A high-efficiency X-ray fluorescence spectrometer and its use method

Abstract

The present invention relates to the field of spectral detection and analysis, and discloses an efficient X-ray fluorescence spectrometer and a method for using the same. The spectrometer comprises: an X-ray generator, a spectroscopic unit, a controller and an XRF workstation, wherein the spectroscopic unit comprises an injection system, a spectrometer, a detector and a temperature-controlled heater; the injection system comprises an injector, a lifter, a rotator and a turntable, wherein the lifter is arranged below the rotator, the injector is connected above the rotator, the turntable is connected to the injector through a fixed block, a sample box is arranged on the upper part of the turntable, and the sample box comprises a plurality of samples, each sample box corresponds to a spectrometer and a detector and is independently detected, and the detector is connected to the controller in communication. The present invention changes and rearranges the internal structure of the spectrometer, and a plurality of spectrometers and detectors are arranged, wherein each sample box independently corresponds to a spectrometer and a detector for detection and analysis, and multiple sample samples can be detected and analyzed simultaneously, greatly improving the detection and analysis efficiency.

Description

Technical Field

[0001] The present invention relates to the field of spectrum detection and analysis, and in particular to an efficient X-ray fluorescence spectrometer and a method for using the same. Background Art

[0002] X-ray fluorescence spectrometer is a device used to detect the types and contents of elements in mixed substances. Its basic principle is to emit primary X-rays to the sample material. The primary X-rays provide enough energy for the electrons on the atoms to free some of the electrons from the atoms and cause electron transitions. During the transition, part of the energy is released in the form of secondary X-rays. The secondary X-rays released by different elements have specific energy characteristics. By comparing these characteristics, the types and contents of elements in the mixed substance sample can be determined.

[0003] Due to its high analysis accuracy, simple samples required, and the fact that solid, powder, and liquid samples can all be tested and analyzed, X-ray fluorescence spectroscopy has been widely used in many fields such as metallurgy, geology, nonferrous metals, building materials, commodity inspection, environmental protection, and sanitation in recent years. The existing detection spectrometers take 8 to 25 minutes to detect a single sample, and most spectrometers cannot detect and analyze multiple samples at the same time. For example, a common XRF spectrometer has a total of 8 sample positions for sample measurement, but can only analyze one sample at a time, and the sample must be replaced manually after the measurement. During use, there are the disadvantages of long total detection and analysis time and frequent sample changes. Therefore, the measurement and analysis efficiency is low, the time is long, and it is not friendly to the sample tester. Summary of the invention

[0004] The present invention provides an efficient X-ray fluorescence spectrometer and a method for using the same, which overcome the disadvantage of low detection and analysis efficiency of the existing XRF spectrometer.

[0005] An efficient X-ray fluorescence spectrometer comprises: an X-ray generator for generating primary X-rays, a spectroscopic unit, a controller and an XRF workstation, wherein the spectroscopic unit comprises a sample introduction system, a spectrometer, a detector and a temperature-controlled heater;

[0006] The sample injection system includes a sample injector, a lifter, a rotator and a turntable for transferring a sample box containing a sample to the inside of a sample chamber, wherein the lifter is arranged below the rotator, the sample injector is connected above the rotator, the turntable is connected to the sample injector through a fixed block, and the sample box is arranged on the upper part of the turntable;

[0007] The sample boxes include a plurality of samples, each of which corresponds to a spectrometer and a detector, and the detectors are independently detected from each other, and the detectors are in communication connection with the controller.

[0008] Furthermore, the sample box comprises a box body, a tray arranged inside the box body and a cover plate arranged on the upper part of the box body, the tray is rotatably arranged at the bottom of the box body through a bearing, and a spring is arranged on the tray.

[0009] Furthermore, the above-mentioned spectrometer includes a primary slit, an attenuator, a crystal converter, a spectroscopic crystal and a secondary slit. The primary slit is connected to the filter inside the sample chamber through a light hole. The attenuator is arranged at the light output end of the primary slit. The spectroscopic crystal is installed on the crystal converter. The secondary slit is connected to the detector at the light output end.

[0010] Furthermore, the above XRF workstation includes a computer with a display, a mouse, and a keyboard. The computer is connected to the CPU via an RS-232C serial port, and the computer is also connected to a printer.

[0011] Furthermore, the controller includes a mainboard and a CPU, the CPU is mounted on the mainboard, the mainboard is respectively connected to the spectroscopic unit and the X-ray generator for communication, and the CPU is connected to a computer of the XRF workstation.

[0012] Furthermore, the above-mentioned X-ray generator includes an X-ray tube, a high-voltage converter and an X-ray power supply. The high-voltage converter is connected to the X-ray tube and the X-ray power supply respectively. The X-ray tube is connected to the X-ray power supply through a filament to form a complete circuit.

[0013] Furthermore, the detector includes a scintillation counter for detecting heavy metals and a gas flow proportional counter for detecting light elements.

[0014] Furthermore, the temperature-controlled heater is arranged in the sample chamber, and includes a heater and a fan.

[0015] Furthermore, the above-mentioned spectrometer is connected to a vacuum system, and the vacuum system includes a vacuum pump, an air release valve, and an air extraction valve.

[0016] An efficient method for using an X-ray fluorescence spectrometer, using the above scheme, comprises the following steps:

[0017] S1: Place the sample box on the turntable, which is driven by a motor to rotate and bring the sample box to the injection port;

[0018] S2: The sample box is brought to the sample inlet by the lifter and the sample injector, and enters the sample chamber under the X-ray tube to wait for detection;

[0019] S3: Open the software analysis window on the computer, select the analysis group, select the sample location and sample name, and make notes;

[0020] S4: The sample is tested and analyzed in the sample chamber, and the sample box is driven to rotate by a rotary motor during the analysis process;

[0021] S5: Determine the test analysis data, confirm the test results, and the sample box exits the sample chamber from the sample inlet.

[0022] The present invention has the following beneficial effects: the X-ray fluorescence spectrometer of the present invention is based on the traditional XRF spectrometer, the internal structure of the spectrometer is changed and rearranged, a plurality of spectrometers and detectors are arranged, and a plurality of sample boxes are arranged in the form of a uniformly distributed ring, which is convenient for containing a variety of sample samples to be detected and analyzed. Each sample box independently corresponds to a spectrometer and a detector for detection and analysis, and a plurality of sample samples can be detected and analyzed at the same time, which greatly improves the detection and analysis efficiency and saves analysis time and labor costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 It is a schematic front view of the basic structure of the present invention;

[0024] Figure 2 It is the working principle diagram of the spectrometer of the present invention;

[0025] Figure 3 A connection diagram of the controller in the present invention;

[0026] Figure 4 is a structural relationship diagram of the light splitting unit in the present invention;

[0027] Figure 5 It is a schematic diagram of the structure of the sample injection system in the present invention;

[0028] Figure 6 is a top view schematic diagram of a sample box in the present invention;

[0029] Figure 7 Schematic diagram of the internal structure of the sample box in the present invention;

[0030] Figure 8 This is a simplified diagram of the working principle of the optical splitter in the present invention.

[0031] In the figure: 1-X-ray generator; 2-spectrometric unit; 21-injection system; 211-sample chamber; 212-sample box; 2121-box body; 2122-cover; 2123-tray; 2124-bearing; 2125-spring; 213-injector; 214-lifter; 215-rotator; 216-turntable; 22-spectrometer; 221-filter; 2211-light hole; 2212-primary slit; 2213-attenuator; 2214-crystal converter; 2215-spectrometric crystal; 2216-secondary slit; 2217-scintillation counter; 2218-gas proportional counter; 23-detector; 24-temperature-controlled heater; 25-vacuum system; 3-controller; 4-XRF workstation; 5-sample. DETAILED DESCRIPTION

[0032] The principles and features of the present invention are described below in conjunction with the accompanying drawings. The examples given are only used to explain the present invention and are not used to limit the scope of the present invention.

[0033] refer to Figures 1 to 8 , the present invention provides an efficient X-ray fluorescence spectrometer, comprising: an X-ray generator 1 for generating primary X-rays, a spectroscopic unit 2, a controller 3 and an XRF workstation 4;

[0034] The X-ray generator 1 includes an X-ray tube, a high-voltage converter and an X-ray power supply. The high-voltage converter is connected to the X-ray tube and the X-ray power supply respectively. The X-ray tube is connected to the X-ray power supply through a filament to form a complete circuit. The X-ray tube generates primary X-rays for irradiating the sample 5.

[0035] When the primary X-rays are irradiated on the surface of the sample 5, the spectroscopic unit 2 can measure the fluorescent X-rays of various wavelengths emitted from the surface of the sample 5, and the types and proportions of elements can be analyzed by comparing the measured X-ray intensities.

[0036] The spectroscopic unit 2 includes an injection system 21, a spectrometer 22, a detector 23 and a temperature-controlled heater 24; the injection system 21 includes an injector 213, a lifter 214, a rotator 215 and a turntable 216 for transferring a sample box 212 containing a sample 5 to the inside of a sample chamber 211, the lifter 214 is arranged below the rotator 215, the injector 213 is connected above the rotator 215, the turntable 216 is connected to the injector 213 through a fixed block, and the sample box 212 is arranged on the upper part of the turntable 216; the sample box 212 includes a plurality of sample boxes, each sample box 212 corresponds to a spectrometer 22 and a detector 23 and detects each other independently, and the detector 23 is communicatively connected to the controller 3.

[0037] The sample box 212 includes a box body 2121 , a tray 2123 disposed inside the box body 2121 , and a cover plate 2122 disposed on the upper portion of the box body 2121 . The tray 2123 is rotatably disposed at the bottom of the box body 2121 via a bearing 2124 , and a spring 2125 is disposed on the tray 2123 .

[0038] The spectrometer 22 includes a primary slit 2212, an attenuator 2213, a crystal converter 2214, a spectroscopic crystal 2215 and a secondary slit 2216. The primary slit 2212 is connected to the filter 221 in the sample chamber 211 through the light hole 2211. The attenuator 2213 is arranged at the light output end of the primary slit 2212. The spectroscopic crystal 2215 is installed on the crystal converter 2214. The secondary slit 2216 and the light output end are connected to the detector 23. The filter 221 can filter out unnecessary characteristic X-rays to improve the accuracy of detection and analysis; the attenuator 2213 is used to adjust the intensity of the X-rays to ensure that there is enough energy to make the electrons on the atoms transition; the spectroscopic crystal 2215 separates the rays with different characteristics to facilitate comparison with the corresponding spectrum to distinguish the types of elements to be detected.

[0039] The spectrometer 22 is connected to a vacuum system 25, which includes a vacuum pump, a relief valve, and an exhaust valve. The vacuum pump is connected to the exhaust valve through a pipeline, and the relief valve and the exhaust valve are arranged in the enclosed space where the spectrometer 22 is located. When the sample 5 needs to be detected and analyzed in a vacuum environment, the vacuum pump and the exhaust valve are turned on, and the relief valve is closed to evacuate the enclosed space where the spectrometer 22 is located. After the detection and analysis is completed, the relief valve is opened, and the exhaust valve is closed.

[0040] The detector 23 includes a scintillation counter 2217 for detecting heavy metals and a flow proportional counter 2218 for detecting light elements.

[0041] The temperature control heater 24 is disposed in the sample chamber 211 and includes a heater and a fan, so that the temperature in the sample chamber 211 is always maintained at 35±0.3°C.

[0042] The controller 3 is mainly the center of information processing and conversion, including a mainboard and a CPU. The CPU is installed on the mainboard. The mainboard communicates with the spectrometer unit 2 and the X-ray generator 1 respectively, and the CPU is connected to the computer of the XRF workstation 4. The mainboard is connected to the I / O system, which drives various motors and distinguishes between mainboard signals and noise interference. The mainboard obtains various analog sensor signals from the spectrometer unit 2 for calculating X-ray pulses, driving pulse motors, and controlling the I / O system, the spectrometer unit 2 and the X-ray generator 1.

[0043] The XRF workstation 4 includes a computer with a display, a mouse, and a keyboard. The computer is connected to the CPU via an RS-232C serial port. The computer is also connected to a printer. The computer is installed with analysis software. During the detection and analysis, a series of operations and data processing of the detection process can be performed through the computer interface.

[0044] A method for using an efficient X-ray fluorescence spectrometer comprises the following steps:

[0045] S1: placing the sample box 212 on the turntable 216, which is driven by a motor to rotate and bring the sample box 212 to the injection port;

[0046] S2: The sample box 212 is brought to the sample inlet by the lifter 214 and the sample injector 213, and enters the sample chamber 211 located below the X-ray tube to wait for detection;

[0047] S3: Open the software analysis window on the computer, select the analysis group, select the sample location and sample name, and make notes;

[0048] S4: The sample 5 is tested and analyzed in the sample chamber 211, and the sample box 212 is driven to rotate by the rotary motor during the analysis process;

[0049] S5: Determine the detection and analysis data, confirm the detection result, and the sample box 212 is removed from the sample chamber 211 through the injection port.

[0050] The above description is only a preferred embodiment of the present invention, which does not represent all possible forms of the present invention, and the protection scope of the present invention is not limited to such special statements and embodiments. According to the technical enlightenment disclosed by the present invention, various other modifications and improvements that do not deviate from the essence of the present invention are made, and these modifications and improvements are still within the protection scope of the present invention.

Claims

1. An efficient X-ray fluorescence spectrometer, characterized in that: include: An X-ray generator (1) for generating primary X-rays, a spectroscopic unit (2), a controller (3) and an XRF workstation (4), wherein the spectroscopic unit (2) comprises a sample introduction system (21), a spectroscopic unit (22), a detector (23) and a temperature-controlled heater (24); The sample injection system (21) comprises a sample injector (213), a lifter (214), a rotator (215) and a turntable (216) for transferring a sample box (212) containing a sample (5) to the inside of a sample chamber (211); the lifter (214) is arranged below the rotator (215); the sample injector (213) is connected to the top of the rotator (215); the turntable (216) is connected to the sample injector (213) via a fixing block; and the sample box (212) is arranged on the top of the turntable (216); The sample boxes (212) include a plurality of sample boxes, each of which corresponds to one of the spectrometers (22) and detectors (23) and detects each other independently, and the detector (23) is in communication connection with the controller (3); The sample box (212) comprises a box body (2121), a tray (2123) arranged inside the box body (2121), and a cover plate (2122) arranged on the upper part of the box body (2121); the tray (2123) is rotatably arranged at the bottom of the box body (2121) via a bearing (2124); and a spring (2125) is provided on the tray (2123); The spectrometer (22) comprises a primary slit (2212), an attenuator (2213), a crystal converter (2214), a spectroscopic crystal (2215) and a secondary slit (2216); the primary slit (2212) is connected to the filter (221) inside the sample chamber (211) through a light hole (2211); the attenuator (2213) is arranged at the light output end of the primary slit (2212); the spectroscopic crystal (2215) is mounted on the crystal converter (2214); and the light output end of the secondary slit (2216) is connected to the detector (23).

2. The high-efficiency X-ray fluorescence spectrometer according to claim 1, characterized in that: The XRF workstation (4) comprises a computer with a display, a mouse and a keyboard. The computer is connected to the CPU via an RS-232C serial port and is also connected to a printer.

3. The efficient X-ray fluorescence spectrometer according to claim 2, characterized in that: The controller (3) comprises a mainboard and a CPU, wherein the CPU is mounted on the mainboard, the mainboard is respectively connected to the light splitting unit (2) and the X-ray generator (1) for communication, and the CPU is connected to a computer of an XRF workstation (4).

4. The high-efficiency X-ray fluorescence spectrometer according to claim 3, characterized in that: The X-ray generator (1) comprises an X-ray tube, a high-voltage converter and an X-ray power supply, wherein the high-voltage converter is connected to the X-ray tube and the X-ray power supply respectively, and the X-ray tube is connected to the X-ray power supply via a filament to form a complete circuit.

5. The high-efficiency X-ray fluorescence spectrometer according to claim 4, characterized in that: The detector (23) includes a scintillation counter (2217) for detecting heavy metals and a gas flow proportional counter (2218) for detecting light elements.

6. The high-efficiency X-ray fluorescence spectrometer according to claim 5, characterized in that: The temperature-controlled heater (24) is arranged in the sample chamber (211), and comprises a heater and a fan.

7. The high-efficiency X-ray fluorescence spectrometer according to claim 6, characterized in that: The spectrometer (22) is connected to a vacuum system (25), and the vacuum system (25) comprises a vacuum pump, an air release valve, and an air extraction valve.

8. A method for using the efficient X-ray fluorescence spectrometer according to claim 7, comprising the following steps: S1: placing the sample box (212) on the turntable (216), the turntable (216) is driven by a motor to rotate and bring the sample box (212) to the injection port; S2: The sample box (212) is brought to the sample inlet by the lifter (214) and the sample injector (213), and enters the sample chamber (211) located below the X-ray tube to wait for detection; S3: Open the software analysis window on the computer, select the analysis group, select the sample location and sample name, and make notes; S4: the sample (5) is tested and analyzed in the sample chamber (211), and during the analysis, the sample box (212) is driven to rotate by a rotary motor; S5: Determine the detection and analysis data, confirm the detection results, and the sample box (212) exits the sample chamber (211) from the sample inlet.

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