Method for analyzing and testing element beryllium in rock

Abstract

The embodiment of the invention relates to the technical field of analysis and test of chemical properties of materials, in particular to a method for analyzing and testing beryllium in rock, which comprises the following steps: S30, acquiring an X-ray fluorescence spectrogram of a standard sample, and determining the relationship between the concentration of a reference element and the X-ray peak signal intensity of the reference element; s40, acquiring an X-ray fluorescence spectrogram of the sample, and determining the concentration of a reference element in the sample; s50, acquiring a laser-induced breakdown spectrogram of the standard sample, and determining sensitivity coefficients of the reference element and the element beryllium; and S60, acquiring a laser-induced breakdown spectrogram of the sample, and determining the concentration of the element beryllium in the sample according to the laser-induced breakdown spectrogram, the sensitivity coefficients of the reference element and the element beryllium determined in the step S50 and the concentration of the reference element in the sample. According to the embodiment of the invention, the sensitivity coefficient of the reference element and the element beryllium is determined, and the coefficient is used for correcting the concentration of the element beryllium in the sample, so that the accuracy of analyzing the test structure is improved.

Description

Technical Field

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

[0002] This section of content merely provides background information related to the present application and does not necessarily constitute prior art.

[0003] The element 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 usually used in technical fields such as the atomic energy industry, metallurgical industry, aerospace, etc.

[0004] At present, the main analytical measurement method for the concentration of beryllium in rocks is inductively coupled plasma emission spectrometry, which uses wet chemical methods to digest rocks and has high accuracy in analytical results. However, inductively coupled plasma emission spectrometry requires chemical pretreatment of samples and standard samples, so there are problems such as complex analytical testing procedures and low analytical testing efficiency. Summary of the invention

[0005] A brief overview of the present application is provided below in order 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 the key or important parts of the present application, nor is it intended to limit the scope of the present application. Its purpose is merely to present certain concepts in a simplified form as a prelude to a more detailed description discussed later.

[0006] The embodiment of the present application provides a method for analyzing and testing the element beryllium in rocks, which comprises: S10: Prepare a rock sample, the sample comprising the element beryllium and a reference element.

[0007] 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.

[0008] 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.

[0009] S40: Obtain an X-ray fluorescence spectrum of the sample, and determine the concentration of the reference element in the sample according to the relationship determined in step S30.

[0010] S50: Obtain a laser induced breakdown spectrum of the standard sample, and determine the 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.

[0011] S60: Obtain a laser induced breakdown spectrum of the sample, and determine 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.

[0012] The embodiment of the present application performs X-ray fluorescence and laser induced breakdown analysis tests on samples and standard samples, thereby eliminating the need for chemical pretreatment of samples and standard samples, simplifying the analysis and testing process and improving the efficiency of the analysis and testing of beryllium concentration 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 by the sensitivity coefficients of the reference element and the element beryllium, thereby improving the accuracy of the analysis results. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] In order to further illustrate the above and other advantages and features of the present application, the specific embodiments of the present application are further described in detail below in conjunction with the accompanying drawings. The accompanying drawings together with the following detailed description are included in this specification and form a part of this specification. Elements with the same function and structure are represented by the same reference numerals. It should be understood that these drawings only describe typical examples of the present application and should not be regarded as limiting the scope of the present application.

[0014] 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 2 is a schematic diagram of an analysis and testing system according to an embodiment of the present application; Figure 3 is a side view of an analytical testing system according to an embodiment of the present application; Figure 4 is a partial cross-sectional view of an analysis and testing system according to an embodiment of the present application; Figure 5 It is a partially enlarged schematic diagram of an analysis and testing system according to an embodiment of the present application.

[0015] 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.

[0016] Description of reference numerals: 1. Analysis and testing system; 10. Laser induced breakdown spectroscopy analysis module; 11. Laser transmitter; 12. Spectrometer; 13. Light guide; 14. First light focusing element; 20. X-ray fluorescence analysis module; 21. X-ray source; 22. X-ray energy detector; 30. Analysis and testing system body; 31. Sample testing cavity; 32. Structure of projecting light; 40. Optical channel; 41. Horizontal channel; 50. a first fixing member; 60. second fixing member; 70. Optical fiber; 80. Support member; 81. Support column; 82. Support body; 90. stage; 91. support portion; 92. rod portion; 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, protrusion; 104, platform connector; 110. Bellows; 120. Vacuum module; 130. Purge module; 140. Measurement and control system. DETAILED DESCRIPTION

[0017] Exemplary embodiments of the present application will be described below in conjunction with the accompanying drawings. For the sake of clarity and conciseness, not all features of the actual implementation 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 from implementation to implementation. In addition, it should be understood that although the development work may be very complex and time-consuming, it is only a routine task for those skilled in the art who benefit from the content of this application.

[0018] It is also necessary to explain here that, in order to avoid obscuring the present application due to unnecessary details, only the device structure and / or processing steps closely related to the scheme according to the present application are shown in the accompanying drawings, while other details that are not very relevant to the present application are omitted.

[0019] It should be noted that, unless otherwise defined, the technical terms or scientific terms used in this application should have the common meanings understood by persons with ordinary skills in the field to which this application belongs.

[0020] In the description of the embodiments of the present application, “plurality” means at least two, such as two, three, etc., unless otherwise clearly and specifically defined.

[0021] The inventors of the present invention have found that the laser induced breakdown spectroscopy method has a fast analysis speed and does not require sample pretreatment in the application of sample analysis. However, its disadvantage is that the spectrum stability is poor, resulting in poor repeatability of the test results; the X-ray fluorescence method has a fast analysis speed in the application of sample analysis, but it is not suitable for analyzing and testing low-mass number elements (such as lithium and beryllium).

[0022] Based on this, an embodiment of the present application provides a method for analyzing and testing the element beryllium in rocks. Figure 1 The following 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: S10: Prepare a rock sample, the sample comprising the element beryllium and a reference element.

[0023] 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.

[0024] 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.

[0025] S40: Obtain an X-ray fluorescence spectrum of the sample, and determine the concentration of the reference element in the sample according to the relationship determined in step S30.

[0026] S50: Obtain a laser induced breakdown spectrum of the standard sample, and determine the 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.

[0027] S60: Obtain a laser induced breakdown spectrum of the sample, and determine 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.

[0028] The embodiment of the present application performs X-ray fluorescence and laser induced breakdown analysis tests on samples and standard samples, thereby eliminating the need for chemical pretreatment of samples and standard samples, simplifying the analysis and testing process, and improving the analysis and testing efficiency of beryllium concentration 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 by the sensitivity coefficients of the reference element and the element beryllium, thereby overcoming the problem in the prior art that the X-ray fluorescence method is not applicable to elements with low mass numbers in the application of sample analysis, that is, improving the accuracy of the analysis results.

[0029] 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: (1).

[0030] In the formula, 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; Indicates a constant. 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.

[0031] 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: (2).

[0032] In the formula, 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.

[0033] In some embodiments, the reference element can be selected according to the composition of the sample. In some embodiments, the reference element can be calcium and iron.

[0034] In some embodiments, in step S50, the sensitivity coefficient of the element beryllium satisfies the following expression: (3).

[0035] In the formula, 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 peak signal intensity of the laser beam 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 element beryllium in the standard sample. The concentration of element beryllium in the sample is corrected by the sensitivity coefficient between the reference element and element beryllium to improve the accuracy of the analysis and test results of element beryllium in the sample.

[0036] In some embodiments, in step S60, the relationship between the concentration of the element beryllium in the sample and the sensitivity coefficient between the reference element and the element beryllium conforms to the following expression: (4).

[0037] In the formula, 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 the 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.

[0038] In some embodiments, in step S10, the following steps are also included: S11: Turn the rock into powder.

[0039] S12: The powder is formed into a disc shape to obtain a sample.

[0040] To obtain samples suitable for X-ray fluorescence spectrometry analysis and laser induced breakdown spectrometry analysis.

[0041] In some embodiments, the rock sample is crushed into powder with a particle size ranging from 20 to 70 μm, for example, 20 μm.

[0042] In some embodiments, the powder can be pressed into a regular round tablet shape with a flat surface by a tablet press.

[0043] In some embodiments, in step S30, the following steps are also included: 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.

[0044] S32: Determine a curve of the relationship between the X-ray peak signal intensity and the reference element according to the intensity of the multiple standard samples and the concentration of the reference element in the multiple standard samples.

[0045] 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.

[0046] A curve of 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 the 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.

[0047] 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, wherein the constants in expression (1) and expression (2) can be determined based on the determined expression: With constant .

[0048] 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.

[0049] 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.

[0050] In some embodiments, in step S50, the following steps are also included: S51: Determine the characteristic wavelength of the laser beam based on the reference element and the element beryllium.

[0051] 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.

[0052] 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.

[0053] Specifically, different elements have corresponding characteristic wavelengths of laser rays, and through their corresponding characteristic wavelengths of laser rays, the laser ray peak corresponding to the element can be determined in the laser induced breakdown spectrum.

[0054] In some embodiments, the characteristic wavelength of beryllium laser radiation may be 313 nm.

[0055] In some embodiments, in step S60, the following steps are also included: S61: Determine the characteristic wavelength of the laser beam based on the reference element and the element beryllium.

[0056] 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.

[0057] 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.

[0058] 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 further comprising: a laser transmitter, and the method further comprising the following steps: adjusting the distance between the laser emitted by the laser transmitter and the sample so that the laser is focused on the sample surface, so as to achieve effective irradiation of the sample with the laser, thereby ensuring the accuracy of the experimental results.

[0059] In some embodiments, the laser wavelength emitted by the laser emitter is less than 1064 nm, for example, may be 532 nm.

[0060] In some embodiments, the laser energy emitted by the laser transmitter can be adjusted according to actual conditions, and the laser energy range is 20-300 mJ, for example, it can be 100 mJ.

[0061] 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.

[0062] Example 1 The rock sample was crushed into powder with a particle size of about 70 μm, and prepared into regular round tablets with a flat surface by a tablet press. A rock standard sample containing the reference element calcium was prepared.

[0063] 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 to obtain the slope and intercept of the relationship curve. Based on the slope and intercept of the relationship curve, an expression (1) between the X-ray peak signal intensity of elemental calcium in the standard sample and the corresponding elemental calcium concentration is obtained.

[0064] Similarly, the rock sample is subjected to X-ray fluorescence spectroscopy analysis 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.

[0065] 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.

[0066] Adjust the distance between the optical lens and the rock sample, set the spectrometer working parameters, integration time, working wavelength, trigger mode, etc.; set the synchronous trigger signal so that the spectrometer and the laser transmitter are in the same frequency working mode. Select 313nm as the characteristic wavelength of the laser beam of the element beryllium, and select 272nm as the characteristic wavelength of the laser beam of the element calcium.

[0067] The rock sample was subjected to laser induced breakdown spectroscopy analysis to obtain a laser induced breakdown spectrum. The signal intensity of the 313nm laser beam peak in the laser induced breakdown spectrum was recorded as the signal intensity of the laser beam peak of the element beryllium in the rock sample, and the signal intensity of the 272nm laser beam peak was recorded as the signal intensity of the laser beam peak of the element calcium in the rock sample.

[0068] 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.

[0069] According to the laser beam peak signal intensity of element beryllium and element calcium in the rock sample and the concentration of element calcium and element beryllium in the rock standard sample, expression (3) and the sensitivity coefficients of element calcium and element beryllium are obtained.

[0070] According to the laser beam peak signal intensity of element beryllium and element calcium in the rock sample, the concentration of element calcium in the rock sample and the sensitivity coefficient of element calcium and element beryllium, expression (4) and the concentration of element beryllium in the rock sample are obtained.

[0071] Example 2 The rock sample is crushed into powder with a particle size of about 20 μm, and is prepared into a regular round tablet with a flat surface by a tablet press. A plurality of rock standard samples containing different concentrations of the reference element iron are prepared.

[0072] 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 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 intensity of elemental iron in the standard samples and the elemental iron content is established, and the relationship expression is determined through the relationship curve to obtain the expression (1) between the X-ray peak signal intensity of elemental iron in the standard samples and the corresponding elemental iron content.

[0073] Similarly, the rock sample is subjected to X-ray fluorescence spectroscopy analysis 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.

[0074] 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.

[0075] Adjust the distance between the optical lens and the rock sample, set the integration time, working wavelength, and trigger mode of the spectrometer; set the synchronous trigger signal so that the spectrometer and the laser transmitter are in the same frequency working mode. Select 313nm as the characteristic wavelength of the laser beam of the element beryllium, and select 234.8nm as the characteristic wavelength of the laser beam of the element iron.

[0076] The rock sample was subjected to laser induced breakdown spectroscopy analysis to obtain a laser induced breakdown spectrum. The signal intensity of the laser ray peak at 313 nm in the laser induced breakdown spectrum was recorded as the signal intensity of the laser ray peak of the element beryllium in the rock sample, and the signal intensity of the laser ray peak at 234.8 nm was recorded as the signal intensity of the laser ray peak of the element iron in the rock sample.

[0077] 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.

[0078] 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.

[0079] 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.

[0080] In order to implement the method of analyzing and testing the element beryllium in rocks in the present application, the embodiment of the present 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 3As 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; and an analysis and testing system body 30, wherein the analysis and testing system body 30 forms a sample test cavity 31, the sample is arranged 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 emitted by the laser induced breakdown spectroscopy analysis module 10 irradiates 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, which is detected by the laser induced breakdown spectroscopy analysis module 10 to determine the elemental composition and content of the sample; the X-rays emitted by the X-ray fluorescence analysis module 20 irradiate the sample in the sample test cavity 31, and detect the fluorescent X-rays generated by the sample after irradiation to determine the chemical properties of the sample.

[0081] 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 therein 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 influence 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.

[0082] Figure 4 FIG. 1 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 a plurality of walls, and the plurality of walls 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 plurality of 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, thereby preventing interference with the laser induced breakdown spectroscopy analysis and the X-ray fluorescence analysis of the sample.

[0083] like Figure 4As shown, in some embodiments, the analysis and testing system 1 further includes: an optical path channel 40, a first fixing member 50, a second fixing member 60, and an optical fiber 70. The analysis and testing system body 30 includes a plurality of walls, and the plurality of walls form a sample test cavity 31. The optical path channel 40 is configured to be fixedly connected to one of the plurality of walls, and a structure 32 for projecting light is provided on the wall, so that the laser emitted from the laser induced breakdown spectrometry analysis module 10 can irradiate the sample disposed in the sample test cavity 31. The first fixing member 50 is configured to be fixedly connected to one of the plurality of walls, and is configured to be fixedly connected to a portion of the X-ray fluorescence analysis module 20, so that the X-ray emitted by the X-ray fluorescence analysis module 20 can irradiate the sample disposed 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 where the first fixing member 50 is disposed. The second fixing member 60 is fixedly disposed on one of the plurality of walls, and is configured to fix the optical fiber 70, so that the optical fiber 70 receives the light reflected by the laser 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 different 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 sample in the sample testing cavity 31 by the laser and X-ray light and the transmission of the laser reflected light.

[0084] In some embodiments, the structure 32 for projecting light may be a quartz window for introducing laser light into the cavity from the atmosphere side.

[0085] In some embodiments, the second fixture 60 is connected to the sample testing cavity 31 and is used to fix the optical fiber 70 so that the optical fiber 70 enters the sample testing cavity 31 through the second fixture 60. In some embodiments, the second fixture 60 may be a through flange.

[0086] In some embodiments, the optical fiber 70 may be a silica optical fiber.

[0087] like Figure 2 and Figure 4As shown, in some embodiments, the analysis and testing system 1 further includes a support 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, wherein the laser emitter 11 is arranged on the support 80, the light guide 13 is arranged in the optical path channel 40, and the spectrometer 12 is arranged outside the analysis and testing system body 30. The laser emitted by the laser emitter 11 irradiates the light guide 13, and then irradiates the sample after being transmitted by the light guide 13, and then is reflected by the sample to the optical fiber 70, and then is transmitted by the optical fiber 70 to the spectrometer 12, and then detected 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, and the composition of the emitted light generated by the sample after 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.

[0088] In some embodiments, the support member 80 is provided with a plurality of support columns 81 and a support body 82, the plurality of support columns 81 are used to support the support body 82, the support body 82 is provided with a plurality of walls, and the laser emitter 11 is arranged on the wall of the support body 82 opposite to the analysis and testing system body 30. In some embodiments, a horizontal channel 41 communicating with the optical path channel 40 is formed on the wall opposite to the support body 82. The horizontal channel 41 is arranged in parallel with the laser emitter 11, and the laser outlet of the laser emitter 11 is in the same straight line as the center of the horizontal channel 41. The laser emitted by the laser emitter 11 can enter the optical path channel 40 through the horizontal channel 41.

[0089] In some embodiments, the output wavelength of the laser emitter 11 can be 1064nm, 532nm or other shorter wavelength lasers (such as 256nm), and the laser power selection range can be 20~300mJ, which is used to provide a high-energy monochromatic excitation light source.

[0090] 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 in the same straight line as the laser outlet of the laser emitter 11 and the center of the horizontal channel 41. Specifically, the laser passes through the horizontal channel 41 and irradiates the light guide 13, and the light guide 13 changes the path of the laser emitted by the laser emitter 11, so that the laser irradiates the sample.

[0091] 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 irradiates the sample.

[0092] In some embodiments, the laser induced breakdown spectroscopy analysis module 10 further includes a first light focusing member 14, which is disposed between the light guide member 13 and the structure 32 for projecting light, so that the laser light is focused on the sample surface inside the cavity after passing through the structure 32 for projecting light light. This prevents unnecessary loss of laser energy, thereby ensuring effective irradiation of the sample by the laser light. Specifically, the first light focusing member 14 may be a convex lens.

[0093] In some embodiments, the LIBS analysis module 10 further includes a second light focusing element for focusing the emission light generated by laser irradiation on the sample surface and transmitting the emission light to the optical fiber 70 .

[0094] 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 to improve the analysis efficiency of the spectrometer 12 .

[0095] 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 disposed on one of the multiple walls through a first fixing member 50, and the X-ray energy detector 22 is fixedly disposed on one of the multiple walls opposite to one of the multiple walls where the first fixing member 50 is disposed. The X-rays emitted by the X-ray source 21 irradiate the sample, and the X-rays reflected from the sample are detected by the X-ray energy detector 22. By respectively arranging the X-ray source 21 and the X-ray energy detector 22 on one of the multiple walls, it is avoided that the X-ray source 21 and the X-ray energy detector 22 come into contact during the analysis and testing process, thereby preventing the X-ray source 21 and the X-ray energy detector 22 from interfering with the normal operation of the X-ray source 21 and the X-ray energy detector 22, and the two walls respectively disposed are opposite to each other, so as to ensure that after the sample is irradiated with the X-rays, the X-rays reflected from the sample can be detected by the X-ray energy detector 22.

[0096] 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 .

[0097] In some embodiments, the excitation voltage range of the X-ray source 21 may be 20 kV to 50 kV, for example, 30 kV.

[0098] 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.

[0099] 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.

[0100] like Figure 4As shown, in some embodiments, the X-ray source 21 and the X-ray energy detector 22 are arranged so that the extension lines of their centers form a predetermined angle and converge on the surface of the sample, which is used to limit the optical path of the X-ray irradiating the sample and the X-ray reflected by the sample, so as to prevent the X-ray and the reflected X-ray from being too close or too far from each other, thereby preventing the accuracy of the X-ray fluorescence spectrum analysis of the sample from being disturbed.

[0101] 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, it can be 45°.

[0102] 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, and the stage 90 is configured to be sealed and connected to the cavity, and can be adjusted in three directions, namely, in the horizontal direction, in the vertical direction, and in the vertical direction. The stage 90 can be used to move the sample to the corresponding test position when switching between laser induced spectroscopy analysis and X-ray fluorescence spectroscopy analysis.

[0103] 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 part of the rod portion 92 are disposed in the sample testing cavity 31, and the sample is disposed on the support portion 91.

[0104] like Figure 4 As shown, in some embodiments, the analysis and testing system 1 further includes a coordinate platform 100 and a coordinate adjustment component 1021. The coordinate platform 100 includes 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 height of the spacing between the first platform 101 and the second platform 102 is adjustable. The coordinate adjustment component 1021 is arranged on the second platform 102, and is used to realize the movement of the sample in the sample testing cavity 31 without destroying the vacuum state of the cavity.

[0105] In some embodiments, the analysis and testing system body 30 is disposed on the first platform 101, and both the first platform 101 and the second platform 102 are formed with through holes. The through hole of the first platform 101 is connected to the sample testing cavity 31, the through hole of the second platform 102 is larger than the through hole of the first platform 101, and the rod 92 of the stage 90 passes through the through holes of the first platform 101 and the second platform 102. Specifically, a protrusion 103 is provided below the through hole of the second platform 102, and the vertical relative position of the protrusion 103 and the second platform 102 is fixed, and the horizontal relative position is adjustable, and the rod 92 of the stage 90 is fixed at the center of the bottom surface of the protrusion 103.

[0106] In some embodiments, the coordinate adjustment component 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 arranged in the transverse direction of the protrusion 103, and the transverse coordinate adjustment member 10211 is used to realize the movement of the protrusion 103 in the transverse direction, and further realize the movement of the rod 92 of the stage 90 in the transverse direction. The longitudinal coordinate adjustment member 10212 is arranged in the longitudinal direction of the protrusion 103, and is used to realize the movement of the protrusion 103 in the longitudinal direction, and further realize the movement of the rod 92 of the stage 90 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 part 102131 is fixedly connected to the first platform 101, and the lower end of the extension part 102131 partially extends into the adjustment part 102132; the upper end of the adjustment part 102132 is fixedly connected to the lower part of the second platform 102, and the adjustment part 102132 is used to adjust the length of the extension part 102131 extending into the adjustment part 102132. By changing the length of the extension part 102131 extending into the adjustment part 102132, the height of the spacing between the first platform 101 and the second platform 102 is changed, so as to realize the movement of the rod part 92 of the stage 90 in the horizontal and vertical directions. The horizontal coordinate adjustment member 10211, the vertical coordinate adjustment member 10212 and the normal coordinate adjustment member 10213 realize the movement of the rod part 92 of the stage 90 in the horizontal, vertical and vertical directions, so as to realize the movement of the sample in the horizontal, vertical and vertical directions.

[0107] In some embodiments, the coordinate platform 100 further includes a plurality of platform connectors 104 , and 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 .

[0108] like Figure 2 and Figure 4As shown, in some embodiments, the analysis and testing system 1 further includes a bellows 110, and both ends of the bellows 110 are respectively sealedly connected to the stage 90 and the cavity, so that the cavity is kept in a vacuum state when the stage 90 adjusts the position of the sample. By providing the bellows 110 sealedly connected to the stage 90 and the sample test cavity 31, the stage 90 is arranged in the sealed vacuum sample test cavity 31, so that the sample can be moved in the sample test cavity 31 without destroying the vacuum state of the sample test cavity 31.

[0109] 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.

[0110] 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.

[0111] 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 degree of the sample testing chamber 31 .

[0112] In some embodiments, the vacuum module 120 may include a vacuum pump unit, a vacuum pipeline, a vacuum gauge, a solenoid valve, etc. The vacuum pump unit is used to evacuate the sample test cavity 31; the vacuum pipeline is connected to the vacuum pump unit to discharge the gas extracted by the vacuum pump unit; the vacuum gauge is connected to the vacuum pipeline to measure the vacuum degree of the sample test cavity 31; the solenoid valve is connected to the vacuum pipeline to control the opening and closing of the vacuum pipeline.

[0113] 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.

[0114] 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; the sample nozzle is connected to the pipeline and is aimed at the sample surface to purge the sample surface.

[0115] 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.

[0116] 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 chamber 31 until the laser induced spectroscopy analysis process is completed.

[0117] 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 of the sample test chamber 31.

[0118] 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.

[0119] 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.

[0120] The above description is only a specific implementation manner 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: Obtain a laser induced breakdown spectrum of the sample, and determine 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.

2. The method according to claim 1, characterized in that 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.

3. The method according to claim 2, characterized in that 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.

4. The method according to claim 3, characterized in that 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 beam 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.

5. The method according to claim 4, characterized in that 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 beam 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.

6. The method according to any one of claims 1 to 5, 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.

7. The method according to claim 6, 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.

8. The method according to claim 7, 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.

9. The method according to claim 7, 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.

10. The method according to claim 9, 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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