CN220854711U - Automatic calibration device for online X-ray fluorescence analysis and spent fuel post-treatment system - Google Patents

Abstract

The utility model discloses an online X-ray fluorescence analysis automatic calibration device and a spent fuel post-treatment system. The automatic calibration device comprises a sample bottle, a flow cell and a measuring mechanism, wherein a plurality of sample cells are arranged in the sample bottle in parallel and are used for storing standard sample solutions with different concentrations, the flow cell is communicated with a process pipeline and is used for storing solutions to be measured, a flow cell window is formed in the flow cell, a sample cell window is formed in the sample cell, the measuring mechanism is arranged outside a box chamber and is used for measuring a plurality of first characteristic X rays emitted by elements to be measured in the standard sample solution of the sample cell and a second characteristic X rays emitted by the elements to be measured in the solutions to be measured in the flow cell, and the processing unit is electrically connected with the detector and is used for establishing a standard curve according to energy data of the first characteristic X rays and calculating the concentration of the elements to be measured in the solutions to be measured according to energy data of the second characteristic X rays. The automatic calibration device for the on-line X-ray fluorescence analysis improves the measurement accuracy of the element to be measured.

Description

Automatic calibration device for online X-ray fluorescence analysis and spent fuel post-treatment system

Technical Field

The utility model belongs to the technical field of nuclear industry, and particularly relates to an online X-ray fluorescence analysis automatic calibration device and a spent fuel aftertreatment system comprising the online X-ray fluorescence analysis automatic calibration device.

Background

In the nuclear industry post-treatment process, the concentration or the change trend of the concentration of part of elements in the process feed liquid needs to be mastered in real time, an analysis bypass is generally arranged on a process pipeline, and online and nondestructive analysis is carried out by using analysis equipment. The plutonium concentration is used as an important parameter in the post-treatment process, and the plutonium concentration needs to be monitored in real time at a plurality of process points so as to monitor the loss of the plutonium and provide data support for the whole post-treatment process flow. The online X-ray fluorescence analysis method is combined with domestic and foreign application practice, and is the most efficient and nondestructive online measurement analysis technology for measuring the low-concentration plutonium in the process point. The calibration mode of the instrument is critical to the accuracy and reliability of plutonium concentration data.

Currently, the plutonium element concentration of the process liquid is usually detected in an off-line manner, i.e. the process liquid is separated from the process pipeline and detected in other environments, but because the environment in which the process liquid in the process pipeline is located is greatly different from the environment in which the process liquid is measured in an off-line manner, the plutonium element concentration measured in an off-line manner and the actual plutonium element concentration of the process liquid in the process pipeline may generate a large measurement error.

In addition, the existing online X-ray fluorescence analysis equipment requires workers to enter an orange area environment with strong radioactivity, a radiation shielding box is opened, sample cells with different standard concentrations are manually replaced, and then measurement of drawing efficiency curves is performed. The operation process of the measuring process is complex, the irradiation dose of personnel can be increased, and meanwhile, the repeated positioning accuracy of the position is difficult to ensure in the process of disassembling and reloading the sample cell, so that the calibration deviation is caused, and the measuring result of the plutonium concentration is influenced.

Disclosure of utility model

The utility model aims to solve the technical problems in the prior art and provides an online X-ray fluorescence analysis automatic calibration device and a spent fuel post-processing system comprising the online X-ray fluorescence analysis automatic calibration device, wherein the online X-ray fluorescence analysis automatic calibration device can greatly improve the measurement precision of elements to be measured.

In order to solve the problems, the utility model adopts the following technical scheme:

An automatic calibration device for on-line X-ray fluorescence analysis comprises a sample bottle, a flow cell and a measuring mechanism, wherein a plurality of mutually-independent sample cells are arranged in the sample bottle in parallel and are respectively used for storing the same standard sample solution with different concentrations, the flow cell is communicated with a process pipeline and is used for storing a solution to be measured, the solution to be measured contains components in the standard sample solution, the sample bottle and the flow cell are both arranged in a box chamber and are arranged on a sealing mechanism on the side wall of the box chamber in parallel, a flow cell window is arranged on one side of the flow cell, facing the outside of the box chamber, of each sample cell of the sample bottle, a sample cell window is arranged on one side of each sample cell, facing the outside of the box chamber, of the measuring mechanism is arranged outside the box chamber, the device comprises an X-ray tube, a detector and a processing unit, wherein the X-ray tube is used for generating primary X-rays so as to excite a standard sample solution and elements to be detected in the solution to be detected to generate certain characteristic X-rays, the detector is used for receiving a plurality of first characteristic X-rays emitted by the elements to be detected in the standard sample solution in a plurality of sample cells and a plurality of second characteristic X-rays emitted by the elements to be detected in the solution to be detected in a flow cell, the processing unit is electrically connected with the detector and used for establishing a standard curve according to the energy data of the plurality of first characteristic X-rays received by the detector and calculating the concentration of the elements to be detected in the solution to be detected in the flow cell according to the energy data of the second characteristic X-rays and the standard curve.

Preferably, the measuring mechanism further comprises a driving assembly, a guide rail assembly and a mounting seat, the guide rail assembly comprises a linear guide rail and a sliding block, the linear guide rail is arranged outside the box chamber and is parallel to the side wall of the box chamber, the sliding block is slidably arranged on the linear guide rail, the mounting seat is fixedly arranged on the sliding block, the X-ray tube and the detector are arranged on the mounting seat, and the driving assembly is used for driving the sliding block to move so as to drive the mounting seat to move along the linear guide rail, so that the measuring end of the detector can be aligned with each sample cell window and each flow cell window respectively.

Preferably, a shielding baffle is arranged in the mounting seat, the shielding baffle is made of copper and is used for blocking other high-energy rays generated in the standard sample solution and the solution to be detected, the energy of the high-energy rays is larger than that of the first characteristic X rays and the second characteristic X rays, and the mounting seat is made of organic glass so as to shield the X rays scattered by the X ray tube.

Preferably, the size, thickness, dimension, cross-sectional shape and material of the plurality of sample cell windows are identical, and the size, thickness, dimension, cross-sectional shape and material of the sample cell windows and the flow cell windows are identical.

Preferably, the sample bottle comprises a first shell, a first cover plate, a first pressing plate and a first sealing pad, wherein the first shell and the first cover plate are spliced to form a closed container structure, the first pressing plate is arranged outside the first cover plate and used for pressing the first cover plate, the first sealing pad is arranged between the first shell and the first cover plate, a plurality of first openings are formed in the first pressing plate, and a plurality of sample pool windows are formed in the first cover plate and aligned with the first openings.

Preferably, the flow cell comprises a second shell, a second cover plate, a second pressing plate and a second sealing pad, the second shell and the second cover plate are spliced to form a closed container structure, the second pressing plate is arranged outside the second cover plate and used for pressing the second cover plate, the second sealing pad is arranged between the second shell and the second cover plate, a second opening is formed in the second pressing plate, and the second cover plate is formed in a position aligned with the second opening to form the flow cell window.

Preferably, the sealing mechanism comprises a welding flange, a third cover plate, a third pressing plate and a third sealing gasket, wherein the welding flange is arranged on the side wall of the box chamber, a mounting hole is formed in the middle of the welding flange, the third cover plate is covered outside the welding flange and used for sealing the mounting hole, the third sealing gasket is arranged between the welding flange and the third cover plate, the third pressing plate is pressed outside the third cover plate and used for pressing the third cover plate, a third opening and a fourth opening are formed in the third pressing plate, a first box chamber window is formed in the position, aligned with the third opening, of the third cover plate and a second box chamber window is formed in the position, aligned with the fourth opening, of the welding flange, a first mounting groove and a second mounting groove are formed in one side, facing the box chamber, of the welding flange, the sample bottle is detachably mounted in the first mounting groove, the flow cell is detachably mounted in the second mounting groove, the first box chamber window is aligned with a plurality of sample cell windows, and the second box chamber window is aligned with the second box chamber window.

Preferably, the first cover plate, the second cover plate and the third cover plate are all made of carbon fibers with weak resistance to X-rays.

Preferably, the automatic calibration device for online X-ray fluorescence analysis further comprises a control mechanism, the control mechanism comprises a PLC controller and photoelectric sensors, the photoelectric sensors are provided with a plurality of photoelectric sensors, the photoelectric sensors are respectively electrically connected with the PLC controller, the photoelectric sensors are sequentially arranged below the linear guide rail, the photoelectric sensors are respectively in one-to-one correspondence with the positions of the sample cell windows and the flow cell windows, are used for sensing the mounting seat, and when the mounting seat is sensed, a first signal is sent to the PLC controller, the PLC controller is electrically connected with the driving assembly, and is used for controlling the driving assembly to stop acting after receiving the first signal, and after a set time passes, the PLC controller controls the driving assembly to be started again until the first signal is received again.

The utility model also provides a spent fuel post-treatment system, which comprises post-treatment equipment and the online X-ray fluorescence analysis automatic calibration device, wherein a flow cell of the online X-ray fluorescence analysis automatic calibration device is communicated with a process pipeline of the post-treatment equipment, the element to be detected is plutonium, and the number of sample cells arranged in parallel in the sample bottles is four.

The utility model sets the sample cell and the flow cell to be in the same structure, and sets the sample cell and the flow cell under the same environment, thereby ensuring that no environmental background error is introduced during calibration and measurement, and realizing that only the concentration of the measured substance is used as a single variable. And the position of the standard sample solution is relatively fixed, the sealing performance is good, and the calibration error can not be introduced, so that the measurement calibration precision of the device is higher than the off-line measurement calibration precision, and the measurement precision is greatly improved. In addition, the utility model realizes remote on-line calibration without entering a high-radioactivity place, opening a radiation shielding box and disassembling a measuring mechanism, thereby greatly reducing the workload, improving the operation convenience and effectively reducing the irradiation dose received by personnel in the calibration operation link.

Drawings

FIG. 1 is a schematic diagram showing the structure of the outside of a cabinet of an automatic calibration device for on-line X-ray fluorescence analysis in embodiment 1 of the present utility model;

FIG. 2 is a schematic diagram showing the structure of a chamber of an automatic calibration device for on-line X-ray fluorescence analysis in example 1 of the present utility model;

FIG. 3 is a schematic view showing the structure of a sample bottle in example 1 of the present utility model;

fig. 4 is a schematic structural view of a flange in embodiment 1 of the present utility model.

In the figure: 1-welding flange, 2-sample bottle, 3-flow cell, 4-driving component, 5-X ray tube, 6-shielding baffle, 7-detector, 8-mount, 9-third clamp plate, 10-first box window, 11-box lateral wall, 12-slider, 13-photoelectric sensor, 14-linear guide rail, 15-mounting baseplate, 16-first clamp plate, 17-plug pin, 18-sample cell window, 19-first sealing pad, 20-second box window, 21-third sealing pad.

Detailed Description

The following description of the embodiments of the present utility model will be made more apparent, and the embodiments described in detail, but not necessarily all, in connection with the accompanying drawings. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to fall within the scope of the utility model.

In the description of the present utility model, it should be noted that, the terms "upper" and the like indicate an orientation or a positional relationship based on the orientation or the positional relationship shown in the drawings, and are merely for convenience and simplicity of description, and do not indicate or imply that the apparatus or element in question must be provided with a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present utility model.

In the description of the present utility model, the terms "first," "second," and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.

In the description of the present utility model, it should be noted that, unless explicitly specified and limited otherwise, the terms "connected," "configured," "mounted," "secured," and the like are to be construed broadly and may be either fixedly connected or detachably connected, or integrally connected, for example; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present utility model can be understood by those skilled in the art according to the specific circumstances.

The utility model provides an automatic calibration device for online X-ray fluorescence analysis, which comprises a sample bottle, a flow cell and a measuring mechanism, wherein a plurality of mutually-non-communicated sample cells are arranged in parallel in the sample bottle, are respectively used for storing the same standard sample solution with different concentrations, the flow cell is communicated with a process pipeline and is used for storing a solution to be measured, the solution to be measured contains components in the standard sample solution, the sample bottle and the flow cell are both arranged in a box chamber and are arranged on a sealing mechanism on the side wall of the box chamber in parallel, a flow cell window is arranged on one side of the flow cell facing the outside of the box chamber, a sample cell window is arranged on one side of each sample cell of the sample bottle facing the outside of the box chamber, the measuring mechanism is arranged outside the box chamber, the X-ray tube is used for generating primary X-rays so as to excite a standard sample solution and elements to be measured in the solution to be measured to generate certain characteristic X-rays, the detector is used for receiving a plurality of first characteristic X-rays emitted by the elements to be measured in the standard sample solution in a plurality of sample cells and a plurality of second characteristic X-rays emitted by the elements to be measured in the solution to be measured in the flow-through cell, and the processing unit is electrically connected with the detector and used for establishing a standard curve according to the energy data of the plurality of first characteristic X-rays received by the detector and calculating the concentration of the elements to be measured in the solution to be measured in the flow-through cell according to the energy data of the second characteristic X-rays.

The utility model also provides a spent fuel post-treatment system, which comprises post-treatment equipment and the online X-ray fluorescence analysis automatic calibration device, wherein a flow cell of the online X-ray fluorescence analysis automatic calibration device is communicated with a process pipeline of the post-treatment equipment, the element to be detected is plutonium, and the number of sample cells arranged in parallel in the sample bottles is four.

Example 1

As shown in fig. 1, this embodiment discloses an online automatic calibration device for X-ray fluorescence analysis, which comprises a sample bottle 2, a flow cell 3 and a measuring mechanism, wherein a plurality of sample cells which are not communicated with each other are arranged in parallel in the sample bottle 2, and are respectively used for storing the same standard sample solution with different concentrations, and the flow cell 3 is communicated with a process pipeline and is used for storing a solution to be measured (the solution circulated in the process pipeline). In this embodiment, the solution to be measured and the standard sample solution both contain the same radioactive element, and differ in concentration.

In this embodiment, the sample bottle 2 is made of stainless steel by milling, and each sample cell is identical, and standard sample solutions with different concentrations are placed in each sample cell. The top of each sample cell is provided with a solution injection hole for injecting and sucking out the standard sample solution, and is correspondingly provided with a plug nail 17 with a sealing gasket, the sealing gasket adopts an acid corrosion-resistant and irradiation-resistant sealing material, after the standard sample solution is injected into the sample cell, the solution injection hole of the sample cell is sealed by using the plug nail 17, so that the standard sample solution is prevented from overflowing and leaking, the sealing performance of the sample cell is ensured, and the storage requirement of the standard sample solution is met.

The sample bottle 2 and the flow cell 3 are both arranged in a box and are arranged on a sealing mechanism of the side wall 11 of the box in parallel, the box has a shielding effect, the box is provided with a personnel operation space, and the outside of the box is provided with a radioactive environment. The flow cell 3 is provided with a flow cell window on the side facing the outside of the tank, and each sample cell of the sample bottle 2 is provided with a sample cell window 18 on the side facing the outside of the tank, and the measuring mechanism is arranged outside the tank.

In this embodiment, the element to be measured is plutonium element in the standard sample solution and the solution to be measured. The measuring mechanism comprises an X-ray tube 5, a detector 7 and a processing unit, wherein the X-ray tube 5 is used for generating primary X-rays so as to excite plutonium elements in a standard sample solution and a solution to be measured to generate characteristic X-rays, the detector 7 is used for receiving a plurality of first characteristic X-rays emitted by the plutonium elements in the standard sample solution in a plurality of sample cells and a plurality of second characteristic X-rays emitted by the plutonium elements in the solution to be measured in the flow cell 3, the processing unit is electrically connected with the detector 7, the energy data of the plurality of first characteristic X-rays measured by the detector 7 are different due to the fact that the concentration of the plutonium elements in the plurality of standard sample solutions is different, the processing unit establishes a standard curve according to the energy data of the plurality of first characteristic X-rays received by the detector 7, and calculates the concentration of the plutonium elements in the solution to be measured in the flow cell 3 according to the energy data of the second characteristic X-rays combined with the standard curve.

In this embodiment, the processing unit is formed by installing dmsas.v31 analysis software of company Wei Feng of shanxi on a computer, the X-ray tube is a KYW700 type X-ray tube of company Yiwei of the family, and the detector is a FAST123 SDD type detector of company AMETEK.

Specifically, the standard curve is established as follows:

And respectively placing standard sample solutions with different concentrations in each sample cell, then starting a measuring mechanism to measure the characteristic X-ray energy of plutonium elements in the standard sample solutions in each sample cell, then transmitting the characteristic X-ray energy data of the plutonium elements measured by the measuring mechanism to analysis software, recording the total energy peak net count rate of the plutonium element characteristic X-rays by the analysis software, and establishing a curve of concentration and count rate, wherein the curve is a standard curve. When the sample to be measured in the flow cell is measured, the counting rate of the solution to be measured is converted into a concentration value through a standard curve.

In this embodiment, the measuring mechanism further includes a driving component 4, a guide rail component and a mounting seat 8, the guide rail component includes a linear guide rail 14 and a sliding block 12, the linear guide rail 14 is disposed outside the box and is parallel to the side wall 11 of the box, the sliding block 12 is slidingly disposed on the linear guide rail 14, the mounting seat 8 is fixedly disposed on the sliding block 12, the X-ray tube 5 and the detector 7 are disposed on the mounting seat 8, and the driving component 4 is used for driving the sliding block 12 to move so as to drive the mounting seat 8 to move along the linear guide rail 14, so that the measuring end of the detector 7 can be aligned with each sample cell window 18 and each flow cell window respectively to measure the first characteristic X-rays emitted by plutonium elements in standard sample solutions in each sample cell and the second characteristic X-rays emitted by plutonium elements in solutions to be measured in the flow cell 3 respectively. Due to the parallel arrangement of the linear guide rail 14 and the side wall 11 of the box chamber, when the mounting seat 8 moves along the linear guide rail 14, the vertical distance between the sample cell window 18 and the flow cell window and the detector 7 can be effectively ensured to be the same.

Specifically, the driving assembly 4 employs a servo motor.

Optionally, a shielding baffle 6 is arranged in the mounting seat 8, and the shielding baffle 6 is made of copper and is used for blocking other high-energy rays generated in the standard sample solution and the solution to be tested, wherein the energy of the high-energy rays is larger than that of the first characteristic X rays and the second characteristic X rays. Specifically, the high-energy ray is greater than the characteristic X-ray energy (14.279 keV) of plutonium element, and the mount 8 is made of organic glass to shield the X-rays scattered by the X-ray tube 5.

In this embodiment, in order to ensure that the standard sample solution and the solution to be measured can only use the difference in concentration of plutonium element as a single variable, the sample bottle 2 and the flow cell 3 are disposed under the same environment, and each of the sample cell windows 18 and the flow cell windows are disposed in the same structure, that is, the size, thickness, size, cross-sectional shape, and material of the plurality of sample cell windows 18 are identical, the size, thickness, size, cross-sectional shape, and material of the sample cell windows 18 and the flow cell windows are identical, thereby improving measurement accuracy and avoiding the measurement result from being affected by other factors.

As shown in fig. 3, the sample bottle 2 includes a first casing, a first cover plate, a first pressing plate 16, and a first sealing gasket 19, where the first casing is a semi-enclosed structure, one end of the first casing is an opening, the first cover plate is a flat plate structure, the first cover plate is installed at the open end of the first casing, and the first cover plate are spliced to form a closed container structure. The first clamp plate 16 is installed outside first apron through the screw for compress tightly first apron, and first sealed pad 19 fills up and locates between first casing and the first apron, in order to increase the leakproofness between first casing and the first apron, has seted up a plurality of first openings on the first clamp plate 16, and the position of aligning with a plurality of first openings on the first apron constitutes a plurality of sample cell windows 18, and sample cell window 18 adopts and blocks weaker material to the X ray to make, so that the characteristic X ray that plutonium element sent can get into detector 7 smoothly.

In this embodiment, the flow cell 3 has a similar structure to that of the sample bottle 2, and includes a second housing, a second cover plate, a second pressure plate, and a second gasket. The second shell is of a semi-surrounding structure, one end of the second shell is of an opening, the two cover plates are of a flat plate structure, the second cover plates are arranged at the opening end of the second shell, and the two cover plates are spliced to form a closed container structure. The second clamp plate passes through the screw and installs outside the second apron for compress tightly the second apron, and the second is sealed fills up and locate between second casing and the second apron, with the leakproofness between increase second casing and the second apron, has seted up the second opening on the second clamp plate, constitutes the flow cell window with the position of second opening alignment on the second apron. The flow cell window is made of a material that is weak against X-rays so that characteristic X-rays emitted by the plutonium element can enter the detector 7 smoothly.

As shown in fig. 1 and 4, the sealing mechanism of the side wall 11 of the box chamber comprises a welding flange 1, a third cover plate, a third pressing plate 9 and a third sealing gasket 21. The welding flange 1 is welded on the side wall 11 of the box chamber in a sealing way, a stainless steel material is adopted, a mounting hole is formed in the middle of the welding flange, a third cover plate cover is arranged outside the welding flange 1 and used for sealing the mounting hole, a third sealing gasket 21 is arranged between the welding flange 1 and the third cover plate in a cushioning way, a third pressing plate 9 is arranged outside the third cover plate through a screw and used for pressing the third cover plate, the third sealing gasket 21 is pressed through the pressing force of the screw, and therefore an airtight structure is formed, and the isolation of the atmosphere inside the box chamber and the atmosphere outside the box chamber at the mounting hole of the welding flange 1 is guaranteed. The third pressing plate 9 is provided with a third opening and a fourth opening, the position of the third cover plate aligned with the third opening forms a first box chamber window 10, and the position of the third cover plate aligned with the fourth opening forms a second box chamber window 20.

As shown in fig. 2, a first mounting groove and a second mounting groove are formed in one side, facing the inside of the box, of the welding flange 1, a first pressing component and a second pressing component are arranged, the sample bottle 2 is detachably mounted in the first mounting groove, the flow cell 3 is detachably mounted in the second mounting groove, and when the sample bottle 2 is mounted in the first mounting groove, the first pressing component presses the sample bottle 2, so that the plane of the first pressing plate 16 can be pressed and attached with the inner side face of the first box window 10. When the flow cell 3 is installed in the second installation groove, the second pressing component presses the flow cell 3 to ensure that the plane of the second pressing plate can be pressed and attached with the inner side surface of the second box window 20 after the flow cell 3 is installed in the second installation groove, so that the relative position of the sample bottle 2 and the flow cell 3 is fixed. If the standard sample solution precipitates in the sample cell, the sample bottle 2 can be quickly detached in the box manually and uniformly shaken.

The first chamber window 10 is aligned with a plurality of sample cell windows 18 and the second chamber window 20 is aligned with a flow cell window. The first chamber window 10 has a rectangular structure, the length dimension of the first chamber window can cover the plurality of sample cell windows 18, the second chamber window 20 has a square structure with the same size as the flow cell windows, and the third cover plate is made of a material with weaker X-ray blocking, so that first characteristic X-rays emitted by plutonium elements of a standard sample solution can sequentially pass through the sample cell windows 18 and the first chamber window 10 to enter the detector 7, and second characteristic X-rays emitted by plutonium elements of a solution to be detected can sequentially pass through the flow cell windows and the second chamber window 20 to enter the detector 7.

Specifically, the first cover plate, the second cover plate and the third cover plate are all made of carbon fibers with weaker X-ray resistance. The first sealing gasket 19, the second sealing gasket and the third sealing gasket 21 are all rubber gaskets resistant to acid corrosion and irradiation.

In this embodiment, the automatic calibration device for online X-ray fluorescence analysis further includes a control mechanism, the control mechanism includes a PLC controller, a plurality of photoelectric sensors 13, the plurality of photoelectric sensors 13 are respectively electrically connected with the PLC controller, the plurality of photoelectric sensors 13 are sequentially disposed below the linear guide rail 14, and the plurality of photoelectric sensors 13 are respectively in one-to-one correspondence with the positions of the plurality of sample cell windows 18 and the flow cell windows, and are used for sensing the mounting seat 8, and when the mounting seat 8 is sensed, a first signal is sent to the PLC controller, the PLC controller is electrically connected with the driving assembly 4, and is used for controlling the driving assembly 4 to stop moving after receiving the first signal, so that the detector 7 on the mounting seat 8 stops at a position aligned with the sample cell window 18 or the flow cell window, thereby measuring the same, and after a set time (after the measurement is completed), the PLC controller again controls the driving assembly 4 to start again until the first signal is received again, thereby measuring the next standard sample solution or the solution to be measured.

Optionally, a mounting bottom plate 15 is further disposed below the linear guide rail 14, the mounting bottom plate 15 is fixedly installed on the ground outside the box, the length direction of the mounting bottom plate 15 is parallel to the side wall 11 of the box, and the linear guide rail 14 and the photoelectric sensor 13 are both installed on the mounting bottom plate 15. The mounting bottom plate 15 is provided with a fine adjustment structure, the sliding block 12 is connected with the linear guide rail 14 through the fine adjustment structure, and the moving direction of the sliding block 12 can be adjusted through the fine adjustment structure, so that the moving direction of the sliding block is always kept parallel to the side wall 11 of the box chamber, and the vertical distance between the measuring mechanism and the sample bottle 2 and the vertical distance between the measuring mechanism and the flow cell 3 are the same.

The PLC controller and the photoelectric sensor 13 in the embodiment ensure that the movement of the measuring mechanism has higher positioning precision, and ensure the repeated positioning precision of the sliding block 12 and the measuring mechanism returning to the measuring position.

The working process of the automatic calibration device for online X-ray fluorescence analysis is as follows:

According to the measuring range, standard sample solutions with different concentrations are injected into each sample cell, and a plug pin 17 is arranged in a solution injection hole at the top of the sample cell so as to seal the sample cell;

The sample bottle 2 is integrally arranged in the first mounting groove and is compressed by the first compressing assembly, and the end face of the first pressing plate 16 is attached and compressed with the inner side face of the first box window 10;

The flow cell 3 is arranged in the second installation groove and is compressed by the second compression assembly, and the end face of the second pressing plate is bonded and compressed with the inner side face of the second box window 20;

Then, the process line is connected to the flow cell 3;

The initial position of the measuring mechanism is aligned with the window of the flow cell so as to measure the energy of the second characteristic X-ray emitted by plutonium element of the solution to be measured in the flow cell 3;

When the measuring calibration is carried out, the PLC controller controls the driving assembly 4 to start, the driving assembly 4 drives the sliding block 12 to move so as to drive the measuring mechanism to move along the linear guide rail 14, when the photoelectric sensor 13 corresponding to the sample cell window 18 at the tail end senses the measuring mechanism, a first signal is sent to the PLC controller, the PLC controller controls the driving assembly 4 to stop acting, at the moment, the measuring end of the detector 7 in the measuring mechanism is aligned with the sample cell window 18 at the tail end, so that the first characteristic X-ray emitted by the standard sample solution in the sample cell is measured, and after a set time, the PLC controller controls the driving assembly 4 to start so as to continuously drive the measuring mechanism to move along the linear guide rail 14;

The PLC controller controls the driving component 4 to drive the measuring mechanism to sequentially measure first characteristic X-rays of plutonium elements in a plurality of sample cells in the same measuring mode as that of the sample cells at the tail end, so that first characteristic X-ray energy data of the plutonium elements of standard sample solutions in all the sample cells are obtained;

The processing unit receives the measurement data of the detector and establishes a standard curve from the energy data of the plurality of first characteristic X-rays received by the detector 7 and calculates the concentration of plutonium in the solution to be measured in the flow-through cell 3 from the energy data of the second characteristic X-rays.

Of course, the initial position of the measuring means may also be set in alignment with the cell window 18 at the head end, so that all cells are measured first and then the flow cell 3.

The utility model sets the sample cell and the flow cell 3 to be in the same structure, and sets the sample cell and the flow cell under the same environment, thereby ensuring that no environmental background error is introduced during calibration and measurement, and realizing that the concentration of the measured substance is only used as a single variable. And the position of the standard sample solution is relatively fixed, the sealing performance is good, and the calibration error can not be introduced, so that the measurement calibration precision of the device is higher than the off-line measurement calibration precision, and the measurement precision is greatly improved. In addition, the utility model can realize remote on-line calibration without entering a high-radioactivity place, opening a radiation shielding box chamber and disassembling a measuring mechanism, thereby greatly reducing the workload, improving the operation convenience and effectively reducing the irradiation dose received by personnel in the calibration operation link.

Example 2

The embodiment 2 discloses a spent fuel aftertreatment system, which comprises aftertreatment equipment, and further comprises an on-line X-ray fluorescence analysis automatic calibration device in the embodiment 1, wherein a flow cell 3 of the on-line X-ray fluorescence analysis automatic calibration device is communicated with a process pipeline of the aftertreatment equipment, the element to be detected is plutonium, and the number of sample cells arranged in parallel in a sample bottle 2 is four.

In this embodiment, the measuring means is used to measure the characteristic X-ray energy of plutonium elements in the standard sample solution and the solution to be measured.

Specifically, four sample cells are arranged in the sample bottle 2, the four sample cells are uniformly arranged at intervals, and the size and the shape of each sample cell are the same. Correspondingly, the photoelectric sensor 13 is provided with five photoelectric sensors, four photoelectric sensors respectively correspond to four sample cells, the other photoelectric sensor corresponds to the flow cell 3, when the measuring mechanism is in an initial position, the photoelectric sensor is aligned to a window of the flow cell to measure energy of second characteristic X rays emitted by plutonium elements of a solution to be measured in the flow cell 3, when measurement calibration is carried out, the PLC controller controls the driving assembly 4 to start, and the driving assembly 4 drives the sliding block 12 to move so as to drive the measuring mechanism to move along the linear guide rail 14, so that energy of first characteristic X rays emitted by standard sample solutions in the four sample cells is measured sequentially.

The processing unit receives the measurement data of the detector and establishes a standard curve from the energy data of the four first characteristic X-rays received by the detector 7 and calculates the concentration of plutonium in the solution to be measured in the flow cell 3 from the energy data of the second characteristic X-rays and the established standard curve.

According to the spent fuel aftertreatment system in the embodiment, the plutonium element concentration of the solution to be measured in the calibration process pipeline can be automatically measured according to the measurement data in the standard sample solution, the influence of other factors can be eliminated in the measurement process, only the difference of the plutonium element concentrations of the standard sample solution and the plutonium element concentration of the solution to be measured is ensured, and the measurement accuracy is greatly improved.

It is to be understood that the above embodiments are merely illustrative of the application of the principles of the present utility model, but not in limitation thereof. Various modifications and improvements may be made by those skilled in the art without departing from the spirit and substance of the utility model, and are also considered to be within the scope of the utility model.

Claims (10)

1. An automatic calibration device for online X-ray fluorescence analysis is characterized by comprising a sample bottle (2), a flow cell (3) and a measuring mechanism,

A plurality of sample tanks which are not communicated with each other are arranged in parallel in the sample bottle (2) and are respectively used for storing the same standard sample solution with different concentrations,

The flow cell (3) is communicated with a process pipeline and is used for storing a solution to be detected, the solution to be detected contains components in the standard sample solution, the sample bottle (2) and the flow cell (3) are both positioned in a box chamber and are arranged on a sealing mechanism of a side wall (11) of the box chamber in parallel,

A flow cell window is arranged on one side of the flow cell (3) facing the outside of the box, a sample cell window (18) is arranged on one side of each sample cell of the sample bottle (2) facing the outside of the box,

The measuring mechanism is arranged outside the box chamber and comprises an X-ray tube (5), a detector (7) and a processing unit,

The X-ray tube (5) is used for generating primary X-rays so as to excite the elements to be tested in the standard sample solution and the solution to be tested to generate characteristic X-rays,

The detector (7) is used for receiving a plurality of first characteristic X-rays emitted by the elements to be detected in the standard sample solution in the sample cells and a plurality of second characteristic X-rays emitted by the elements to be detected in the solution to be detected in the flow cell (3),

The processing unit is electrically connected with the detector (7) and is used for establishing a standard curve according to the energy data of a plurality of first characteristic X rays received by the detector (7) and calculating the concentration of an element to be detected in the solution to be detected in the flow cell (3) according to the energy data of the second characteristic X rays and the standard curve.

2. The automatic calibration device for on-line X-ray fluorescence analysis according to claim 1, wherein the measuring mechanism further comprises a driving assembly (4), a guide rail assembly and a mounting seat (8),

The guide rail component comprises a linear guide rail (14) and a sliding block (12), wherein the linear guide rail (14) is arranged outside the box chamber and is parallel to the side wall (11) of the box chamber, the sliding block (12) is arranged on the linear guide rail (14) in a sliding way,

The mounting seat (8) is fixedly arranged on the sliding block (12), the X-ray tube (5) and the detector (7) are arranged on the mounting seat (8),

The driving assembly (4) is used for driving the sliding block (12) to move so as to drive the mounting seat (8) to move along the linear guide rail (14), so that the measuring end of the detector (7) can be aligned with each sample cell window (18) and each flow cell window respectively.

3. The automatic calibration device for on-line X-ray fluorescence analysis according to claim 2, wherein a shielding baffle (6) is arranged in the mounting seat (8), the shielding baffle (6) is made of copper and is used for blocking other high-energy rays generated in a standard sample solution and a solution to be tested, the energy of the high-energy rays is larger than that of the first characteristic X-rays and the second characteristic X-rays,

The mounting seat (8) is made of organic glass so as to shield X-rays scattered by the X-ray tube (5).

4. The automatic calibration device for on-line X-ray fluorescence analysis according to claim 1, wherein the plurality of sample cell windows (18) are identical in size, thickness, dimension, cross-sectional shape, material,

The sample cell window (18) and the flow cell window are identical in size, thickness, size, cross-sectional shape, and material.

5. The automatic calibration device for on-line X-ray fluorescence analysis according to claim 1, wherein the sample bottle (2) comprises a first housing, a first cover plate, a first pressure plate (16), a first sealing gasket (19),

The first shell and the first cover plate are spliced to form a closed container structure, the first pressing plate (16) is arranged outside the first cover plate in a covering way and is used for pressing the first cover plate,

The first sealing gasket (19) is arranged between the first shell and the first cover plate in a cushioning mode, a plurality of first openings are formed in the first pressing plate (16), and a plurality of sample pool windows (18) are formed in the first cover plate at positions aligned with the first openings.

6. The automatic calibration device for on-line X-ray fluorescence analysis according to claim 5, wherein the flow cell (3) comprises a second housing, a second cover plate, a second pressure plate, a second gasket,

The second shell and the second cover plate are spliced to form a closed container structure, the second pressing plate cover is arranged outside the second cover plate and used for pressing the second cover plate,

The second sealing gasket is arranged between the second shell and the second cover plate,

And a second opening is formed in the second pressing plate, and the position, aligned with the second opening, of the second cover plate forms the flow cell window.

7. The automatic calibration device for on-line X-ray fluorescence analysis according to claim 6, wherein the sealing mechanism comprises a welding flange (1), a third cover plate, a third pressing plate (9) and a third sealing gasket (21),

The welding flange (1) is arranged on the side wall (11) of the box chamber, the middle part of the welding flange is provided with a mounting hole, the third cover plate is covered outside the welding flange (1) and is used for sealing the mounting hole,

The third sealing gasket (21) is arranged between the welding flange (1) and the third cover plate in a cushioning way,

The third pressing plate (9) is pressed outside the third cover plate and used for pressing the third cover plate, a third opening and a fourth opening are formed in the third pressing plate (9), a first box window (10) is formed in the position, aligned with the third opening, of the third cover plate, a second box window (20) is formed in the position, aligned with the fourth opening, of the third cover plate,

A first mounting groove and a second mounting groove are formed in one side, facing the inside of the box chamber, of the welding flange (1), the sample bottle (2) is detachably mounted in the first mounting groove, the flow cell (3) is detachably mounted in the second mounting groove,

The first compartment window (10) is aligned with a plurality of sample cell windows (18) and the second compartment window (20) is aligned with a flow cell window.

8. The on-line X-ray fluorescence analysis automatic calibration device of claim 7, wherein the first cover plate, the second cover plate, and the third cover plate are all made of carbon fibers that are weak to X-rays.

9. An on-line X-ray fluorescence analysis automatic calibration device according to claim 2 or 3, further comprising a control mechanism comprising a PLC controller, a photosensor (13),

The photoelectric sensors (13) are provided with a plurality of photoelectric sensors (13) which are respectively and electrically connected with the PLC, the photoelectric sensors (13) are sequentially arranged below the linear guide rail (14), the photoelectric sensors (13) are respectively and one-to-one corresponding to the positions of the sample cell windows (18) and the flow cell windows, are used for sensing the mounting seat (8) and sending a first signal to the PLC when the mounting seat (8) is sensed,

The PLC controller is electrically connected with the driving assembly (4) and is used for controlling the driving assembly (4) to stop after receiving the first signal, and controlling the driving assembly (4) to start again after the set time passes until receiving the first signal again.

10. A spent fuel aftertreatment system, comprising aftertreatment equipment, and further comprising the on-line X-ray fluorescence analysis automatic calibration device according to any one of claims 1-9,

The flow cell (3) of the automatic calibration device for the online X-ray fluorescence analysis is communicated with a process pipeline of the post-treatment equipment,

The element to be detected is plutonium, and the number of the sample cells arranged in parallel in the sample bottle (2) is four.