Method for analyzing and testing the element beryllium in rocks

Abstract

The embodiment of the present application relates to the technical field of chemical property analysis and testing materials for determining materials, and specifically to a method for analyzing and testing beryllium in rocks, comprising the steps of: S30: obtaining an X-ray fluorescence spectrum of a standard sample, and determining the relationship between the concentration of a reference element and its X-ray peak signal intensity; S40: obtaining an X-ray fluorescence spectrum of a sample, and determining the concentration of the reference element in the sample; S50: obtaining a laser induced breakdown spectrum of a standard sample, and determining the sensitivity coefficient of the reference element and beryllium; S60: obtaining a laser induced breakdown spectrum of a sample, and determining the concentration of beryllium in the sample according to the laser induced breakdown spectrum, the sensitivity coefficient of the reference element and beryllium determined in step S50, and the concentration of the reference element in the sample. The embodiment of the present application improves the accuracy of the analysis and testing structure by determining the sensitivity coefficient of the reference element and beryllium, and using the coefficient to correct the concentration of beryllium in the sample.

Description

Technical Field

[0001] The present application relates to the technical field of chemical property analysis and testing materials for determining materials, and in particular to a method for analyzing and testing the element beryllium in rocks. Background Art

[0002] The content in this section only provides background information related to this application and does not necessarily constitute prior art.

[0003] Beryllium is a metal element with a low atomic number. It is light in weight and has excellent corrosion resistance and mechanical properties. It is commonly used in technical fields such as the atomic energy industry, metallurgical industry, aerospace, etc.

[0004] Currently, the primary method for analyzing and measuring beryllium concentrations in rocks is inductively coupled plasma optical emission spectrometry (ICP-OES). This method utilizes wet chemical digestion of rocks, resulting in highly accurate analytical results. However, ICP-OES requires chemical pretreatment of both the sample and the standard, leading to complex analytical procedures and low efficiency. Summary of the Invention

[0005] A brief overview of the present application is provided below to provide a basic understanding of certain aspects of the present application. It should be understood that this overview is not an exhaustive overview of the present application. It is not intended to identify key or important portions of the present application, nor is it intended to limit the scope of the present application. Its purpose is simply to present certain concepts in a simplified form as a prelude to the more detailed description that will be discussed later.

[0006] An embodiment of the present application provides a method for analyzing and testing the element beryllium in rocks, comprising:

[0007] S10: Prepare a rock sample, the sample including the element beryllium and a reference element.

[0008] S20: preparing a standard sample of rock with known composition, wherein the standard sample includes a reference element and element beryllium, and the concentrations of the reference element and element beryllium in the standard sample are known.

[0009] S30: Obtain an X-ray fluorescence spectrum of the standard sample, and determine the relationship between the concentration of the reference element and the X-ray peak signal intensity thereof according to the X-ray fluorescence spectrum.

[0010] S40: Obtain an X-ray fluorescence spectrum of the sample, and determine the concentration of the reference element in the sample based on the relationship determined in step S30.

[0011] S50: Obtain a laser induced breakdown spectrum of the standard sample, and determine 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.

[0012] S60: Obtain a laser induced breakdown spectrum of the sample, and determine the concentration of the element beryllium in the sample based on the laser induced breakdown spectrum, the sensitivity coefficient of the reference element and the element beryllium determined in step S50, and the concentration of the reference element in the sample.

[0013] The embodiments of the present application perform X-ray fluorescence and laser-induced breakdown analysis on samples and standard samples, eliminating the need for chemical pretreatment of the samples and standard samples, simplifying the analysis and testing process and improving the efficiency of analyzing beryllium concentrations in rocks. Furthermore, based on the analysis results of the two analysis methods, the sensitivity coefficients of the reference element and the element beryllium are determined, and the sensitivity coefficients of the reference element and the element beryllium are used to calibrate the beryllium concentration in the sample, thereby improving the accuracy of the analysis results. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] To further illustrate the above and other advantages and features of the present application, the following detailed description of specific embodiments of the present application is provided in conjunction with the accompanying drawings. The accompanying drawings, together with the detailed description below, are incorporated into and form a part of this specification. Elements with the same function and structure are denoted by the same reference numerals. It should be understood that these drawings depict only typical examples of the present application and should not be construed as limiting the scope of the present application.

[0015] Figure 1 This is a flow chart of analyzing and testing the element beryllium in rocks according to one embodiment of the present application;

[0016] Figure 2 is a schematic diagram of an analysis and testing system according to one embodiment of the present application;

[0017] Figure 3 is a side view of an analytical testing system according to one embodiment of the present application;

[0018] Figure 4 is a partial cross-sectional view of an analysis and testing system according to one embodiment of the present application;

[0019] Figure 5 It is a partially enlarged schematic diagram of an analysis and testing system according to an embodiment of the present application.

[0020] It should be noted that the drawings are not necessarily drawn to scale, but are merely shown in a schematic manner that does not affect the reader's understanding.

[0021] Description of reference numerals:

[0022] 1. Analysis and testing system;

[0023] 10. Laser-induced breakdown spectroscopy analysis module; 11. Laser emitter; 12. Spectrometer; 13. Light guide; 14. First light concentrating element;

[0024] 20. X-ray fluorescence analysis module; 21. X-ray source; 22. X-ray energy detector;

[0025] 30. Analysis and testing system body; 31. Sample testing cavity; 32. Light projection structure;

[0026] 40. Optical channel; 41. Horizontal channel;

[0027] 50. First fixing member;

[0028] 60. Second fixing member;

[0029] 70. Optical fiber;

[0030] 80. Support member; 81. Support column; 82. Support body;

[0031] 90. Loading platform; 91. Support portion; 92. Rod portion;

[0032] 100, coordinate platform; 101, first platform; 102, second platform; 1021, coordinate adjustment assembly; 10211, transverse coordinate adjustment member; 10212, longitudinal coordinate adjustment member; 10213, normal coordinate adjustment member; 102131, extension portion; 102132, adjustment portion; 103, raised portion; 104, platform connector;

[0033] 110. Bellows;

[0034] 120. Vacuum module;

[0035] 130. Purge module;

[0036] 140. Measurement and control system. DETAILED DESCRIPTION

[0037] Exemplary embodiments of the present application will be described below with reference to the accompanying drawings. For the sake of clarity and conciseness, not all features of actual implementations are described in the specification. However, it should be understood that many implementation-specific decisions must be made in the process of developing any such actual implementation in order to achieve the developer's specific goals, such as meeting those constraints related to the system and business, and these constraints may vary depending on the implementation. In addition, it should be understood that although the development work may be very complex and time-consuming, it is a routine task for those skilled in the art who benefit from the content of this application.

[0038] It is also necessary to explain here that, in order to avoid obscuring the present application due to unnecessary details, the accompanying drawings only show the device structure and / or processing steps that are closely related to the solution according to the present application, while other details that are not closely related to the present application are omitted.

[0039] It should be noted that, unless otherwise defined, the technical or scientific terms used in this application should have the common meanings understood by persons having ordinary skills in the field to which this application belongs.

[0040] In the description of the embodiments of the present application, “multiple” means at least two, such as two, three, etc., unless otherwise clearly and specifically defined.

[0041] The inventors of the present invention have discovered that laser-induced breakdown spectroscopy (LIBS) offers rapid analysis speed and requires no sample pretreatment. However, its drawback is poor spectral stability, resulting in poor repeatability of test results. X-ray fluorescence (XRF) also offers rapid analysis speed but is unsuitable for analyzing low-mass elements (e.g., lithium and beryllium).

[0042] Based on this, an embodiment of the present application provides a method for analyzing and testing the element beryllium in rocks. Figure 1 This is a flow chart of analyzing and testing the element beryllium in rocks according to one embodiment of the present application. Figure 1 As shown, it includes:

[0043] S10: Prepare a rock sample, the sample including the element beryllium and a reference element.

[0044] S20: preparing a standard sample of rock with known composition, wherein the standard sample includes a reference element and element beryllium, and the concentrations of the reference element and element beryllium in the standard sample are known.

[0045] S30: Obtain an X-ray fluorescence spectrum of the standard sample, and determine the relationship between the concentration of the reference element and the X-ray peak signal intensity thereof according to the X-ray fluorescence spectrum.

[0046] S40: Obtain an X-ray fluorescence spectrum of the sample, and determine the concentration of the reference element in the sample based on the relationship determined in step S30.

[0047] S50: Obtain a laser induced breakdown spectrum of the standard sample, and determine 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.

[0048] S60: Obtain a laser induced breakdown spectrum of the sample, and determine the concentration of the element beryllium in the sample based on the laser induced breakdown spectrum, the sensitivity coefficient of the reference element and the element beryllium determined in step S50, and the concentration of the reference element in the sample.

[0049] The embodiments of the present application perform X-ray fluorescence and laser-induced breakdown analysis on samples and standard samples, eliminating the need for chemical pretreatment of the samples and standard samples, simplifying the analysis and testing process and improving the efficiency of analyzing beryllium concentrations in rocks. Furthermore, the sensitivity coefficients of the reference element and the element beryllium are determined based on the analysis results of the two analysis methods, and the concentration of the element beryllium in the sample is corrected using the sensitivity coefficients of the reference element and the element beryllium. This overcomes the problem in the prior art that X-ray fluorescence methods are not suitable for analyzing low-mass elements in sample analysis, thereby improving the accuracy of the analysis results.

[0050] In some embodiments, in step S30, the relationship between the concentration of the reference element in the standard sample and the intensity of its X-ray peak signal conforms to the following expression:

[0051] (1).

[0052] Where, Indicates the X-ray peak signal intensity of the reference element in the standard sample; Indicates the concentration of the reference element in the standard sample; represents a constant; Represents a constant. It is used to determine the relationship between the X-ray peak signal intensity of the reference element in the standard sample and the concentration of the reference element in the standard sample.

[0053] In some embodiments, in step S40, the relationship between the concentration of the reference element in the sample and the intensity of its X-ray peak signal conforms to the following expression:

[0054] (2).

[0055] Where, Indicates the X-ray peak signal intensity of the reference element in the sample; Indicates the concentration of the reference element in the sample; represents a constant; Denotes a constant. The concentration of the reference element in the sample is determined by using expression (2) and the X-ray peak signal intensity of the reference element in the sample.

[0056] In some embodiments, the reference element can be selected based on the composition of the sample. In some embodiments, the reference element can be calcium and iron.

[0057] In some embodiments, in step S50, the sensitivity coefficient of the element beryllium satisfies the following expression:

[0058] (3).

[0059] Where R LIBS (i / j) represents the sensitivity coefficient of the reference element and the element beryllium; A LIBS (j) represents the peak signal intensity of the laser beam of element beryllium in the standard sample; A LIBS (i) represents the laser beam peak signal intensity of the reference element in the standard sample; C Indicates the concentration of the reference element in the standard sample; C Indicates the concentration of elemental beryllium in a standard sample. By using the sensitivity coefficient between the reference element and elemental beryllium, the concentration of elemental beryllium in the sample is corrected to improve the accuracy of the analysis and test results of elemental beryllium in the sample.

[0060] In some embodiments, in step S60, the relationship between the concentration of element beryllium in the sample and the sensitivity coefficient of the reference element to element beryllium conforms to the following expression:

[0061] (4).

[0062] Where C LIBS (j) represents the concentration of 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 peak signal intensity of the laser beam of element beryllium in the sample; A LIBS (i) represents the peak signal intensity of the laser beam of the reference element in the sample; represents the concentration of the reference element in the sample. Thus, the concentration of the element beryllium in the sample can be determined by using expression (4) and the laser beam peak signal intensity of the element beryllium in the sample and the reference element, the concentration of the reference element, and the sensitivity coefficients of the reference element and the element beryllium.

[0063] In some embodiments, step S10 further includes the following steps:

[0064] S11: Reduce the rock to powder.

[0065] S12: The powder is formed into a disc shape to obtain a sample.

[0066] To obtain samples suitable for X-ray fluorescence spectrometry analysis and laser induced breakdown spectroscopy analysis.

[0067] In some embodiments, the rock sample is crushed into powder with a particle size ranging from 20 to 70 μm, for example, 20 μm.

[0068] In some embodiments, the powder can be compressed into regular round tablets with flat surfaces using a tablet press.

[0069] In some embodiments, step S30 further includes the following steps:

[0070] S31: Obtain X-ray fluorescence spectra of multiple standard samples, and determine the X-ray peak signal intensity of the reference elements in the multiple standard samples.

[0071] S32: Determine a curve showing a relationship between X-ray peak signal intensity and reference elements according to the intensities of the plurality of standard samples and the concentrations of the reference elements in the plurality of standard samples.

[0072] S33: According to the curve determined in step S32, an expression of the X-ray peak signal intensity and the concentration of the reference element is determined.

[0073] A curve showing the relationship between X-ray peak signal intensity and reference element is established based on multiple standard samples with different reference element concentrations, thereby reducing accidental experimental errors and determining an accurate expression of X-ray peak signal intensity and reference element concentration, thereby ensuring the reliability of the expression of X-ray peak signal intensity and reference element concentration.

[0074] In some embodiments, a curve of the relationship between the X-ray peak signal intensity and the reference element can be determined by fitting. For example, the curve of the relationship between the X-ray peak signal intensity and the reference element is a straight line. Based on the curve of the above relationship, an expression between the two can be determined. According to the determined expression, the constants in Expression (1) and Expression (2) can be determined. With constant .

[0075] In some embodiments, the X-ray peak signal intensity may be the X-ray peak area or the X-ray peak height in the X-ray fluorescence spectrum according to actual conditions.

[0076] In some embodiments, the excitation voltage of the X-ray fluorescence spectroscopy is greater than or equal to 50 kV, for example, 100 kV, and the maximum current is 1 mA, for example, 0.7 mA.

[0077] In some embodiments, step S50 further includes the following steps:

[0078] S51: Determine the characteristic wavelength of the laser beam based on the reference element and the element beryllium.

[0079] S52: Determine the laser beam peak signal intensities of the reference element and the element beryllium in the laser induced breakdown spectrum according to the characteristic wavelength of the laser beam.

[0080] By determining the characteristic wavelengths of the laser beams of the reference element and the element beryllium, the laser beam peaks of the reference element and the element beryllium and their corresponding signal intensities can be quickly and accurately determined in the laser induced breakdown spectrum of the standard sample.

[0081] Specifically, different elements have corresponding laser ray characteristic wavelengths. Through the corresponding laser ray characteristic wavelengths, the laser ray peak corresponding to the element can be determined in the laser induced breakdown spectrum.

[0082] In some embodiments, the characteristic wavelength of beryllium laser radiation may be 313 nm.

[0083] In some embodiments, step S60 further includes the following steps:

[0084] S61: Determine the characteristic wavelength of the laser beam based on the reference element and the element beryllium.

[0085] S62: Determine the laser beam peak signal intensities of the reference element and the element beryllium in the laser induced breakdown spectrum according to the characteristic wavelength of the laser beam.

[0086] By determining the characteristic wavelengths of the laser beams of the reference element and the element beryllium, the laser beam peaks of the reference element and the element beryllium and their corresponding signal intensities can be quickly and accurately determined in the laser induced breakdown spectrum of the sample.

[0087] In some embodiments, the method is implemented using an analytical testing system that combines X-ray fluorescence spectroscopy and laser-induced breakdown spectroscopy. The analytical testing system also includes a laser emitter. The method further includes the following steps: adjusting the distance between the laser emitted by the laser emitter and the sample so that the laser is focused on the sample surface. This ensures effective laser irradiation of the sample, thereby ensuring the accuracy of the experimental results.

[0088] In some embodiments, the laser wavelength emitted by the laser emitter is less than 1064 nm, for example, may be 532 nm.

[0089] In some embodiments, the laser energy emitted by the laser emitter can be adjusted according to actual conditions, and the laser energy range is 20-300 mJ, for example, it can be 100 mJ.

[0090] The following is a specific example to further illustrate the process of analyzing and testing the element beryllium in rocks using the method of the present invention.

[0091] Example 1

[0092] The rock sample was crushed into a powder with a particle size of approximately 70 μm and then pressed into a flat, regular, round tablet. A rock standard sample containing the reference element calcium was prepared.

[0093] The X-ray fluorescence spectrometer is adjusted to the optimal working state, and X-ray fluorescence spectrometry analysis is performed on multiple rock standard samples containing elemental calcium to obtain multiple X-ray fluorescence spectra. Based on the multiple X-ray fluorescence spectra, multiple X-ray peak signal intensities of elemental calcium are obtained. Combining the X-ray peak signal intensities of elemental calcium in multiple standard samples with the corresponding elemental calcium concentrations, a relationship curve between the X-ray peak signal intensity of elemental calcium in the standard samples and the elemental calcium concentration is established, and the slope and intercept of the relationship curve are obtained. Based on the slope and intercept of the relationship curve, an expression (1) is obtained for the X-ray peak signal intensity of elemental calcium in the standard samples and the corresponding elemental calcium concentration.

[0094] Similarly, X-ray fluorescence spectrometry is performed on the rock sample to obtain the X-ray fluorescence spectrum and the X-ray peak signal intensity of elemental calcium. Substituting the X-ray peak signal intensity of elemental calcium of the rock sample into expression (1), expression (2) and the concentration of elemental calcium in the rock sample are obtained.

[0095] Adjust the laser emitter and spectrometer to the ideal working state, place the disc-shaped rock sample on the coordinate platform, and adjust the focus of the laser to the surface of the rock sample.

[0096] Adjust the distance between the optical lens and the rock sample, set the spectrometer operating parameters, such as integration time, operating wavelength, and trigger mode, and set the synchronization trigger signal so that the spectrometer and laser transmitter are in the same frequency mode. Select 313nm as the characteristic wavelength of the laser beam for the element beryllium, and select 272nm as the characteristic wavelength of the laser beam for the element calcium.

[0097] Laser-induced breakdown spectroscopy (LIBS) analysis was performed on the rock sample to obtain a LBS graph. The signal intensity of the 313 nm laser beam peak in the LBS graph was recorded as the signal intensity of the laser beam peak for the element beryllium in the rock sample, and the signal intensity of the 272 nm laser beam peak was recorded as the signal intensity of the laser beam peak for the element calcium in the rock sample.

[0098] Similarly, laser induced breakdown spectroscopy analysis is performed on the rock standard sample to obtain the signal intensity of the laser beam peak of the element beryllium in the rock standard sample and the signal intensity of the laser beam peak of the element calcium in the rock standard sample.

[0099] According to the laser beam peak signal intensity of elemental beryllium and elemental calcium in the rock sample and the concentration of elemental calcium and elemental beryllium in the rock standard sample, expression (3) and the sensitivity coefficients of elemental calcium and elemental beryllium are obtained.

[0100] According to the laser beam peak signal intensity of elemental beryllium and elemental calcium in the rock sample, the concentration of elemental calcium in the rock sample and the sensitivity coefficients of elemental calcium and elemental beryllium, expression (4) and the concentration of elemental beryllium in the rock sample are obtained.

[0101] Example 2

[0102] The rock sample was crushed into a powder with a particle size of approximately 20 μm and then pressed into a flat, regular, round tablet. A number of rock standard samples containing different concentrations of the reference element iron were prepared.

[0103] The X-ray fluorescence spectrometer is adjusted to the optimal working state, and X-ray fluorescence spectrometry is performed on multiple standard rock samples containing elemental iron to obtain multiple X-ray fluorescence spectra. Based on the multiple X-ray fluorescence spectra, multiple X-ray peak signal intensities of elemental iron are obtained. Combining the X-ray peak signal intensities of elemental iron in multiple standard samples with the corresponding elemental iron contents, a relationship curve between the X-ray peak signal intensities of elemental iron in the standard samples and the elemental iron contents is established. The relationship expression is determined through the relationship curve, and the expression (1) between the X-ray peak signal intensities of elemental iron in the standard samples and the corresponding elemental iron contents is obtained.

[0104] Similarly, X-ray fluorescence spectrometry is performed on the rock sample to obtain the X-ray fluorescence spectrum and the X-ray peak signal intensity of elemental iron. Substituting the X-ray peak signal intensity of elemental iron of the rock sample into expression (1), expression (2) and the content of elemental iron in the rock sample are obtained.

[0105] Adjust the laser emitter and spectrometer to the ideal working state, place the disc-shaped rock sample on the coordinate platform, and adjust the focus of the laser to the surface of the rock sample.

[0106] Adjust the distance between the optical lens and the rock sample, set the spectrometer's integration time, operating wavelength, and trigger mode, and set a synchronous trigger signal so that the spectrometer and laser emitter operate at the same frequency. Select 313 nm as the characteristic wavelength of the laser beam for beryllium and 234.8 nm for iron.

[0107] Laser-induced breakdown spectroscopy (LIBS) analysis was performed on the rock sample to obtain a LBS graph. The signal intensity of the 313 nm laser beam peak in the LBS graph was recorded as the signal intensity of the laser beam peak for the element beryllium in the rock sample, and the signal intensity of the 234.8 nm laser beam peak was recorded as the signal intensity of the laser beam peak for the element iron in the rock sample.

[0108] Similarly, laser induced breakdown spectroscopy analysis is performed on the rock standard sample to obtain the signal intensity of the laser beam peak of the element beryllium in the rock standard sample and the signal intensity of the laser beam peak of the element iron in the rock standard sample.

[0109] According to the laser beam peak signal intensity of elemental beryllium and elemental iron in the rock sample and the concentration of elemental iron and elemental beryllium in the rock standard sample, expression (3) and the sensitivity coefficients of elemental iron and elemental beryllium are obtained.

[0110] According to the laser beam peak signal intensity of elemental beryllium and elemental iron in the rock sample, the concentration of elemental iron in the rock sample and the sensitivity coefficients of elemental iron and elemental beryllium, expression (4) and the concentration of elemental beryllium in the rock sample are obtained.

[0111] In order to implement the method of analyzing and testing the element beryllium in rocks in this application, the embodiment of this application also provides an analysis and testing system suitable for analyzing and testing samples. Figure 2 is a schematic diagram of an analysis and testing system according to an embodiment of the present application. Figure 3 FIG. 1 is a side view of an analysis and testing system according to an embodiment of the present application. Figure 2 and Figure 3 As shown, the analysis and testing system 1 includes: a laser induced breakdown spectroscopy analysis module 10, which is configured to determine the elemental composition and content of the sample; an X-ray fluorescence analysis module 20, which is configured to determine the chemical properties of the sample; an analysis and testing system body 30, wherein the analysis and testing system body 30 forms a sample test cavity 31, the sample is set in the sample test cavity 31, and the sample can change its position in the sample test cavity 31; wherein, the laser induced breakdown spectroscopy analysis module 10 and the X-ray fluorescence analysis module 20 are configured to be fixedly connected to the analysis and testing system body 30 respectively, the laser induced breakdown spectroscopy analysis module 10 emits a laser to irradiate the sample in the sample test cavity 31, and collects the emission light of the high-temperature plasma generated by the sample after irradiation, and transmits the emission light to the laser induced breakdown spectroscopy analysis module 10 for detection to determine the elemental composition and content of the sample; the X-ray fluorescence analysis module 20 emits X-rays to irradiate the sample in the sample test cavity 31, and detects the fluorescent X-rays generated by the sample after irradiation to determine the chemical properties of the sample.

[0112] The embodiments of the present application arrange the laser induced breakdown spectroscopy analysis module and the X-ray fluorescence analysis module to be fixedly connected to the analysis and testing system body respectively, so that laser induced breakdown spectroscopy analysis and X-ray fluorescence analysis can be performed on the same sample in the same cavity on a single device, and the position of the sample can be adjusted inside it during the test process. Therefore, when using the laser induced breakdown spectroscopy analysis module and the X-ray fluorescence analysis module respectively, there is no need to reinsert the sample, thereby avoiding the impact of different test environments on the analysis results of the sample, and simplifying the analysis and testing process, thereby improving the accuracy of the analysis results and the efficiency of the analysis and testing.

[0113] Figure 4FIG is a partial cross-sectional view of an analysis and testing system 1 according to an embodiment of the present application. Figure 2 and Figure 4 As shown, in some embodiments, the analysis and testing system body 30 includes multiple walls, which form a sample testing cavity 31. Part of the laser induced breakdown spectroscopy analysis module 10 and part of the X-ray fluorescence analysis module 20 are respectively fixedly connected to different ones of the multiple walls, thereby avoiding contact between the laser induced breakdown spectroscopy analysis module 10 and the X-ray fluorescence analysis module 20 during the analysis and testing process, which would interfere with the laser induced breakdown spectroscopy analysis and X-ray fluorescence analysis of the sample.

[0114] like Figure 4 As shown, in some embodiments, the analysis and testing system 1 further includes: an optical channel 40, a first fixture 50, a second fixture 60, and an optical fiber 70. The analysis and testing system body 30 includes multiple walls, which form a sample testing chamber 31. The optical channel 40 is fixedly connected to one of the multiple walls and has a light projection structure 32 disposed on the wall, so that laser light emitted from the laser-induced breakdown spectrometry analysis module 10 can illuminate the sample disposed in the sample testing chamber 31. The first fixture 50 is fixedly connected to one of the multiple walls and is also fixedly connected to a portion of the X-ray fluorescence analysis module 20, so that X-rays emitted by the X-ray fluorescence analysis module 20 can enter the sample disposed in the sample testing chamber 31. A portion of the X-ray fluorescence analysis module 20 is fixedly attached to one of the multiple walls opposite the one of the multiple walls to which the first fixture 50 is disposed. The second fixture 60 is fixedly attached to one of the multiple walls and is configured to secure the optical fiber 70, so that the optical fiber 70 receives light reflected by the laser light from the sample and transmits it to the laser-induced breakdown spectrometry analysis module 10. By respectively arranging the optical path channel 40, the first fixing member 50 and the second fixing member 60 on one of the multiple walls of the analysis and testing system body 30, the cross-interference of the optical paths of the laser, X-rays and the light reflected by the laser is avoided, thereby ensuring the irradiation of the laser and X-ray light on the sample in the sample testing cavity 31 and the transmission of the laser reflected light.

[0115] In some embodiments, the light-projecting structure 32 may be a quartz window for introducing laser light into the cavity from the atmospheric side.

[0116] In some embodiments, the second fixture 60 is in communication with the sample testing cavity 31 and is used to fix the optical fiber 70 so that the optical fiber 70 passes through the second fixture 60 and enters the sample testing cavity 31. In some embodiments, the second fixture 60 can be a through flange.

[0117] In some embodiments, the optical fiber 70 may be a silica optical fiber.

[0118] like Figure 2 and Figure 4 As shown, in some embodiments, the analysis and testing system 1 further includes a support member 80, which is arranged in parallel with the analysis and testing system body 30. The laser induced breakdown spectroscopy analysis module 10 includes a laser emitter 11, a spectrometer 12, and a light guide 13. The laser emitter 11 is disposed on the support member 80, the light guide 13 is disposed within the optical path 40, and the spectrometer 12 is disposed outside the analysis and testing system body 30. The laser emitted by the laser emitter 11 irradiates the light guide 13, is transmitted through the light guide 13, and then irradiates the sample. The laser is reflected by the sample to the optical fiber 70, and is then transmitted by the optical fiber 70 to the spectrometer 12 for detection by the spectrometer 12. Specifically, by setting a support member 80 parallel to the analysis and testing system body 30, the laser emitted by the laser emitter 11 set on the support member 80 can be injected into the optical path channel 40 of the analysis and testing system body 30, and the laser path is changed by the light guide 13 set in the optical path channel 40 so that the laser is irradiated to the sample. The composition of the emitted light generated by the sample after laser irradiation is detected by the spectrometer 12, and the elemental composition and content of the sample are obtained, thereby completing the laser induced breakdown spectroscopy analysis of the sample.

[0119] In some embodiments, the support member 80 includes multiple support columns 81 and a support body 82. The multiple support columns 81 are used to support the support body 82. The support body 82 has multiple walls, and the laser emitter 11 is disposed on the wall of the support body 82 opposite the analysis and testing system body 30. In some embodiments, a horizontal channel 41 is formed on the wall opposite the optical path 40 and the support body 82, communicating with the optical path 40. The horizontal channel 41 is arranged in parallel with the laser emitter 11, with the laser outlet of the laser emitter 11 aligned with the center of the horizontal channel 41. This allows the laser light emitted by the laser emitter 11 to enter the optical path 40 through the horizontal channel 41.

[0120] In some embodiments, the output wavelength of the laser emitter 11 can be 1064 nm, 532 nm or other shorter wavelength lasers (such as 256 nm), and the laser power selection range can be 20~300 mJ, which is used to provide a high-energy monochromatic excitation light source.

[0121] In some embodiments, the light guide 13 is disposed upstream of the structure 32 for projecting light, and the center of the light guide 13 is aligned with the laser outlet of the laser emitter 11 and the center of the horizontal channel 41. Specifically, the laser light passes through the horizontal channel 41 and is irradiated to the light guide 13. The light guide 13 then changes the path of the laser light emitted by the laser emitter 11 so that the laser light is irradiated to the sample.

[0122] In some embodiments, the light guide 13 may be a 45-degree reflector, which is tilted at a 45-degree angle in the optical path 40 to reflect the horizontal laser emitted by the laser emitter 11 into a vertical laser, so that the laser can irradiate the sample.

[0123] In some embodiments, the laser-induced breakdown spectroscopy analysis module 10 further includes a first light focusing element 14, disposed between the light guide 13 and the light projection structure 32. This first light focusing element 14 focuses the laser light on the sample surface within the cavity after passing through the light projection structure 32. This prevents unnecessary loss of laser energy, thereby ensuring effective laser irradiation of the sample. Specifically, the first light focusing element 14 may be a convex lens.

[0124] In some embodiments, the laser-induced breakdown spectroscopy analysis module 10 further includes a second light-collecting element for collecting the emission light generated by the laser irradiation on the sample surface and transmitting the emission light to the optical fiber 70 .

[0125] In some embodiments, the wavelength monitoring range of the spectrometer 12 may be selected according to the composition of the sample to avoid interference from other wavelength ranges and improve the analysis efficiency of the spectrometer 12 .

[0126] like Figure 2 As shown, 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 is mounted on one of the multiple walls via a first fixing member 50, and the X-ray energy detector 22 is fixedly mounted on one of the multiple walls opposite to the one of the multiple walls where the first fixing member 50 is mounted. X-rays emitted by the X-ray source 21 irradiate a sample, and X-rays reflected from the sample are detected by the X-ray energy detector 22. By separately mounting the X-ray source 21 and the X-ray energy detector 22 on one of the multiple walls, contact between the X-ray source 21 and the X-ray energy detector 22 during the analysis and testing process is avoided, thereby preventing interference with the normal operation of the X-ray source 21 and the X-ray energy detector 22. Furthermore, the two separately mounted walls are positioned opposite each other, ensuring that X-rays reflected from the sample after irradiation by the X-rays can be detected by the X-ray energy detector 22.

[0127] In some embodiments, the first fixing member 50 may be a flange interface for achieving a fastened connection between the X-ray source 21 and one of the walls of the analysis and testing system body 30 .

[0128] In some embodiments, the excitation voltage of the X-ray source 21 may range from 20 kV to 50 kV, for example, 30 kV.

[0129] In some embodiments, the X-ray energy detector 22 is used to detect the composition of X-rays reflected by the sample to obtain the chemical properties of the sample.

[0130] In some embodiments, the material of the X-ray source 21 detector can be selected according to the test requirements, for example, it can be rhodium, silver, tungsten, etc.

[0131] like Figure 4 As shown, in some embodiments, the X-ray source 21 and the X-ray energy detector 22 are arranged so that their center extensions form a predetermined angle and converge on the surface of the sample. This is used to limit the optical path of the X-rays irradiating the sample and the X-rays reflected by the sample, preventing interference with the accuracy of the X-ray fluorescence spectrum analysis of the sample due to the optical paths of the X-rays and the reflected X-rays being too close or too far.

[0132] In some embodiments, a certain angle is formed between the X-ray source 21 and the X-ray energy detector 22, and the angle range is 30° to 90°, for example, 45°.

[0133] Figure 5 FIG. 1 is a partially enlarged schematic diagram of an analysis and testing system 1 according to an embodiment of the present application. Figure 4 and Figure 5 As shown, in some embodiments, the analysis and testing system 1 further includes a stage 90, on which the sample is placed. The stage 90 is configured to be sealed with the chamber and capable of adjustment in three directions: horizontally, vertically, and perpendicular to the horizontal and vertical directions. The stage 90 can be used to move the sample to the corresponding testing position when switching between laser induced spectroscopy analysis and X-ray fluorescence spectroscopy analysis.

[0134] like Figure 4 and Figure 5 As shown, in some embodiments, the stage 90 is formed with a support portion 91 and a rod portion 92, wherein the support portion 91 is disposed directly above the rod portion 92, and the rod portion 92 is used to support the support portion 91. The support portion 91 and a portion of the rod portion 92 are disposed in the sample testing cavity 31, and the sample is disposed on the support portion 91.

[0135] like Figure 4 As shown, in some embodiments, the analysis and testing system 1 further includes a coordinate platform 100 and a coordinate adjustment assembly 1021. The coordinate platform 100 includes a first platform 101 and a second platform 102. The first platform 101 is disposed above the second platform 102. The first platform 101 and the second platform 102 are fixed in horizontal relative position, and the height of the spacing between the first platform 101 and the second platform 102 is adjustable. The coordinate adjustment assembly 1021 is disposed on the second platform 102 and is used to enable movement of the sample within the sample testing chamber 31 without disrupting the vacuum state of the chamber.

[0136] In some embodiments, the analysis and testing system body 30 is disposed on a first platform 101. Both the first platform 101 and the second platform 102 are formed with through-holes. The through-hole of the first platform 101 communicates with the sample testing cavity 31. The through-hole of the second platform 102 is larger than the through-hole of the first platform 101. The rod 92 of the stage 90 extends through the through-holes of the first and second platforms 101, 102. Specifically, a raised portion 103 is provided below the through-hole of the second platform 102. The vertical relative position of the raised portion 103 and the second platform 102 is fixed, but the horizontal relative position is adjustable. The rod 92 of the stage 90 is fixed to the center of the bottom surface of the raised portion 103.

[0137] In some embodiments, the coordinate adjustment assembly 1021 includes a transverse coordinate adjustment member 10211, a longitudinal coordinate adjustment member 10212, and a normal coordinate adjustment member 10213. The transverse coordinate adjustment member 10211 is disposed in the transverse direction of the raised portion 103 and is used to enable the raised portion 103 to move in the transverse direction, thereby further enabling the rod portion 92 of the loading platform 90 to move in the transverse direction. The longitudinal coordinate adjustment member 10212 is disposed in the longitudinal direction of the raised portion 103 and is used to enable the raised portion 103 to move in the longitudinal direction, thereby further enabling the rod portion 92 of the loading platform 90 to move in the longitudinal direction. The normal coordinate adjustment member 10213 includes an extension portion 102131 and an adjustment portion 102132. The upper end of the extension portion 102131 is fixedly connected to the first platform 101, and the lower end of the extension portion 102131 partially extends into the adjustment portion 102132. The upper end of the adjustment portion 102132 is fixedly connected to the lower portion of the second platform 102. The adjustment portion 102132 is used to adjust the length of the extension portion 102131 extending into the adjustment portion 102132. By changing the length of the extension portion 102131 extending into the adjustment portion 102132, the height of the distance between the first platform 101 and the second platform 102 is changed, thereby enabling the rod portion 92 of the sample stage 90 to move in the lateral and vertical directions. The lateral coordinate adjustment member 10211, the longitudinal coordinate adjustment member 10212, and the normal coordinate adjustment member 10213 enable the rod portion 92 of the sample stage 90 to move in the lateral, longitudinal, and perpendicular directions.

[0138] In some embodiments, the coordinate platform 100 further includes a plurality of platform connectors 104 . The plurality of platform connectors 104 penetrate the first platform 101 and the second platform 102 to improve the stability of the coordinate platform 100 .

[0139] like Figure 2 and Figure 4As shown, in some embodiments, the analysis and testing system 1 further includes a bellows 110, the ends of which are sealedly connected to the stage 90 and the chamber, respectively, to maintain a vacuum state within the chamber when the stage 90 adjusts the position of the sample. By providing the bellows 110, which is sealedly connected to the stage 90 and the sample testing chamber 31, the stage 90 is placed in the sealed vacuum sample testing chamber 31, thereby enabling the sample to be moved within the sample testing chamber 31 without disrupting the vacuum state of the sample testing chamber 31.

[0140] like Figure 2 As shown, in some embodiments, the outer diameter of the bellows 110 is smaller than the through hole of the second platform 102 to prevent the bellows 110 from colliding with the second platform 102 when the height between the first platform 101 and the second platform 102 is reduced.

[0141] like Figure 2 and Figure 4 As shown, in some embodiments, the analysis and testing system 1 also includes a vacuum module 120, which is configured to be fixedly connected to the analysis and testing system body 30, and is configured to maintain the vacuum degree of the sample test cavity 31 when testing using the laser induced breakdown spectroscopy analysis module 10, so as to provide the vacuum environment required for laser induced breakdown spectroscopy analysis.

[0142] In some embodiments, the vacuum module 120 is disposed on one of the walls of the analysis and testing system body 30 and communicates with the sample testing chamber 31 to adjust the vacuum level of the sample testing chamber 31 .

[0143] In some embodiments, the vacuum module 120 may include a vacuum pump unit, a vacuum pipe, a vacuum gauge, a solenoid valve, etc. The vacuum pump unit is used to evacuate the sample test chamber 31; the vacuum pipe is connected to the vacuum pump unit to exhaust the gas extracted by the vacuum pump unit; the vacuum gauge is connected to the vacuum pipe to measure the vacuum level of the sample test chamber 31; and the solenoid valve is connected to the vacuum pipe to control the opening and closing of the vacuum pipe.

[0144] like Figure 4 As shown, in some embodiments, the analysis and testing system 1 also includes a purge module 130, which is configured to be fixedly connected to the analysis and testing system body 30, and is configured to purge the sample surface when testing using the laser induced breakdown spectroscopy analysis module 10 to remove impurities remaining on the sample surface to avoid affecting the analysis results.

[0145] In some embodiments, the purge module 130 may include a gas source, a pipeline, a flow control valve, and a sample nozzle. The gas source is used to provide purge gas; the pipeline is connected to the gas source and is used to transmit the purge gas provided by the gas source; the flow control valve is connected to the pipeline and is used to control the flow of the purge gas in the pipeline to purge the sample at different flow rates; and the sample nozzle is connected to the pipeline and is directed at the sample surface to purge the sample surface.

[0146] like Figure 2 As shown, in some embodiments, the analysis and testing system 1 also includes a measurement and control system 140, which can measure and control the laser induced breakdown spectroscopy analysis module 10, the X-ray fluorescence analysis module 20, the optical path channel 40, the coordinate platform 100, the sample test chamber 31, the vacuum module 120 and the purge module 130 through communication.

[0147] In some embodiments, when performing laser induced spectroscopy analysis, the measurement and control system 140 can control the coordinate adjustment component 1021 to synchronously move the sample along a preset path in the sample testing cavity 31 until the laser induced spectroscopy analysis process is completed.

[0148] In some embodiments, when performing laser induced spectroscopy analysis, the measurement and control system 140 can start and stop the vacuum pump unit by controlling the power switch of the vacuum pump unit, thereby achieving a vacuum state in the sample testing chamber 31.

[0149] In some embodiments, when performing laser induced spectroscopy analysis, the measurement and control system 140 can synchronously purge the sample with the purge gas by controlling the flow regulating valve.

[0150] Regarding the embodiments of the present application, it should also be noted that, in the absence of conflict, the embodiments of the present application and the features therein can be combined with each other to obtain new embodiments.

[0151] The above description is only a specific implementation method of the present application, but the protection scope of the present application is not limited thereto. The protection scope of the present application shall be based on the protection scope of the claims.

Claims

1. A method for analyzing and testing the element beryllium in rocks, characterized in that: It includes the following steps: S10: preparing a sample of the rock, wherein the sample includes the element beryllium and a reference element; S20: preparing a standard sample of rock with known composition, wherein the standard sample includes the reference element and the element beryllium, and the concentrations of the reference element and the element beryllium in the standard sample are known; S30: Obtain an X-ray fluorescence spectrum of the standard sample, and determine the relationship between the concentration of the reference element and its X-ray peak signal intensity according to the X-ray fluorescence spectrum; S40: Obtaining an X-ray fluorescence spectrum of the sample, and determining the concentration of the reference element in the sample according to the relationship determined in 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, the sensitivity coefficient of the reference element and the element beryllium determined in step S50, and the concentration of the reference element in the sample; In step S30, The relationship between the concentration of the reference element in the standard sample and the intensity of its X-ray peak signal conforms to the following expression: ； In the formula, represents the X-ray peak signal intensity of the reference element in the standard sample; represents the concentration of the reference element in the standard sample; represents a constant; represents a constant; In step S40, The relationship between the concentration of the reference element in the sample and the intensity of its X-ray peak signal conforms to the following expression: ； In the formula, represents the X-ray peak signal intensity of the reference element in the sample; represents the concentration of the reference element in the sample; represents a constant; represents a constant; In step S50, The sensitivity coefficient of the element beryllium conforms to the following expression: ； In the formula, R LIBS ( i / j ) represents the sensitivity coefficient of the reference element to 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 beam peak signal intensity of the reference element in the standard sample; C represents the concentration of the reference element in the standard sample; C represents the concentration of the element beryllium in the standard sample; In step S60, The relationship between the concentration of the element beryllium in the sample and the sensitivity coefficient of the reference element to the element beryllium conforms to the following expression: ； In the formula, 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 to the element beryllium; A LIBS ( j ) represents the laser ray peak signal intensity of the element beryllium in the sample; A LIBS ( i ) represents the laser beam peak signal intensity of the reference element in the sample; represents the concentration of the reference element in the sample.

2. The method according to claim 1, characterized in that In step S10, the following steps are also included: S11: Powdering the rock; S12: Form the powder into a disk shape to obtain the sample.

3. The method according to claim 2, characterized in that In step S30, the following steps are also included: S31: Obtain X-ray fluorescence spectra of the plurality of standard samples, and determine the X-ray peak signal intensity of the reference element in the plurality of standard samples; S32: determining a curve of the relationship 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: Determine a relationship between the X-ray peak signal intensity and the concentration of the reference element according to the curve determined in step S32.

4. The method according to claim 3, characterized in that In step S50, the following steps are also included: Determining the characteristic wavelength of the laser beam according to the reference element and the element beryllium; The laser beam peak signal intensities of the reference element and the element beryllium in the laser induced breakdown spectrum are determined according to the laser beam characteristic wavelength.

5. The method according to claim 4, characterized in that In step S60, the following steps are also included: Determining the characteristic wavelength of the laser beam according to the reference element and the element beryllium; The laser beam peak signal intensities of the reference element and the element beryllium in the laser induced breakdown spectrum are determined according to the laser beam characteristic wavelength.

6. The method according to claim 5, characterized in that The method is implemented by using an analysis and testing system that combines X-ray fluorescence spectroscopy and laser induced breakdown spectroscopy, and the analysis and testing system also includes: a laser transmitter, The method further comprises the following steps: The distance between the laser emitted by the laser emitter and the sample is adjusted so that the laser is focused on the surface of the sample.

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