of standard samples with the corresponding content of the element iron, and establishing a relation curve of the X-ray peak signal intensity of the element iron in the standard samples with the content of the element iron to obtain the slope and intercept of the relation curve. And according to the slope and intercept of the relation curve, obtaining an expression (1) of the X-ray peak signal intensity of the element iron in the standard sample and the content of the corresponding element iron.
And similarly, performing X-ray fluorescence spectrum analysis on the rock sample to obtain an X-ray fluorescence spectrum chart and the X-ray peak signal intensity of the element iron. The X-ray peak signal intensity of elemental iron of the rock sample is brought into expression (1), and expression (2) and the content of elemental iron in the rock sample are obtained.
The laser transmitter 11 and the spectrometer 12 are adjusted to an ideal working state, a disc-shaped rock sample is placed on a coordinate platform, and the focus of the laser is adjusted to the surface of the rock sample.
Adjusting the distance between the optical lens and the rock sample, setting the integration time, the working wavelength and the triggering mode of the spectrometer 12, and setting the synchronous triggering signal to enable the spectrometer 12 and the laser transmitter 11 to be in the same-frequency working mode. 313nm is selected as the characteristic wavelength of the laser ray of the element beryllium, and 234.8nm is selected as the characteristic wavelength of the laser ray of the element iron.
And carrying out laser-induced breakdown spectroscopy analysis on the rock sample to obtain a laser-induced breakdown spectrogram. The signal intensity of the 313nm laser ray peak in the laser induced breakdown spectrum is recorded as the signal intensity of the laser ray peak of the element beryllium in the rock sample, and the signal intensity of the 234.8nm laser ray peak is recorded as the signal intensity of the laser ray peak of the element iron in the rock sample.
And similarly, performing laser-induced breakdown spectroscopy analysis on the rock standard sample to obtain the signal intensity of the laser ray peak of the element beryllium in the rock standard sample and the signal intensity of the laser ray peak of the element iron in the rock standard sample.
And obtaining an expression (3) and a sensitivity coefficient of the element iron and the element beryllium according to the laser ray peak signal intensity of the element beryllium and the element iron in the rock sample and the concentration of the element iron and the beryllium element in the rock standard sample.
And obtaining an expression (4) and the concentration of the element beryllium in the rock sample according to the laser ray peak signal intensity of the element beryllium and the element iron in the rock sample, the concentration of the element iron in the rock sample and the sensitivity coefficient of the element iron and the element beryllium.
It should also be noted that, in the embodiments of the present application, features of the embodiments of the present application and features of the embodiments of the present application may be combined with each other to obtain new embodiments without conflict.
The above description is only specific embodiments of the present application, but the scope of the present application is not limited thereto, and the scope of the present application shall be defined by the claims.
Claims (11)
1. An analytical test system adapted for analytical testing of a sample, comprising:
a laser induced breakdown spectroscopy module arranged to determine elemental composition of the sample and its content;
an X-ray fluorescence analysis module arranged to determine a chemical property of the sample;
An analytical test system body forming a sample test cavity, the sample disposed within the sample test cavity and the sample capable of changing position within the sample test cavity;
wherein the laser-induced breakdown spectroscopy analysis module and the X-ray fluorescence analysis module are respectively and fixedly connected with the analysis test system body,
The laser emitted by the laser-induced breakdown spectroscopy analysis module irradiates a sample in the sample testing cavity, collects emitted light of high-temperature plasma generated after the sample is irradiated, and transmits the emitted light to the laser-induced breakdown spectroscopy analysis module for detection so as to determine the elemental composition and the content of the sample;
And the X-ray fluorescence analysis module emits X-rays to irradiate the sample in the sample testing cavity, and detects fluorescent X-rays generated after the sample is irradiated so as to determine the chemical properties of the sample.
2. The analytical test system of claim 1 wherein the analytical test device comprises,
The analytical test system body includes a plurality of walls that form the sample test cavity,
The portion of the laser-induced breakdown spectroscopy module and the portion of the X-ray fluorescence spectroscopy module are each fixedly connected to a different one of the plurality of walls.
3. The analytical test system of claim 1, further comprising:
the optical path channel, the first fixing piece, the second fixing piece and the optical fiber;
The analytical test system body includes a plurality of walls forming the sample test cavity;
The light path channel is fixedly connected with one of the walls, and a structure for projecting light rays is arranged on one of the walls, so that the laser emitted by the laser-induced breakdown spectroscopy analysis module can irradiate the sample arranged in the sample testing cavity;
The first fixing piece is fixedly connected with one of the walls and is fixedly connected with a part of the X-ray fluorescence analysis module so that X-rays emitted by the X-ray fluorescence analysis module can irradiate into the sample arranged in the sample testing cavity;
a portion of the X-ray fluorescence analysis module is fixedly disposed on one of the plurality of walls opposite to one of the plurality of walls on which the first fixture is disposed;
The second mount is fixedly disposed on one of the plurality of walls and is configured to mount the optical fiber such that the optical fiber receives light reflected from the sample by the laser light and transmits it to the laser-induced breakdown spectroscopy module.
4. The analytical test system of claim 3 wherein the analytical test device comprises,
The system also comprises a support piece, wherein the support piece is arranged in parallel with the analysis and test system body;
the laser-induced breakdown spectroscopy analysis module comprises a laser emitter, a spectrometer and a light guide piece,
The laser transmitter is arranged on the supporting piece, the light guide piece is arranged in the light path channel, the spectrometer is arranged outside the analysis and test system body,
The laser emitted by the laser emitter irradiates the light guide piece, irradiates the sample after being conducted by the light guide piece, reflects the sample to the optical fiber, is conducted to the spectrometer by the optical fiber, and is detected by the spectrometer.
5. The analytical test system of claim 3 wherein the analytical test device comprises,
The X-ray fluorescence analysis module includes an X-ray source disposed on one of the plurality of walls via the first fixture, and an X-ray energy detector fixedly disposed on one of the plurality of walls opposite the one of the plurality of walls disposed by the first fixture,
X-rays emitted from the X-ray source irradiate the sample, and X-rays reflected from the sample are detected by the X-ray energy detector.
6. The analytical test system of claim 5 wherein the analytical test device comprises,
The X-ray source and the X-ray energy detector are disposed with their central extension lines at a predetermined angle and are focused on the surface of the sample.
7. The analytical test system of claim 1 wherein the analytical test device comprises,
Also comprises an objective table, the sample is arranged on the objective table,
The stage is arranged in sealing connection with the sample testing cavity and is capable of adjusting position along a transverse direction, a longitudinal direction and three directions perpendicular to the transverse direction and the longitudinal direction.
8. The analytical test system of claim 7 wherein the analytical test device comprises,
The device also comprises a corrugated pipe, wherein two ends of the corrugated pipe are respectively connected with the objective table and the sample testing cavity in a sealing way, so that the interior of the sample testing cavity is kept in a vacuum state when the objective table adjusts the position of the sample.
9. The analytical test system of claim 1 wherein the analytical test device comprises,
The system further comprises a vacuum module which is fixedly connected with the analysis and test system body and is used for maintaining the vacuum degree of the sample test cavity when the laser-induced breakdown spectroscopy analysis module is used for testing.
10. The analytical test system of claim 1 wherein the analytical test device comprises,
The system further comprises a purging module, wherein the purging module is fixedly connected with the analysis and test system body and is used for purging the surface of the sample when the laser-induced breakdown spectroscopy analysis module is used for testing.
11. An analytical test method, characterized in that it is suitable for analytical testing of a sample, which utilizes the analytical test system according to any one of claims 1-10, comprising the steps of:
Obtaining a laser-induced breakdown spectroscopy spectrogram of the sample by using the laser-induced breakdown spectroscopy analysis module;
obtaining an X-ray fluorescence method spectrogram of the sample by utilizing the X-ray fluorescence analysis module;
And determining the property of the sample according to the laser-induced breakdown method spectrogram and the X-ray fluorescence method spectrogram.
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