Fluorescent x-ray analysis device, information storage medium, and program
Patent Information
- Application Number
- PCT/JP2024/031412
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2023-09-01
- Filing Date
- 2024-08-30
- Publication Date
- 2025-03-06
Smart Images

Figure JP2024031412_06032025_PF_FP_ABST
Abstract
Description
X-ray fluorescence analyzer, information storage medium, and program
[0001] The present invention relates to an X-ray fluorescence analyzer, an information storage medium, and a program.
[0002] X-ray fluorescence analyzers are known as devices for analyzing elements contained in a sample. X-ray fluorescence analyzers irradiate a sample with primary X-rays and perform analysis based on the intensity and energy of fluorescent X-rays emitted from the sample. A simple X-ray fluorescence analyzer is also known, which has a structure in which the sample chamber and the irradiation chamber are separated by a partition membrane so that the sample can be easily replaced while maintaining the irradiation chamber in a helium atmosphere (see Patent Document 1).
[0003] International Publication No. 2004-088296
[0004] For simple measurements, it is desirable for the sample chamber to be at atmospheric pressure. Helium or air is typically used as the gas filled in the sample chamber. Helium has low X-ray absorption, allowing for sensitive measurement of low-energy fluorescent X-rays emitted by light elements, but it is expensive to distribute. Air, on the other hand, contains oxygen, so ozone is generated in the sample chamber by X-rays during measurement. Ozone deteriorates the partition film, which can cause damage to the film. If the partition film is damaged, the inside of the instrument may become contaminated with the sample, etc.
[0005] The present disclosure has been made in consideration of the above-mentioned problems, and its purpose is to provide a fluorescent X-ray analysis apparatus that can prevent damage to the partition film and damage to or contamination of components placed in the irradiation chamber.
[0006] (1) An X-ray fluorescence analysis apparatus according to one aspect of the present disclosure is an X-ray fluorescence analysis apparatus having: a sample chamber in which a sample is placed; an irradiation chamber separated from the sample chamber by a partition wall including a partition wall film that transmits X-rays in part; and an information processing device in which an X-ray source is placed, the irradiation chamber emitting X-rays to the sample through the partition wall film; and the information processing device is characterized in that the information processing device has an irradiation time acquisition unit that acquires an irradiation time for which X-rays are irradiated onto the partition wall film; and a control unit that performs protection control to protect the partition wall film from X-ray irradiation based on the irradiation time acquired by the irradiation time acquisition unit.
[0007] (2) In another aspect of the X-ray fluorescence analysis apparatus of the present disclosure, the information processing device has a replacement information acquisition unit that acquires replacement information indicating that the partition film has been replaced, the irradiation time acquisition unit measures a cumulative irradiation time, which is the cumulative time that X-rays have been irradiated onto the partition film since the replacement information was acquired, and the control unit performs the protection control when the cumulative irradiation time exceeds a first set value.
[0008] (3) In another aspect of the X-ray fluorescence analyzer according to the present disclosure, the irradiation time acquisition unit measures a continuous irradiation time, which is the time during which X-rays are continuously irradiated onto the partition film after irradiation of the partition film with X-rays has started, and the control unit performs the protection control when the continuous irradiation time exceeds a second set value.
[0009] (4) In another aspect of the X-ray fluorescence analysis apparatus of the present disclosure, the information processing device includes a measurement condition acquisition unit that acquires measurement conditions including a measurement time, and the irradiation time acquisition unit calculates a predicted continuous irradiation time as the time during which X-rays are irradiated onto the partition film through a measurement performed according to the measurement conditions based on the measurement time included in the acquired measurement conditions, and the control unit performs the protection control based on the predicted continuous irradiation time.
[0010] (5) In another aspect of the X-ray fluorescence analysis apparatus of the present disclosure, the information processing device further includes a replacement information acquisition unit that acquires replacement information indicating that the partition film has been replaced, and a memory unit that stores a cumulative irradiation time, which is the cumulative time over which X-rays have been irradiated onto the partition film since the replacement information was acquired, wherein the irradiation time acquisition unit adds the predicted continuous irradiation time to the cumulative irradiation time stored in the memory unit to calculate the predicted cumulative irradiation time, and the control unit performs the protection control when the predicted cumulative irradiation time exceeds a first set value.
[0011] (6) In another aspect of the X-ray fluorescence analyzer of the present disclosure, the control unit performs the protection control when the predicted continuous irradiation time exceeds a second set value.
[0012] (7) In a fluorescent X-ray analyzer according to another aspect of the present disclosure, the protection control is a control that does not allow measurement to be started.
[0013] (8) Another aspect of the X-ray fluorescence analysis apparatus according to the present disclosure further includes a shutter that, when closed, isolates the sample chamber from the irradiation chamber and blocks X-rays, and the irradiation time acquisition unit measures the time during which the X-ray source emits X-rays and the shutter is open as the irradiation time.
[0014] (9) In a fluorescent X-ray analyzer according to another aspect of the present disclosure, the protection control is a control to close the shutter.
[0015] (10) In a fluorescent X-ray analyzer according to another aspect of the present disclosure, the protection control is a control that causes the X-ray source to stop emitting X-rays.
[0016] (11) In another aspect of the X-ray fluorescence analysis apparatus of the present disclosure, the information processing device has a display unit that displays information based on control by the control unit, and the protection control is control that causes the display unit to display information indicating that the partition film may be damaged.
[0017] (12) In another aspect of the X-ray fluorescence analyzer of the present disclosure, the replacement information includes information representing the material and / or thickness of the replaced partition film, and the first set value and / or the second set value are set based on the information representing the material and / or thickness.
[0018] (13) In the fluorescent X-ray analyzer according to another aspect of the present disclosure, the display unit further displays the cumulative irradiation time and / or the continuous irradiation time.
[0019] (14) Another aspect of the present disclosure provides an information storage medium that is a non-transitory computer-readable information storage medium that stores a program executed by a computer used in an X-ray fluorescence analyzer, the X-ray fluorescence analyzer including: a sample chamber in which a sample is placed; an irradiation chamber that is separated from the sample chamber by a partition that includes an X-ray-transmitting partition film in part, and in which an X-ray source is placed that emits X-rays to the sample through the partition film; and the computer, wherein the program causes the computer to execute an irradiation time acquisition step that acquires an irradiation time for irradiating the partition film with X-rays; and a protection control step that performs protection control to protect the partition film from X-ray irradiation based on the irradiation time acquired in the irradiation time acquisition step.
[0020] (15) Another aspect of the present disclosure provides a program executed by a computer used in an X-ray fluorescence analyzer, the program comprising: a sample chamber in which a sample is placed; an irradiation chamber separated from the sample chamber by a partition wall including a partition wall film that transmits X-rays in part; and the computer; the program causing the computer to execute an irradiation time acquisition step of acquiring an irradiation time for irradiating the partition wall film with X-rays; and a protection control step of performing protection control to protect the partition wall film from X-ray irradiation based on the irradiation time acquired in the irradiation time acquisition step.
[0021] According to the present disclosure, damage to the partition film and damage and contamination of components placed in the irradiation chamber can be prevented.
[0022] FIG. 1 is a diagram illustrating an outline of an X-ray fluorescence analyzer. FIG. 2 is a diagram illustrating the hardware configuration of an information processing device. FIG. 3 is a diagram illustrating an example of an image representing the state of an X-ray fluorescence analyzer. FIG. 4 is a diagram illustrating an example of an error image. FIG. 5 is a diagram illustrating functional blocks of an information processing device. FIG. 6 is a diagram illustrating an example of a partition film replacement image. FIG. 7 is an example of a flowchart executed by an X-ray fluorescence analyzer during measurement. FIG. 8 is an example of a flowchart for determining whether a measurement recipe includes an executable measurement condition. FIG. 9 is a flowchart for measuring irradiation time. FIG. 10 is a flowchart illustrating first protection control. FIG. 11 is a flowchart executed when replacing a partition film. FIG. 12 is a flowchart illustrating second protection control.
[0023] Preferred embodiments (hereinafter referred to as "embodiments") for carrying out the present invention will be described below with reference to the drawings. FIG. 1 is a schematic diagram of an X-ray fluorescence analyzer 100. As shown in FIG. 1, the X-ray fluorescence analyzer 100 includes a sample chamber 102, an irradiation chamber 104, a partition wall 106, a shutter 108, a counter 110, and an information processing device 112. The sample chamber 102 and the irradiation chamber 104 are separated by a partition wall including the partition wall 106 to prevent gas from moving between them. The partition wall 106 has an opening that allows X-rays to pass from the irradiation chamber 104 to the sample chamber 102.
[0024] The irradiation chamber 104 is separated from the sample chamber 102 by a partition wall that includes a partition film 114 that transmits X-rays. Specifically, for example, the irradiation chamber 104 is in a vacuum environment and has an X-ray source 116, a spectroscopic element 118, and a detector 120 disposed therein. The X-ray source 116 emits X-rays toward the sample through the partition film 114. Fluorescent X-rays are emitted from the sample irradiated with the X-rays. The spectroscopic element 118 separates the fluorescent X-rays of a predetermined wavelength emitted from the sample. The detector 120 is disposed at a position where the fluorescent X-rays dispersed by the spectroscopic element 118 are incident. The detector 120 detects the fluorescent X-rays and outputs a pulse signal. The detector 120 is, for example, a proportional counter. The counter 110 counts the pulse signals output from the detector 120 and obtains the intensity of the fluorescent X-rays. Data representing the intensity of the fluorescent X-rays counted by the counter 110 is transmitted to an information processing device 112 .
[0025] The spectroscopic element 118 and the detector 120 may be provided for each element to be analyzed, or a single set of spectroscopic element 118 and detector 120 may be configured to rotate. When a single set of spectroscopic element 118 and detector 120 is rotated, a mechanism (goniometer) for rotating the spectroscopic element 118 and detector 120 is disposed in the irradiation chamber 104. The X-ray fluorescence analyzer 100 shown in FIG. 1 is a wavelength-dispersive type, but it may also be an energy-dispersive type. The interior of the irradiation chamber 104 is preferably a vacuum so that the X-rays emitted by the X-ray source 116 are not absorbed. However, the interior of the irradiation chamber 104 may be an air or helium atmosphere depending on the element to be analyzed.
[0026] A sample cell 122 is placed in the sample chamber 102. Specifically, a sample stage 124 is provided in the sample chamber 102, and the sample cell 122 is placed on the sample stage 124. The interior of the sample chamber 102 is filled with air or helium. The sample may be a liquid or a solid (including powder), but the following description will focus on the case where the sample is a liquid. The liquid sample is placed in the sample cell 122. The sample cell 122 is cylindrical, and a sample-holding film is attached to cover the bottom. The liquid sample is placed on the sample-holding film. The top of the sample cell 122 may be sealed with another film to prevent the sample from spilling. The interior of the sample chamber 102 may be filled with air, and helium may be flowed between the sample-holding film and the partition film 114. If the sample is a solid, the interior of the sample chamber 102 may be evacuated.
[0027] As an example, the sample stage 124 includes a window frame holding member, a window frame member 126, a film support member 128, and a cover member 130. The window frame holding member has an opening that allows X-rays to pass from the irradiation chamber 104 to the sample chamber 102, and is disposed in the sample chamber 102 to support the outer edge of the film support member 128 and the outer edge of the window frame member 126 from below. Specifically, the window frame holding member has a lower holding member 132 and an upper holding member 134. The lower holding member 132 and the upper holding member 134 have openings that allow X-rays to pass from the irradiation chamber 104 to the sample chamber 102.
[0028] The lower holding member 132 is a member that is placed in contact with the partition wall 106. When viewed from the top and bottom, the lower holding member 132 has a substantially circular outer edge, and has a circular opening at a position corresponding to the opening provided in the partition wall 106. The lower holding member 132 has a step that corresponds to the outer edge of the film support member 128. The film support member 128 is placed so that its outer edge is positioned at the step of the lower holding member 132. In this way, the lower holding member 132 supports the outer edge of the film support member 128. The lower holding member 132 also supports the window frame member 126 that is placed above the film support member 128.
[0029] The upper holding member 134 is a member that is placed on top of and in contact with the lower holding member 132. When viewed from the top and bottom, the upper holding member 134 has a substantially circular outer edge and a circular opening with a larger diameter that is centered at the same position as the opening provided in the lower holding member 132. The upper holding member 134 has an O-ring at a position where it comes into contact with the lower holding member 132. The upper holding member 134 supports the window frame member 126 together with the lower holding member 132.
[0030] The window frame member 126 holds the partition wall film 114, which is made of a material that transmits X-rays and constitutes part of the partition wall, and is disposed within an opening provided in the partition wall 106. Specifically, the window frame member 126 holds the partition wall film 114, which is made of a material that transmits X-rays and constitutes part of the partition wall, and is disposed within the opening of the window frame holding member. The window frame member 126 has an inner film holding member and an outer film holding member, each of which is annular. The window frame member 126 is disposed within the opening of the window frame holding member with the partition wall film 114 sandwiched between the inner film holding member and the outer film holding member. The partition wall film 114 in the opening constitutes part of the partition wall.
[0031] The film support member 128 has an opening that allows X-rays to pass through, and is disposed adjacent to the partition film 114 on the irradiation chamber 104 side to support the partition film 114 from the irradiation chamber 104 side.
[0032] The cover member 130 seals the space in which the sample cell 122 is placed. Specifically, as shown in FIG. 1 , the cover member 130 has a shape that covers the space in which the sample cell 122 is placed, and is placed in contact with an upper holding member 134 of the window frame holding member. The cover member 130 has an O-ring at a position where it contacts the upper holding member 134. The cover member 130 is opened and closed under the control of the control unit 508 (see FIG. 5 ) or by the user when the sample cell 122 is loaded and unloaded.
[0033] When the shutter 108 is closed, it separates the sample chamber 102 from the irradiation chamber 104 and blocks X-rays. Specifically, the shutter 108 is formed of a material that is opaque to X-rays and is arranged to cover the opening provided in the partition wall 106. The shutter 108 is arranged closer to the irradiation chamber 104 than the partition film 114. The controller 508 controls the operation of the motor to open and close the shutter 108. When the shutter 108 is closed, it separates the sample chamber 102 from the irradiation chamber 104. Note that even when the shutter 108 is open, the sample chamber 102 and the irradiation chamber 104 are still separated by the partition film 114.
[0034] The information processing device 112 acquires the intensity of the fluorescent X-rays from the counter 110 and analyzes the sample based on the intensity of the fluorescent X-rays. The information processing device 112 also controls the operation of each component within the irradiation chamber 104. Specifically, for example, FIG. 2 is a diagram showing the hardware configuration of the information processing device 112. The information processing device 112 is a computer and includes a calculation unit 202, a storage unit 204, a display unit 206, an input / output unit 208, and an internal bus 210.
[0035] The calculation unit 202 is a CPU (Central Processing Unit) that is a processor and performs various calculations. For example, the calculation unit 202 executes various calculations and measurement programs related to sample analysis based on the acquired fluorescent X-ray intensity.
[0036] The storage unit 204 is a non-transitory computer-readable information storage medium that stores a program executed by a computer used in the X-ray fluorescence analyzer 100. Specifically, the storage unit 204 is, for example, a random access memory (RAM) or a device capable of statically recording information, such as a hard disk drive (HDD) or solid state drive (SSD). The storage unit 204 stores a program that executes steps for performing protective control to protect the partition wall. The program causes the computer to execute an irradiation time acquisition step that acquires an irradiation time for which X-rays are irradiated onto the partition wall film 114, and a control step that performs protective control to protect the partition wall film 114 from X-ray irradiation based on the irradiation time acquired by the irradiation time acquisition unit 504. Details of these steps will be described later. The storage unit 204 also stores a cumulative irradiation time, which is the cumulative time for which X-rays have been irradiated onto the partition wall film 114 since the replacement information (described below) was acquired.
[0037] The display unit 206 is a so-called flat panel display such as a liquid crystal monitor, and displays images. For example, the display unit 206 displays the status of the device under the control of the control unit 508. Specifically, the display unit 206 displays information representing the status of the X-ray fluorescence analyzer 100, as shown in FIG. 3 . This information includes information representing the status of the X-ray source 116, the shutter 108, the atmospheres of the irradiation chamber 104 and the sample chamber 102, and the partition film 114. The status of the X-ray source 116 is a state in which the X-ray source 116 emits X-rays (hereinafter referred to as the ON state) or a state in which the X-ray source 116 does not emit X-rays (hereinafter referred to as the OFF state). The status of the shutter 108 is an open state or a closed state. The atmospheres of the irradiation chamber 104 and the sample chamber 102 are the pressures inside the irradiation chamber 104 and the sample chamber 102, respectively. The status of the partition film 114 is the material and thickness of the partition film 114 held therein, and the irradiation time.
[0038] The display unit 206 also displays error images and warning images. Specifically, the error image is displayed when the cumulative irradiation time exceeds a first set value (described below) and is an image that prompts the user to replace the partition film 114. Specifically, for example, the display unit 206 displays an error image such as that shown in FIG. 4 . The error image in FIG. 4 displays a message stating, "The cumulative X-ray irradiation time to the partition is approaching its upper limit. Please replace the partition film." below the toolbar of the application window that is displayed when the measurement program is executed. The error image also includes a button labeled "Partition Replacement." When the user clicks this button, a partition film replacement image (described below) is displayed. The warning image is displayed when the continuous irradiation time exceeds a second set value (described below) and is an image that indicates that measurement needs to be temporarily stopped.
[0039] The input / output unit 208 is one or more interfaces for the computer to exchange information with external devices, and is one or more devices for the user to input information, such as a keyboard, mouse, or touch panel. The input / output unit 208 may also include various ports for wired connections and a controller for wireless connections. The input / output unit 208 acquires the intensity of the fluorescent X-rays incident on the detector 120 from the counter.
[0040] The internal bus 210 interconnects the calculation unit 202, the storage unit 204, the display unit 206, and the input / output unit 208.
[0041] Fig. 5 is a diagram showing functional blocks of the information processing device 112. As shown in Fig. 5, the information processing device 112 functionally includes an exchange information acquisition unit 502, an irradiation time acquisition unit 504, a control unit 508, and an analysis unit 510.
[0042] The replacement information acquisition unit 502 acquires replacement information indicating that the partition wall film 114 has been replaced. Specifically, for example, when the partition wall film 114 is replaced, the replacement information acquisition unit 502 acquires replacement information including information indicating the material and / or thickness of the replaced partition wall film 114.
[0043] 6 is an example of an image (hereinafter referred to as a partition film replacement image) displayed by the display unit 206 when replacing the partition film 114. The partition film replacement image includes information about the partition film 114 held in the window frame member 126 before replacement (information about the current partition film 114) and a list of candidates for the partition film 114 to be newly held after replacement (information about the replaced partition film 114). The information about the current partition film 114 is information about the replaced partition film 114 selected in the previous partition film 114 replacement. The information about the partition film 114 includes information about the material and thickness of the partition film 114.
[0044] 6, the information of the current barrier rib film 114 indicates that the material is polyester and the thickness is 3.0 μm. The list of candidates for the information of the barrier rib film 114 after replacement includes a candidate whose material is polyester and the thickness is 3.0 μm, a candidate whose material is polyester and the thickness is 2.5 μm, a candidate whose material is polyester and the thickness is 2.0 μm, and a candidate whose material is polyimide and the thickness is 5.0 μm.
[0045] After replacing the partition wall film 114 held by the window frame member 126, the user operates the input / output unit 208, such as a mouse, to select, from the candidates, information on the replaced partition wall film 114 that corresponds to the replaced partition wall film 114. When the OK button on the partition wall film replacement image is further clicked, the replacement information acquisition unit 502 acquires replacement information including information on the selected partition wall film 114.
[0046] The irradiation time acquisition unit 504 acquires the irradiation time during which X-rays are irradiated onto the partition film 114. Specifically, for example, the irradiation time acquisition unit 504 measures the time during which the X-ray source 116 emits X-rays and the shutter 108 is open as the irradiation time. The control unit 508 controls whether the X-ray source 116 is emitting X-rays or is stopped. The control unit 508 also controls the opening and closing of the shutter 108. Therefore, the irradiation time acquisition unit 504 can measure the time during which the X-ray source 116 emits X-rays and the shutter 108 is open. In a case where the shutter 108 is not provided and the irradiation time during which X-rays are irradiated onto the partition film 114 is controlled only by ON / OFF control of the X-ray source 116, the irradiation time acquisition unit 504 measures the time during which the X-ray source 116 is in the ON state and emits X-rays. The irradiation time is measured in units of, for example, 0.1 hours. In the following examples, an irradiation time of 10 hours and 30 minutes will be expressed as 10.5H, etc.
[0047] In the present disclosure, the irradiation time includes two types of irradiation time: cumulative irradiation time and continuous irradiation time. Specifically, the cumulative irradiation time is the cumulative time that X-rays have been irradiated onto the partition film 114 since the replacement information was acquired. The cumulative irradiation time is set to an initial value (e.g., 0.0 hours) when the replacement information is acquired. The cumulative irradiation time is stored in the memory unit 204 at the end of measurement. Each time a measurement is performed, the time that X-rays have been irradiated in that measurement is added to the stored value. In other words, the cumulative irradiation time is the total time of irradiation times in all measurements performed after the initial value was set.
[0048] The continuous irradiation time is the time during which X-rays are continuously irradiated onto the partition film 114 from the start of irradiation. Specifically, the continuous irradiation time is the time during which X-rays are irradiated onto the partition film 114 in one measurement. For example, the X-ray source 116 starts emitting X-rays with the shutter 108 closed. After the intensity of the X-rays emitted by the X-ray source 116 stabilizes, the shutter 108 is opened and X-rays are irradiated onto the sample. After a predetermined measurement time has elapsed, the shutter 108 is closed. The continuous irradiation time is the time from when the shutter 108 opens to when it closes. When air is present around the partition film 114, for example, if the continuous irradiation time is extended with the cover member 130 closed, the ozone concentration increases, accelerating deterioration of the partition film 114.
[0049] Furthermore, based on the measurement time included in the acquired measurement conditions (described later), the irradiation time acquisition unit 504 calculates a predicted continuous irradiation time as the time during which X-rays will be irradiated onto the partition film 114 through measurements performed in accordance with the measurement conditions. Specifically, for example, the irradiation time acquisition unit 504 acquires the measurement time included in the acquired measurement conditions as the predicted continuous irradiation time. Furthermore, for example, the irradiation time acquisition unit 504 adds the measurement time included in the acquired measurement conditions to the cumulative irradiation time stored in the storage unit 204 to acquire the predicted cumulative irradiation time.
[0050] That is, the irradiation time includes two types of irradiation time: the actual irradiation time measured during actual measurement and the predicted irradiation time obtained by calculation. The actual irradiation time is a value measured for the time during which X-rays are emitted and the shutter 108 is open, and the predicted irradiation time is a value calculated based on the measurement time included in the measurement conditions. Therefore, the cumulative irradiation time includes the actual cumulative irradiation time and the predicted cumulative irradiation time. Furthermore, the continuous irradiation time includes the actual continuous irradiation time and the predicted continuous irradiation time.
[0051] The measurement condition acquisition unit 506 acquires measurement conditions, including measurement time. Specifically, for example, by executing a program for sample analysis, the display unit 206 displays a screen (not shown) for accepting input of measurement conditions. The measurement conditions include a cell identification number that identifies the placement position of the sample cell 122 in the preparation chamber (not shown), and conditions such as the voltage of the X-ray source 116 and measurement time associated with the cell identification number. The measurement conditions may also include other conditions related to the measurement. The measurement condition acquisition unit 506 acquires the measurement conditions when the user inputs the measurement conditions using a keyboard or the like. Each measurement condition is assigned a measurement identification number (hereinafter referred to as a measurement ID) to distinguish it from other measurement conditions, and the measurement conditions are stored in the storage unit 204. Furthermore, when consecutive analyses are performed based on multiple measurement conditions, the multiple measurement conditions may be stored in association with each other. The associated multiple measurement conditions are also referred to as a measurement recipe, etc.
[0052] The control unit 508 performs protection control to protect the partition wall film 114 from X-ray irradiation based on the irradiation time acquired by the irradiation time acquisition unit 504. Specifically, the control unit 508 performs protection control when the cumulative irradiation time exceeds a first set value. The first set value is set based on information representing the material and / or thickness of the partition wall film 114. The first set value is a value representing time. For example, a value of 24H is set as the first set value corresponding to a partition wall film 114 made of polypropylene and having a thickness of 3.0 μm. The first set value is set to a larger value as the material of the partition wall film 114 is more resistant to X-rays and ozone. Furthermore, the first set value is set to a larger value as the thickness of the partition wall film 114 is larger. The relationship between the first set value and the information representing the material and / or thickness of the partition wall film 114 is stored in advance in the storage unit 204.
[0053] Furthermore, the control unit 508 performs protection control based on the continuous irradiation time (actual continuous irradiation time or predicted continuous irradiation time). Specifically, for example, the control unit 508 performs protection control when the continuous irradiation time (actual continuous irradiation time or predicted continuous irradiation time) exceeds a second set value. The second set value is a value representing one preset time. For example, a value of 1H is set as the second set value. Note that, similar to the first set value, the second set value may be set to a different value for each piece of information representing the material and / or thickness of the partition film 114.
[0054] The control unit 508 performs protection control to protect the partition film 114 from X-ray irradiation. For example, the protection control is control to prevent measurement from starting. Specifically, the control unit 508 prevents measurements that may damage the partition film 114 in advance by not performing measurements for some or all of the measurement conditions included in the measurement recipe based on the predicted irradiation time. For example, the control unit 508 controls the measurement condition acquisition unit 506 not to accept input of measurement conditions or instructions to start measurement. This makes it impossible to register a measurement ID or press the measurement start button, thereby preventing measurement from being performed.
[0055] Furthermore, for example, the protection control is control to close the shutter 108. Specifically, the control unit 508 controls to close the shutter 108 when the cumulative irradiation time exceeds a first set value and / or when the continuous irradiation time exceeds a second set value. Furthermore, for example, the protection control is control to stop the X-ray source 116 from emitting X-rays. Specifically, the control unit 508 controls the X-ray source 116 from emitting X-rays when the cumulative irradiation time exceeds a first set value and / or when the continuous irradiation time exceeds a second set value. Furthermore, for example, the protection control is control to cause the display unit 206 to display a message indicating that the partition film 114 may be damaged. Specifically, the control unit 508 causes the display unit 206 to display an error image or a warning image.
[0056] The control unit 508 may control the operation of each component of the X-ray fluorescence analyzer 100. For example, the control unit 508 may control switching between the ON and OFF states of the X-ray source 116, opening and closing the cover member 130, transporting the sample cell 122, operation of a pump that evacuates the irradiation chamber 104, the orientation of the spectroscopic element 118, and the like.
[0057] The analysis unit 510 analyzes the sample. Specifically, the analysis unit 510 analyzes the elements contained in the sample based on the intensity of the fluorescent X-rays acquired by the input / output unit 208.
[0058] Next, the protection control performed by the control unit 508 will be described with reference to the flowcharts shown in Figures 7 to 12. It is assumed that the user has placed the sample cell 122 in which the sample has been placed in advance in a preparation room (not shown).
[0059] First, the measurement condition acquisition unit 506 acquires measurement conditions (S701). Specifically, for example, the control unit 508 executes a program for sample analysis, causing the display unit 206 to display a screen (not shown) for accepting measurement conditions and measurement instructions. The measurement condition acquisition unit 506 acquires measurement conditions when the user inputs measurement conditions such as measurement time using a keyboard or the like. Furthermore, the control unit 508 acquires a measurement instruction when the user issues an instruction to start measurement using a mouse or the like. Note that each of the following steps is executed by the above program. Furthermore, it is assumed here that the measurement condition acquisition unit 506 has acquired a measurement recipe including M measurement conditions with measurement IDs 1 to M.
[0060] Next, the control unit 508 determines whether an executable measurement condition is included (S702). Specifically, FIG. 8 is a flowchart for determining whether an executable measurement condition is included in a measurement recipe. At the start of the flowchart in FIG. 8, variables i and k are set to 1, and the continuous irradiation time is set to an initial value (zero). The initial value of the predicted cumulative irradiation time is set to the cumulative irradiation time stored in the storage unit 204. First, the irradiation time is calculated based on the i-th measurement condition (initial value: 1) (S802). The calculated irradiation time may be, for example, the measurement time included in the measurement condition, or may be a value obtained by multiplying a predetermined coefficient or adding a predetermined value to the measurement time included in the measurement condition.
[0061] Next, the irradiation time acquisition unit 504 adds the calculated irradiation time to the cumulative irradiation time to acquire a predicted cumulative irradiation time (S804). For example, when i is 1, the irradiation time acquisition unit 504 adds the measurement time included in the first measurement condition to the cumulative irradiation time stored in the storage unit 204, and acquires the calculated value as the predicted cumulative irradiation time.
[0062] Next, it is determined whether the predicted cumulative irradiation time exceeds a first set value (S806). For example, if the first set value is 24 hours, it is determined that the predicted cumulative irradiation time exceeds the first set value when the predicted cumulative irradiation time exceeds 24 hours. If the predicted cumulative irradiation time exceeds the first set value, the execution of the flowchart in FIG. 8 is terminated.
[0063] Next, the irradiation time acquisition unit 504 adds the calculated irradiation time to the continuous irradiation time to acquire the predicted continuous irradiation time (S808). For example, when i is 1, the irradiation time acquisition unit 504 adds the measurement time included in the first measurement condition to the continuous irradiation time, which is the initial value (zero value), and acquires the calculated value as the predicted continuous irradiation time.
[0064] Next, it is determined whether the predicted continuous irradiation time exceeds a second set value (S810). For example, if the second set value is 1 H, it is determined that the predicted continuous irradiation time exceeds the second set value when the predicted continuous irradiation time exceeds 1 H. If the predicted continuous irradiation time exceeds the second set value, the execution of the flowchart in FIG. 8 is terminated.
[0065] Next, if the sample cell 122 is to be unloaded after the measurement based on the i-th measurement condition is performed (Yes in S812), the continuous irradiation time is set to the initial value (zero value) (S814), and the process proceeds to S816. On the other hand, if the sample cell 122 is not to be unloaded after the measurement based on the i-th measurement condition is performed (No in S812), the process proceeds to S816. Whether or not to unload the sample cell 122 is determined based on whether the samples to be successively measured are the same or different. Specifically, for example, if the cell identification number included in the i-th measurement condition is different from the cell identification number included in the (i+1)-th measurement condition, it is determined in S812 that the sample cell 122 is to be unloaded. On the other hand, if the cell identification number included in the i-th measurement condition is the same as the cell identification number included in the (i+1)-th measurement condition, it is determined in S812 that the sample cell 122 is not to be unloaded.
[0066] While the partition film 114 is being irradiated with X-rays, the ozone concentration in the space inside the lid member 130 increases. Because the lid member 130 is opened when the sample cell 122 is unloaded, the ozone concentration in the space inside the lid member 130 becomes equivalent to the concentration in the atmosphere each time the sample cell 122 is unloaded. Therefore, by setting the continuous irradiation time to an initial value (zero value) when it is determined that the sample cell 122 is to be unloaded, it is possible to predict a continuous irradiation time that reflects actual conditions.
[0067] In S816, it is determined whether i is equal to M, i.e., whether the irradiation time has been calculated for all measurement conditions included in the measurement recipe (S816). If i is smaller than M, 1 is added to i and the process returns to S802, where steps S802 to S814 are executed for the next measurement condition. The cumulative irradiation time in S804 is added each time the process is repeated. The continuous irradiation time in S808 is added repeatedly unless an initial value is set in S814. On the other hand, if it is determined that i is equal to M, it is determined that all measurement conditions included in the measurement recipe are executable, and the flowchart in FIG. 8 ends.
[0068] If the determination in S806 or S810 is Yes, some or all of the measurement conditions included in the measurement recipe are determined to be unfeasible. Specifically, the i-th to M-th measurement conditions are determined to be unfeasible. That is, the 1st to (i-1)th measurement conditions are determined to be feasible. Assume that the number of measurement recipes (i-1) determined to be feasible at the end of the flowchart in FIG. 8 is N.
[0069] 7 ends without performing measurement. On the other hand, if it is determined in S702 that an executable measurement condition is not included (i.e., N is 0), the control unit 508 controls the X-ray source 116 to be in the ON state (S704). This control causes the X-ray source 116 to emit X-rays. After the X-ray source 116 starts emitting X-rays, a certain time period elapses until the intensity of the emitted X-rays stabilizes, and then the next step is executed.
[0070] Next, the sample cell 122 is loaded based on the kth measurement condition (S706). Specifically, the control unit 508 controls the opening of the lid member 130, and causes a transport device (not shown), such as a robot arm, to transport the sample cell 122 placed in the preparation room by the user to the measurement position. At this time, the sample cell 122 placed at the position indicated by the cell identification number included in the kth measurement condition is transported. The measurement position is the position where the sample is irradiated with X-rays, as shown in FIG. 1. After the sample cell 122 is placed at the measurement position, the control unit 508 controls the closing of the lid member 130.
[0071] Next, the control unit 508 controls the shutter 108 to open, and starts detecting fluorescent X-rays (S708). Specifically, the control unit 508 controls the motor to open the shutter 108. When the shutter 108 is open and the X-ray source 116 is emitting X-rays, the X-rays are irradiated onto the sample through the partition film 114. Fluorescent X-rays are emitted from the sample irradiated with X-rays, and a portion of the fluorescent X-rays is dispersed by the spectroscopic element 118. The dispersed fluorescent X-rays are detected by the detector 120, and the intensity of the fluorescent X-rays is counted by the counter 110. The counter 110 starts transmitting the intensity of the fluorescent X-rays to the information processing device 112. The detection of the fluorescent X-rays is continued until the measurement time has elapsed or protective control is executed.
[0072] The irradiation time acquisition unit 504 starts measuring the irradiation time when the control unit 508 opens the shutter 108. Fig. 9 is a flowchart for measuring the irradiation time. The flowchart shown in Fig. 9 is executed in parallel with the flowchart shown in Fig. 7 while fluorescent X-rays are being detected.
[0073] First, the continuous irradiation time is set to an initial value (S902). Specifically, the continuous irradiation time is set to 0.0 H. This step may be executed when the control unit 508 performs control to close the lid member 130. The control unit also acquires the cumulative irradiation time stored in the storage unit 204.
[0074] Next, the irradiation time acquisition unit 504 measures the continuous irradiation time and the accumulated irradiation time (S904). Specifically, for example, the irradiation time acquisition unit 504 measures the difference between the current time and the time when the shutter 108 is opened as the continuous irradiation time. Furthermore, the irradiation time acquisition unit 504 adds the difference between the current time and the time when the shutter 108 is opened to the accumulated irradiation time acquired from the storage unit 204, and measures it as the accumulated irradiation time.
[0075] Step S904 is continuously executed as long as the shutter 108 is open (Yes in S906). When the shutter 108 is closed (No in S906), the irradiation time acquisition unit 504 ends measurement of the continuous irradiation time and the cumulative irradiation time (S908). The irradiation time acquisition unit 504 also stores the cumulative irradiation time in the storage unit 204 (S910).
[0076] While fluorescent X-ray detection is being performed, the display unit 206 displays information indicating the status of the X-ray fluorescence analyzer 100, as shown in Fig. 3. This allows the user to check the accumulated irradiation time. The continuous irradiation time may also be displayed in Fig. 3. Furthermore, if the accumulated irradiation time reaches a predetermined percentage (e.g., 80%) of the first set value while steps S710, S714, and S710 are being repeatedly executed, a message may be displayed indicating that the irradiation time is approaching the upper limit.
[0077] While fluorescent X-rays are being detected, the determinations of S710, S714, and S718 are made. In S710, it is determined whether the cumulative irradiation time exceeds a first set value. For example, if the first set value is 24 hours, it is determined that the cumulative irradiation time exceeds the first set value when the cumulative irradiation time exceeds 24 hours. If it is determined that the cumulative irradiation time exceeds the first set value, a first protection control (S712) is executed (described below).
[0078] In S714, it is determined whether the continuous irradiation time exceeds a second set value. For example, if the second set value is 1 H, when the continuous irradiation time exceeds 1 H, it is determined that the continuous irradiation time exceeds the second set value. If it is determined that the continuous irradiation time exceeds the second set value, a second protection control (S716) is executed (described below).
[0079] If the specified measurement time has elapsed while the cumulative irradiation time does not exceed the first set value and the continuous irradiation time does not exceed the second set value (Yes in S718), the control unit 508 controls the shutter 108 to close, thereby ending the detection of fluorescent X-rays (S720). Specifically, the control unit 508 closes the shutter 108 by controlling the motor. In addition, the counter 110 stops transmitting the intensity of the fluorescent X-rays to the information processing device 112. The analysis unit 510 analyzes the elements contained in the sample based on the intensity of the fluorescent X-rays.
[0080] Next, the sample cell 122 is removed, and the continuous irradiation time is set to the initial value (S722). Specifically, the control unit 508 controls the opening of the lid member 130 and causes a transport device (not shown), such as a robot arm, to transport the sample cell 122 from the measurement position to the preparation chamber. After the sample cell 122 is placed in the preparation chamber, the control unit 508 controls the closing of the lid member 130. Note that step S722 is executed only when the cell identification number included in the kth measurement condition is different from the cell identification number included in the k+1th measurement condition. If the cell identification number included in the kth measurement condition is the same as the cell identification number included in the k+1th measurement condition, measurements based on the k+1th measurement condition are performed continuously, and step S722 is omitted.
[0081] In S723, it is determined whether k is equal to N, i.e., whether measurements have been completed for all feasible measurement conditions. If k is smaller than N, 1 is added to k (S724) and the process returns to S706, where steps S706 to S722 are executed for the next measurement condition. Note that if S724 is omitted and steps S706 to S722 are executed again, S706 is omitted.
[0082] If it is determined that k is equal to N, the control unit 508 controls the X-ray source 116 to be in the OFF state (S725), which causes the X-ray source 116 to stop emitting X-rays.
[0083] S725 is a step that is executed when the measurement is completed without executing protective control based on the irradiation time, which is the actual value. If it is determined in S710 that the cumulative irradiation time exceeds the first set value, the control unit 508 executes the first protective control (S712).
[0084] 10 is a flowchart showing the first protection control. First, the display unit 206 displays an error image (S1002). The error image informs the user that the partition film 114 needs to be replaced.
[0085] Next, the detection of the fluorescent X-rays is stopped (S1004). Specifically, the counter 110 stops transmitting the intensity of the fluorescent X-rays to the information processing device 112.
[0086] Next, the control unit 508 closes the shutter 108 (S1006), unloads the sample cell 122 (S1008), and turns off the X-ray source 116 (S1010). These operations may be performed in any order.
[0087] According to the present disclosure, measurements that may damage the partition film 114 can be avoided in advance by not performing measurements for some or all of the measurement conditions included in the measurement recipe based on the predicted irradiation time. Furthermore, by having the control unit 508 close the shutter 108, X-rays can be prevented from being irradiated onto the partition film 114, which may be damaged. Turning the X-ray source 116 off can also prevent X-rays from being irradiated onto the partition film 114, which may be damaged. Furthermore, by displaying an error image in S1002, the user can be prompted to replace the partition film 114. This disclosure is particularly suitable for cases where the irradiation chamber 104 is filled with air and the interior of the irradiation chamber 104 is a vacuum. In this case, if the partition film 114 is damaged, air inside the irradiation chamber 104 will suddenly flow into the interior of the irradiation chamber 104. At this time, it is possible to prevent each component (e.g., the detector 120) arranged in the irradiation chamber 104 from being temporarily subjected to large pressure, which could result in damage.
[0088] 11 is a flowchart of the process executed when replacing the partition wall film 114. The user replaces the partition wall film 114 when the error image is displayed.
[0089] First, the display unit 206 displays a partition film replacement image (S1102). Specifically, the display unit 206 displays a partition film replacement image as shown in FIG. 6. After replacing the partition film 114 held by the window frame member 126, the user operates the input / output unit 208, such as a mouse, to select information on the replaced partition film 114 corresponding to the replaced partition film 114 from the candidates. When the OK button on the partition film replacement image is clicked, the replacement information acquisition unit 502 acquires replacement information including information on the selected partition film 114.
[0090] Next, when the replacement information acquisition unit 502 acquires the replacement information (Yes in S1104), a first set value is set based on the information about the partition wall film 114 included in the replacement information (S1106). For example, if the information about the partition wall film 114 indicates that the material is polypropylene and the thickness is 3.0 μm, a first set value of 24H is set. Note that if the information about the partition wall film 114 includes information about a second set value, the second set value may be set.
[0091] Furthermore, the cumulative irradiation time is set to an initial value (S1108). Specifically, the control unit 508 sets the cumulative irradiation time stored in the memory unit 204 to an initial value (0H). The cumulative irradiation time is added up according to the time for which X-rays are irradiated, but an initial value is not set for each measurement. Therefore, the cumulative irradiation time continues to be added up unless the partition film 114 is replaced. According to the present disclosure, since the initial value of the cumulative irradiation time is set in this step, it is possible to manage the cumulative time for which X-rays are irradiated onto one sheet of partition film 114. In other words, the degree of deterioration of the partition film 114 can be grasped by measuring the cumulative irradiation time.
[0092] Even when the partition film replacement image is displayed, if the partition film 114 is not replaced, replacement information is not acquired in S1104. In this case, the first set value and the cumulative irradiation time are not updated.
[0093] 12 is a flowchart showing the second protective control. If it is determined in S714 that the continuous irradiation time exceeds the second set value, the control unit 508 executes the second protective control (S716). First, the display unit 206 displays a warning image (S1202). The warning image indicates that measurement needs to be temporarily stopped.
[0094] Next, the detection of the fluorescent X-rays is stopped (S1204). Specifically, the counter 110 stops transmitting the intensity of the fluorescent X-rays to the information processing device 112.
[0095] Then, the control unit 508 closes the shutter 108 (S1206) and unloads the sample cell 122 (S1208). When unloading the sample cell 122, the cover member 130 is opened.
[0096] Because air is present inside the lid member 130, some of the oxygen contained in the air is converted to ozone while the sample is being irradiated with X-rays. Therefore, if the continuous irradiation time is long, the ozone concentration inside the lid member 130 increases. If measurement is continued while the ozone concentration inside the lid member 130 is high, the partition film 114 is likely to be damaged even if the cumulative irradiation time does not exceed the first set value.
[0097] If the continuous irradiation time exceeds the second set value, the sample cell 122 is temporarily transported to the preparation room, thereby reducing the ozone concentration inside the cover member 130. This prevents the partition film 114 from being damaged in a time shorter than the first set value. Furthermore, the second protection control prevents the X-ray source 116 from being turned off. Therefore, measurement can be immediately resumed.
[0098] The present disclosure is not limited to the above-described embodiments and various modifications are possible. The configuration of the X-ray fluorescence analyzer 100 described above is an example and is not intended to be limiting. The configuration described in the above-described embodiments may be replaced with a configuration that is substantially the same as the configuration described in the above-described embodiments, that provides the same effects, or that achieves the same purpose.
[0099] For example, in the flowchart shown in Fig. 7, the determinations in S710 and S714 are made during measurement. Therefore, if a Yes is determined in S710 and S714 while a measurement based on one measurement condition is being performed, the measurement is interrupted. However, the determinations in S710 and S714 may be made after the measurement based on each measurement condition is completed. In other words, steps S718 and S720 may be performed between S708 and S710.
[0100] 7 is an example of a flowchart illustrating protection control while performing measurements based on multiple measurement conditions, but is not limited to this as long as protection control can be performed based on irradiation time. For example, as long as the irradiation time during which the sample is irradiated with X-rays can be measured, the timing of turning the X-ray source 116 on or off, the timing of opening and closing the shutter, and the timing of loading and unloading the sample cell are design items that may be changed as appropriate.
[0101] REFERENCE SIGNS LIST 100 X-ray fluorescence analyzer, 102 sample chamber, 104 irradiation chamber, 106 partition wall, 108 shutter, 110 counter, 112 information processing device, 114 partition film, 116 X-ray source, 118 spectroscopic element, 120 detector, 122 sample cell, 124 sample stage, 126 window frame member, 128 film support member, 130 lid member, 132 lower holding member, 134 upper holding member, 202 calculation unit, 204 memory unit, 206 display unit, 208 input / output unit, 210 internal bus, 502 exchange information acquisition unit, 504 irradiation time acquisition unit, 506 measurement condition acquisition unit, 508 control unit, 510 analysis unit.
Claims
1. A fluorescent X-ray analysis apparatus having: a sample chamber in which a sample is placed; an irradiation chamber separated from the sample chamber by a partition including a partition film that is transparent to X-rays, and in which an X-ray source is placed that emits X-rays to the sample through the partition film; and an information processing device, wherein the information processing device has: an irradiation time acquisition unit that acquires an irradiation time for which X-rays are irradiated onto the partition film; and a control unit that performs protection control to protect the partition film from irradiation with X-rays based on the irradiation time acquired by the irradiation time acquisition unit.
2. The fluorescent X-ray analysis apparatus described in claim 1, characterized in that the information processing device has a replacement information acquisition unit that acquires replacement information indicating that the partition film has been replaced, the irradiation time acquisition unit measures a cumulative irradiation time, which is the cumulative time during which X-rays have been irradiated onto the partition film since the replacement information was acquired, and the control unit performs the protection control when the cumulative irradiation time exceeds a first set value.
3. The fluorescent X-ray analysis apparatus according to claim 2, characterized in that the irradiation time acquisition unit measures a continuous irradiation time, which is the time during which X-rays are continuously irradiated from the start of irradiation of the partition film, and the control unit performs the protection control when the continuous irradiation time exceeds a second set value.
4. The fluorescent X-ray analysis apparatus of claim 1, characterized in that the information processing device includes a measurement condition acquisition unit that acquires measurement conditions including a measurement time, the irradiation time acquisition unit calculates a predicted continuous irradiation time as the time for which X-rays are irradiated to the partition film by a measurement performed according to the measurement conditions based on the measurement time included in the acquired measurement conditions, and the control unit performs the protection control based on the predicted continuous irradiation time.
5. The information processing device further includes a replacement information acquisition unit that acquires replacement information indicating that the partition film has been replaced, and a memory unit that stores a cumulative irradiation time, which is the cumulative time during which the partition film has been irradiated with X-rays since the replacement information was acquired, wherein the irradiation time acquisition unit adds the predicted continuous irradiation time to the cumulative irradiation time stored in the memory unit to calculate the predicted cumulative irradiation time, and the control unit performs the protection control when the predicted cumulative irradiation time exceeds a first set value. The fluorescent X-ray analysis device described in claim 4, characterized in that the information processing device further includes a replacement information acquisition unit that acquires replacement information indicating that the partition film has been replaced, and a memory unit that stores a cumulative irradiation time, which is the cumulative time during which the partition film has been irradiated with X-rays since the replacement information was acquired, wherein the irradiation time acquisition unit calculates the predicted cumulative irradiation time by adding the predicted continuous irradiation time to the cumulative irradiation time stored in the memory unit, and the control unit performs the protection control when the predicted cumulative irradiation time exceeds a first set value.
6. The fluorescent X-ray analysis apparatus according to claim 5, characterized in that the control unit performs the protective control when the predicted continuous irradiation time exceeds a second set value.
7. The fluorescent X-ray analysis apparatus according to any one of claims 4 to 6, characterized in that the protective control is a control that does not allow measurement to be started.
8. The fluorescent X-ray analysis apparatus according to any one of claims 1 to 3, further comprising a shutter that, when closed, isolates the sample chamber from the irradiation chamber and blocks X-rays, and the irradiation time acquisition unit measures the time during which the X-ray source emits X-rays and the shutter is open as the irradiation time.
9. The fluorescent X-ray analysis apparatus according to claim 8, wherein the protection control is a control for closing the shutter.
10. The fluorescent X-ray analysis apparatus according to any one of claims 1 to 3, wherein the protection control is a control for stopping the emission of X-rays from the X-ray source.
11. The fluorescent X-ray analysis apparatus according to any one of claims 1 to 6, characterized in that the information processing device has a display unit that performs display based on the control of the control unit, and the protection control is control that causes the display unit to display a message indicating that the partition film may be damaged.
12. The fluorescent X-ray analysis apparatus of claim 3 or 6, characterized in that the replacement information includes information representing the material and / or thickness of the replaced partition film, and the first set value and / or the second set value are set based on the information representing the material and / or thickness.
13. The fluorescent X-ray analysis apparatus according to claim 11, wherein the display unit further displays the accumulated exposure time and / or the continuous exposure time.
14. A non-transitory computer-readable information storage medium storing a program executed by a computer used in an X-ray fluorescence analyzer, the X-ray fluorescence analyzer comprising: a sample chamber in which a sample is placed; an irradiation chamber separated from the sample chamber by a partition including a partition film that is transparent to X-rays in part, and in which an X-ray source is placed, which emits X-rays to the sample through the partition film; and the computer, the program causing the computer to execute an irradiation time acquisition step of acquiring an irradiation time for which X-rays are irradiated onto the partition film; and a protection control step of performing protection control to protect the partition film from irradiation with X-rays based on the irradiation time acquired in the irradiation time acquisition step.
15. A program executed by a computer for use in an X-ray fluorescence analyzer, the X-ray fluorescence analyzer having: a sample chamber in which a sample is placed; an irradiation chamber separated from the sample chamber by a partition including a partition film that is transparent to X-rays, and in which an X-ray source is placed, which emits X-rays to the sample through the partition film; and the computer, the program causing the computer to execute an irradiation time acquisition step of acquiring an irradiation time for which X-rays are irradiated onto the partition film; and a protection control step of performing protection control to protect the partition film from irradiation with X-rays based on the irradiation time acquired in the irradiation time acquisition step.
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