CN109951940B - X-ray analysis device and method for determining replacement time of X-ray detector - Google Patents

X-ray analysis device and method for determining replacement time of X-ray detector Download PDF

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CN109951940B
CN109951940B CN201811238688.1A CN201811238688A CN109951940B CN 109951940 B CN109951940 B CN 109951940B CN 201811238688 A CN201811238688 A CN 201811238688A CN 109951940 B CN109951940 B CN 109951940B
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detector
ray
data
replacement time
ray detector
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CN109951940A (en
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铃木桂次郎
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Shimadzu Corp
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Shimadzu Corp
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Abstract

The invention provides an X-ray analysis device capable of judging the proper replacement time of an X-ray detector and a replacement time judging method of the X-ray detector. In the present invention, an X-ray tube (1) irradiates X-rays onto a sample (S). The detector (3) detects X-rays after the sample (S) has been irradiated. A detector high voltage circuit (4) applies a voltage to the detector (3). A data acquisition unit (81) acquires data having a wave height distribution curve of a peak unique to the sample (S) from a detection signal from the detector (3). A replacement time determination unit (82) determines the replacement time of the detector (3) on the basis of the peak included in the data of the wave height distribution curve acquired by the data acquisition unit (81) by measuring the standard sample.

Description

X-ray analysis device and method for determining replacement time of X-ray detector
Technical Field
The present invention relates to an X-ray analyzer and a replacement time determination method for an X-ray detector, which are provided with an X-ray source for irradiating an X-ray onto a sample, an X-ray detector for detecting the X-ray after the irradiation onto the sample, and a voltage applying section for applying a voltage to the X-ray detector.
Background
An X-ray analysis apparatus such as a wavelength-dispersive fluorescent X-ray apparatus is equipped with an X-ray source for irradiating a sample with X-rays and an X-ray detector for detecting the X-rays after the irradiation of the sample. As the X-ray light source, for example, an X-ray tube is used. As the X-ray detector, for example, a proportional counter tube or a scintillation counter is used.
The X-ray tube includes a filament and a target, and applies high voltage between the filament and the target. As a result, thermal electrons are emitted from the filament toward the target, and the thermal electrons strike the target, thereby generating X-rays. Since the filament and the target have a long life, when the X-ray tube reaches the replacement time, the X-ray tube is replaced with a new one (for example, refer to patent document 1 below).
Similarly, the X-ray detector such as the proportional counter tube and the scintillation counter is also degraded with use, and therefore needs to be replaced periodically. For example, the proportional counter tube is configured such that a core wire made of tungsten wire is provided in the enclosed argon gas, and the core wire needs to be replaced with argon gas deteriorated, or with dirt or the like. The scintillation counter includes a scintillator and a photomultiplier tube, and needs to be replaced as these components deteriorate.
Conventionally, the replacement time of an X-ray source and an X-ray detector is based on the use time of the X-ray source and the X-ray detector. Namely, the following constitution is adopted: the use time is accumulated and recorded, and if the use time exceeds a certain time, the replacement time is determined.
[ Prior Art literature ]
[ patent literature ]
Japanese patent laid-open No. 5-283192
Disclosure of Invention
[ problem to be solved by the invention ]
However, when the replacement timing of the X-ray detector is determined based on the usage time, the proper replacement timing may not be determined. For example, when the circuit side to which the voltage is applied is degraded, not the degradation of the X-ray detector itself, or the like, even if the X-ray detector does not reach the replacement time, the X-ray detector may be determined as the replacement time. In this way, when the proper replacement timing of the X-ray detector cannot be determined, there is a concern that the X-ray detector that does not need to be replaced may be replaced or that the X-ray detector may malfunction before replacement.
The present invention has been made in view of the above circumstances, and an object thereof is to provide an X-ray analysis device capable of determining an appropriate replacement timing of an X-ray detector, and a replacement timing determination method for an X-ray detector.
[ means for solving the problems ]
(1) An X-ray analysis device is provided with an X-ray light source, an X-ray detector, a voltage application unit, a data acquisition unit, and a replacement time determination unit. The X-ray source irradiates X-rays toward a sample. The X-ray detector detects X-rays after the sample is irradiated. The voltage applying section applies a voltage to the X-ray detector. The data acquisition unit acquires data having a wave height distribution curve of a peak unique to a sample from a detection signal from the X-ray detector. The replacement time determination unit determines a replacement time of the X-ray detector based on a peak included in the data of the wave height distribution curve acquired by the data acquisition unit by measuring the standard sample.
According to this configuration, the replacement timing of the X-ray detector can be determined using: the peak included in the data of the wave height distribution curve obtained by measuring the standard sample with a constant voltage applied to the X-ray detector changes with the deterioration of the X-ray detector. Specifically, the position of the peak when a certain voltage is applied to the X-ray detector to measure the same standard sample is shifted to the low energy side with the deterioration of the X-ray detector. By utilizing such characteristics, an appropriate replacement timing of the X-ray detector can be determined.
(2) The X-ray analysis apparatus may further include a voltage adjustment unit that adjusts the voltage applied to the X-ray detector by the voltage application unit so that a position of a peak included in the data of the wave height distribution curve acquired by the data acquisition unit reaches a predetermined reference position by measuring a standard sample. In this case, the replacement time determination unit may determine the replacement time of the X-ray detector based on the voltage value adjusted by the voltage adjustment unit.
According to this configuration, the voltage applied to the X-ray detector is adjusted so that the peak included in the data of the wave height distribution curve obtained by measuring the standard sample reaches a predetermined reference position. In this case, since the higher the voltage value is required to be adjusted as the X-ray detector is degraded, the proper replacement timing of the X-ray detector can be determined from the adjusted voltage value.
(3) The replacement time determination unit may determine the replacement time of the X-ray detector by comparing the voltage value adjusted by the voltage adjustment unit with a threshold value.
According to this configuration, when the voltage applied to the X-ray detector is adjusted so that the peak reaches a predetermined reference position, the voltage value is compared with the threshold value, and thus, the appropriate replacement timing of the X-ray detector can be determined in real time.
(4) The X-ray analysis apparatus may further include a history storage unit that stores a history of the voltage value adjusted by the voltage adjustment unit. In this case, the replacement time determination unit may determine the replacement time of the X-ray detector based on the history of the voltage values stored in the history storage unit.
According to this configuration, a history of voltage values at the time of adjusting the voltage applied to the X-ray detector so that the peak reaches a predetermined reference position can be stored, and the replacement timing of the X-ray detector can be predicted from the history. Thus, the preparation for replacement can be performed by confirming the replacement timing of the X-ray detector in advance, and therefore the X-ray detector can be reliably replaced at an appropriate time.
(5) The replacement time determination unit may determine the replacement time of the X-ray detector based on a change in the position of the peak included in the data of the wave height distribution curve acquired by the data acquisition unit by measuring the standard sample.
According to this configuration, the position of the peak included in the data of the wave height distribution curve obtained by measuring the standard sample changes with the deterioration of the X-ray detector. In this case, the degree of change in the position of the peak increases as the X-ray detector is degraded, so that the proper replacement timing of the X-ray detector can be determined from the change in the position of the peak.
(6) The replacement time determination unit may determine the replacement time of the X-ray detector by comparing a change amount of the position of the peak included in the data of the wave height distribution curve acquired by the data acquisition unit by measuring the standard sample with a threshold value.
According to this configuration, by comparing the amount of change in the position of the peak that changes with the deterioration of the X-ray detector with the threshold value, the appropriate replacement timing of the X-ray detector can be determined in real time.
(7) The X-ray analysis apparatus may further include a history storage unit that stores a history of positions of peaks included in the data of the wave height distribution curve acquired by the data acquisition unit by measuring the standard sample. In this case, the replacement time determination unit may determine the replacement time of the X-ray detector based on the history of the position of the peak stored in the history storage unit.
According to this configuration, a history of the position of the peak that changes with the deterioration of the X-ray detector can be stored, and the replacement timing of the X-ray detector can be predicted from the history. Thus, the preparation for replacement can be performed by confirming the replacement timing of the X-ray detector in advance, and therefore the X-ray detector can be reliably replaced at an appropriate time.
(8) The replacement time determination unit may determine the replacement time of the X-ray detector based on a change in an area value of a peak included in the data of the wave height distribution curve obtained by the data obtaining unit by measuring the standard sample.
According to this configuration, the area value of the peak included in the data of the wave height distribution curve obtained by measuring the standard sample in a certain section changes with the deterioration of the X-ray detector. In this case, the degree of change in the area value increases as the X-ray detector is degraded, so that the appropriate replacement timing of the X-ray detector can be determined from the change in the area value.
(9) The replacement time determination unit may determine the replacement time of the X-ray detector by comparing a change amount of an area value within a predetermined section of a peak included in the data of the wave height distribution curve acquired by the data acquisition unit by measuring the standard sample with a threshold value.
According to this configuration, the area value in the constant section of the peak that changes with the deterioration of the X-ray detector is compared with the threshold value, so that the appropriate replacement timing of the X-ray detector can be determined in real time.
(10) The X-ray analysis apparatus may further include a history storage unit that stores a history of area values within a predetermined section of a peak included in the data of the wave height distribution curve acquired by the data acquisition unit by measuring the standard sample. In this case, the replacement time determination unit may determine the replacement time of the X-ray detector based on the history of the area value of the peak stored in the history storage unit.
According to this configuration, a history of the area value in a certain section of the peak that changes with the deterioration of the X-ray detector can be stored, and the replacement timing of the X-ray detector can be predicted from the history. Thus, the preparation for replacement can be performed by confirming the replacement timing of the X-ray detector in advance, and therefore the X-ray detector can be reliably replaced at an appropriate time.
(11) The method for determining the replacement time of an X-ray detector according to the present invention is a method for determining the replacement time of an X-ray detector in an X-ray analysis apparatus including an X-ray source for irradiating an X-ray onto a sample, an X-ray detector for detecting the X-ray after the irradiation onto the sample, and a voltage applying unit for applying a voltage to the X-ray detector, the method for determining the replacement time of the X-ray detector including a data acquisition step and a replacement time determination step. In the data acquisition step, data having a wave height distribution curve of a peak inherent to the sample is acquired from a detection signal from the X-ray detector. In the replacement time determining step, the replacement time of the X-ray detector is determined based on a peak included in the data of the wave height distribution curve acquired in the data acquiring step by measuring the standard sample.
[ Effect of the invention ]
According to the present invention, the appropriate replacement period of the X-ray detector can be determined using: the peak included in the data of the wave height distribution curve obtained by measuring the standard sample with a constant voltage applied to the X-ray detector changes with the deterioration of the X-ray detector.
Drawings
Fig. 1 is a block diagram showing an example of the structure of an X-ray analyzer according to embodiment 1 of the present invention.
Fig. 2 is a diagram showing an example of a wave height distribution curve.
Fig. 3 is a flowchart showing an example of processing performed by the data processing apparatus when the replacement timing of the detector is determined.
Fig. 4 is a flowchart showing an example of processing performed by the data processing device when the replacement timing of the detector is determined in the X-ray analysis device according to embodiment 2 of the present invention.
Fig. 5 is a flowchart showing an example of processing performed by the data processing device when the replacement timing of the detector is determined in the X-ray analysis device according to embodiment 3 of the present invention.
Fig. 6 is a flowchart showing an example of processing performed by the data processing device when the replacement timing of the detector is determined in the X-ray analysis device according to embodiment 4 of the present invention.
Fig. 7 is a flowchart showing an example of processing performed by the data processing device when the replacement timing of the detector is determined in the X-ray analysis device according to embodiment 5 of the present invention.
Fig. 8 is a flowchart showing an example of processing performed by the data processing device when the replacement timing of the detector is determined in the X-ray analysis device according to embodiment 6 of the present invention.
Detailed Description
1. Embodiment 1
Fig. 1 is a block diagram showing an example of the structure of an X-ray analyzer according to embodiment 1 of the present invention. The X-ray analyzer is, for example, a wavelength-dispersive fluorescent X-ray apparatus, and measures fluorescent X-rays generated by irradiating the sample S with X-rays by a spectroscopic crystal (not shown). The X-ray analyzer includes, for example, an X-ray tube 1, an X-ray high voltage circuit 2, a detector 3, a detector high voltage circuit 4, a preamplifier 5, an MCA (Multi Channel Analyzer (multi-channel analyzer)) 6, a control circuit 7, a data processing device 8, a storage unit 9, and the like.
The X-ray tube 1 is an example of an X-ray source that irradiates the sample S with X-rays. The X-ray tube 1 is subjected to high voltage by an X-ray high voltage circuit 2. The X-rays irradiated to the sample S are detected by the detector 3 as fluorescent X-rays generated from the sample S. The detector 3 is an X-ray detector such as a proportional counter tube or a scintillation counter, and a high voltage is applied by a detector high voltage circuit 4. The detector high-voltage circuit 4 constitutes a voltage applying section that applies a voltage to the detector 3.
The detector 3 outputs a detection signal of the X-rays in the form of an electric pulse. The wave height of the electrical pulse is proportional to the energy of the detected X-rays. The electric pulse output from the detector 3 is amplified by a preamplifier 5 and input to the MCA 6. The MCA6 outputs the energy division of the input electric pulse to each channel, thereby generating data of the wave height distribution curve.
The X-ray high-voltage circuit 2, the detector high-voltage circuit 4, and the MCA6 are connected to a data processing device 8 via a control circuit 7. The control circuit 7 controls the X-ray high voltage circuit 2 and the detector high voltage circuit 4, thereby adjusting voltages applied to the X-ray tube 1 and the detector 3. The data of the wave height distribution curve generated in the MCA6 is input from the control circuit 7 to the data processing device 8.
The data processing device 8 is constituted by, for example, a personal computer including a CPU (Central Processing Unit (central processing unit)). The data processing device 8 functions as a data acquisition unit 81, a replacement time determination unit 82, and the like by executing a program by a CPU. The data acquisition unit 81 acquires data of the wave height distribution curve generated by the MCA6 based on the detection signal from the detector 3 via the control circuit 7. The replacement timing determination unit 82 determines the replacement timing of the detector 3 based on the data of the wave height distribution curve acquired by the data acquisition unit 81.
The storage unit 9 is configured by, for example, a hard disk, and stores information (time information) related to the time when the detector 3 is used, data of a high voltage applied to the detector 3 at this time, data of a wave height distribution curve acquired by the data acquisition unit 81, and the like. The time information may be, for example, information of date and time when the detector 3 is used, or may be an integrated value of time when the detector 3 is used.
Fig. 2 is a diagram showing an example of a wave height distribution curve. The wave height distribution curve is expressed by a curve (so-called pulse height distribution curve) in which the horizontal axis is energy and the vertical axis is the count number, which is generated by the MCA6 based on a detection signal from, for example, a proportional counter as the detector 3. As shown in fig. 2, the wave height distribution curve is a curve having a peak unique to the sample S to be measured.
On the low energy side of the wave height distribution curve, electrical noise (so-called amplification noise) is sometimes measured. Further, on the high energy side of the wave height distribution curve, interference rays such as high-order rays may be measured. In order to remove such noise and interference rays, the low energy level LL and the high energy level UL of energy are set, and data of a predetermined interval LL to UL between them is used for analysis. Specifically, a calibration curve is prepared from the area values of peaks in the predetermined sections LL to UL (the area values of the hatched portions in fig. 2), and analysis is performed using the calibration curve.
In the present embodiment, the data acquisition unit 81 acquires the data of the wave height distribution curve by measuring a standard sample having an inherent peak on the wave height distribution curve, and the replacement time determination unit 82 determines the replacement time of the detector 3 based on the peak included in the data of the wave height distribution curve. As the standard sample, for example, silicon, magnesium oxide, calcium carbonate, or the like is used.
The replacement timing of the detector 3 is determined by the following: when a constant voltage is applied to the detector 3, a standard sample is measured, and the peak included in the data of the acquired wave height distribution curve changes with the degradation of the detector 3. Specifically, the position of the peak when a certain voltage is applied to the detector 3 to measure the same standard sample moves to the low energy side (left side in fig. 2) with degradation of the detector 3. By utilizing such characteristics, an appropriate replacement timing of the detector 3 can be determined.
Fig. 3 is a flowchart showing an example of processing performed by the data processing device 8 when the replacement timing of the detector 3 is determined. In the present embodiment, the data acquisition unit 81 acquires data based on the wave height distribution curve of the standard sample by measuring the standard sample periodically or aperiodically, and determines the replacement timing of the detector 3 in real time based on the data. At this time, a high voltage is applied to the detector 3 by the detector high-voltage circuit 4 (step S101), and the control circuit 7 controls the detector high-voltage circuit 4 so that the position of the peak included in the acquired data of the wave height distribution curve reaches a predetermined reference position (steps S102 and S103).
That is, if the position of the peak is not at a predetermined reference position in the horizontal axis direction as shown in fig. 2 (no in step S102), the control circuit 7 controls the detector high-voltage circuit 4, and thereby adjusts the voltage applied to the detector 3 so that the position of the peak reaches the reference position (step S103). In this case, the control circuit 7 constitutes the following voltage adjustment section: the voltage applied to the detector 3 by the detector high-voltage circuit 4 is adjusted so that the position of the peak included in the data of the wave height distribution curve reaches a predetermined reference position.
When adjusting the voltage applied to the detector 3, the detector 3 is degraded, and the voltage value needs to be adjusted to be higher. Therefore, in the present embodiment, the replacement time determination unit 82 determines the replacement time of the detector 3 based on the voltage value adjusted by the control circuit 7, so that the proper replacement time of the detector 3 can be determined. Specifically, the replacement time determination unit 82 compares the voltage value adjusted by the control circuit 7 with a threshold value (step S104), thereby determining the replacement time of the detector 3.
That is, when the voltage value adjusted by the control circuit 7 is equal to or greater than the threshold value (yes in step S104), the replacement time determination unit 82 determines the replacement time of the detector 3 (step S105), and notifies the user of the determination result (step S106). In this way, when the voltage applied to the detector 3 is adjusted so that the peak reaches a predetermined reference position, the voltage value is compared with the threshold value, and thus, the appropriate replacement timing of the detector 3 can be determined in real time. The notification of the determination result may be performed by a display on a display unit (not shown), a voice from a speaker (not shown), or the like.
2. Embodiment 2
Fig. 4 is a flowchart showing an example of processing performed by the data processing device 8 when the replacement timing of the detector 3 is determined in the X-ray analysis device according to embodiment 2 of the present invention. In the present embodiment, the replacement timing of the detector 3 is determined based on the history of the high pressure of the detector stored in the storage unit 9 by measuring the standard sample periodically or aperiodically. At this time, the storage unit 9 functions as a history storage unit that stores a history of the voltage values adjusted by the control circuit 7.
Specifically, when the user performs an operation for confirming the replacement timing of the detector 3 (yes in step S201), the history of the detector high voltage stored in the storage unit 9 is read out (step S202). The detector high voltage read out at this time is a history of the voltage value applied to the detector 3 when the same standard sample is measured.
When the voltage applied to the detector 3 is adjusted so that the position of the peak included in the data of the wave height distribution curve obtained by periodically or aperiodically measuring the standard sample reaches a certain reference position, the voltage value (detector high voltage) stored as a history in the storage unit 9 changes with the degradation of the detector 3. Therefore, in the present embodiment, the replacement time determination unit 82 predicts the replacement time of the detector 3 based on the history of the detector high pressure stored in the storage unit 9 (step S203).
That is, the replacement timing of the detector 3 is predicted from the history of the detector high voltages stored in the storage unit 9 and the time information (the date and time when the detector 3 is used or the integrated value of the time when the detector 3 is used) when each detector high voltage is applied to the detector 3. For example, in the case where the voltage applied to the detector 3 increases in proportion to the use time of the detector 3, the relationship of the proportion can be used to predict the replacement period of the detector 3.
The predicted result of the replacement timing of the detector 3 obtained by the replacement timing determination unit 82 is notified to the user by a display on a display unit (not shown), a voice from a speaker (not shown), or the like (step S204). This allows preparation for replacement to be performed by confirming the replacement timing of the detector 3 in advance, and thus the detector 3 can be reliably replaced at an appropriate timing.
3. Embodiment 3
Fig. 5 is a flowchart showing an example of processing performed by the data processing device 8 when the replacement timing of the detector 3 is determined in the X-ray analysis device according to embodiment 3 of the present invention. In the present embodiment, the data acquisition unit 81 acquires data based on the wave height distribution curve of the standard sample by measuring the standard sample periodically or aperiodically, and determines the replacement timing of the detector 3 in real time based on the data. At this time, a high voltage is applied to the detector 3 by the detector high-voltage circuit 4 (step S301), and the position of the peak included in the acquired data of the wave height distribution curve is confirmed (step S302).
The more the detector 3 is degraded, the greater the degree to which the position of the peak included in the data of the wave height distribution curve changes toward the low energy side (left side in fig. 2). Therefore, in the present embodiment, the replacement timing determination unit 82 determines the replacement timing of the detector 3 from the change in the position of the peak included in the data of the wave height distribution curve, thereby determining the appropriate replacement timing of the detector 3. Specifically, the replacement time determination unit 82 compares the amount of change in the position of the peak included in the data of the wave height distribution curve with a threshold value (step S303), thereby determining the replacement time of the detector 3.
That is, if the amount of change in the position of the peak is equal to or greater than the threshold value (yes in step S303), the replacement time determination unit 82 determines the replacement time of the detector 3 (step S304), and notifies the user of the determination result (step S305). In this way, by comparing the amount of change in the position of the peak that changes with the degradation of the detector 3 with the threshold value, it is possible to determine in real time the proper replacement timing of the detector 3. The notification of the determination result may be performed by a display on a display unit (not shown), a voice from a speaker (not shown), or the like.
4. Embodiment 4
Fig. 6 is a flowchart showing an example of processing performed by the data processing device 8 when the replacement timing of the detector 3 is determined in the X-ray analysis device according to embodiment 4 of the present invention. In the present embodiment, the replacement timing of the detector 3 is determined from the history of the positions of the peaks included in the data of the wave height distribution curve stored in the storage unit 9 by periodically or aperiodically measuring the standard sample. At this time, the storage unit 9 functions as a history storage unit that stores a history of the positions of peaks included in the data of the wave height distribution curve.
Specifically, when the user performs an operation for confirming the replacement timing of the detector 3 (yes in step S401), the history of the position of the peak included in the data of the wave height distribution curve stored in the storage unit 9 is read (step S402). The position of the peak read out at this time is a history of the position of the peak included in the data of the wave height distribution curve obtained when the same standard sample is measured.
The position of the peak included in the data of the wave height distribution curve obtained by periodically or aperiodically measuring the standard sample changes with the degradation of the detector 3. Therefore, in the present embodiment, the history of the position of the peak that changes with the degradation of the detector 3 is stored in the storage unit 9, and the replacement time determination unit 82 predicts the replacement time of the detector 3 based on the history (step S403).
That is, the replacement timing of the detector 3 is predicted from the history of the position of the peak included in the data of the wave height distribution curve stored in the storage unit 9 and the time information (the date and time when the detector 3 is used or the integrated value of the time when the detector 3 is used) when the data of each wave height distribution curve is acquired. For example, when the amount of change in the position of the peak included in the data of the wave height distribution curve increases in proportion to the time of use of the detector 3, the relationship of the ratio can be used to predict the replacement timing of the detector 3.
The predicted result of the replacement timing of the detector 3 obtained by the replacement timing determination unit 82 is notified to the user by a display on a display unit (not shown), a voice from a speaker (not shown), or the like (step S404). This allows preparation for replacement to be performed by confirming the replacement timing of the detector 3 in advance, and thus the detector 3 can be reliably replaced at an appropriate timing.
5. Embodiment 5
Fig. 7 is a flowchart showing an example of processing performed by the data processing device 8 when the replacement timing of the detector 3 is determined in the X-ray analysis device according to embodiment 5 of the present invention. In the present embodiment, the data acquisition unit 81 acquires data based on the wave height distribution curve of the standard sample by measuring the standard sample periodically or aperiodically, and determines the replacement timing of the detector 3 in real time based on the data. At this time, the detector 3 is subjected to high voltage by the detector high-voltage circuit 4 (step S501), and the area values (the area values of the hatched portions in fig. 2) within the predetermined sections LL to UL of the peaks included in the acquired data of the wave height distribution curve are checked (step S502).
The more the detector 3 is degraded, the greater the degree to which the position of the peak included in the data of the wave height distribution curve changes toward the low energy side (left side in fig. 2). With such a change in the position of the peak, the area value of the peak in the constant section LL to UL also changes. Therefore, in the present embodiment, the replacement timing determination unit 82 determines the replacement timing of the detector 3 from the change in the area value within the constant sections LL to UL of the peaks included in the data of the wave height distribution curve, thereby determining the appropriate replacement timing of the detector 3. Specifically, the replacement time determination unit 82 compares the amount of change in the area value within the constant sections LL to UL of the peaks included in the data of the wave height distribution curve with a threshold value (step S503), thereby determining the replacement time of the detector 3.
That is, if the amount of change in the area value of the peak in the fixed section LL to UL is equal to or greater than the threshold value (yes in step S503), the replacement time determination unit 82 determines the replacement time of the detector 3 (step S504), and notifies the user of the determination result (step S505). In this way, by comparing the amount of change in the area value within the constant sections LL to UL of the peak that changes with the degradation of the detector 3 with the threshold value, it is possible to determine in real time the proper replacement timing of the detector 3. The notification of the determination result may be performed by a display on a display unit (not shown), a voice from a speaker (not shown), or the like.
6. Embodiment 6
Fig. 8 is a flowchart showing an example of processing performed by the data processing device 8 when the replacement timing of the detector 3 is determined in the X-ray analysis device according to embodiment 6 of the present invention. In the present embodiment, the replacement timing of the detector 3 is determined based on the history of the area values (the area values of the hatched portions in fig. 2) within the certain sections LL to UL of the peaks included in the data of the wave height distribution curve stored in the storage unit 9 by periodically or aperiodically measuring the standard sample. At this time, the storage unit 9 functions as a history storage unit that stores a history of area values within the constant sections LL to UL of the peaks included in the data of the wave height distribution curve.
Specifically, when the user performs an operation for confirming the replacement timing of the detector 3 (yes in step S601), the history of the area values within the constant sections LL to UL of the peaks included in the data of the wave height distribution curve stored in the storage unit 9 is read (step S602). The area value of the peak read out at this time is a history of the area value of the peak included in the data of the wave height distribution curve obtained when the same standard sample is measured.
The area values within a certain section LL to UL of the peak included in the data of the wave height distribution curve obtained by periodically or aperiodically measuring the standard sample change with the degradation of the detector 3. Therefore, in the present embodiment, the history of the area values in the constant sections LL to UL of the peaks that change with the degradation of the detector 3 is stored in the storage unit 9, and the replacement time determination unit 82 predicts the replacement time of the detector 3 based on the history (step S603).
That is, the replacement timing of the detector 3 is predicted from the history of the area values within the constant sections LL to UL of the peaks included in the data of the wave height distribution curve stored in the storage unit 9 and the time information (the date and time when the detector 3 is used or the integrated value of the time when the detector 3 is used) when the data of each wave height distribution curve is acquired. For example, when the amount of change in the area value within a certain section LL to UL of the peak included in the data of the wave height distribution curve increases in proportion to the time of use of the detector 3, the replacement timing of the detector 3 can be predicted using the relationship of the ratio.
The predicted result of the replacement timing of the detector 3 obtained by the replacement timing determination unit 82 is notified to the user by a display on a display unit (not shown), a voice from a speaker (not shown), or the like (step S604). This allows preparation for replacement to be performed by confirming the replacement timing of the detector 3 in advance, and thus the detector 3 can be reliably replaced at an appropriate timing.
7. Modification examples
In the above embodiments, the following configuration is explained: in the X-ray analysis apparatus, a data acquisition step of acquiring data having a wave height distribution curve unique to a sample based on a detection signal from the detector 3, a replacement time determination step of determining a replacement time of the detector 3 based on a peak included in the data of the wave height distribution curve acquired in the data acquisition step by measuring a standard sample, and a voltage adjustment step of adjusting a voltage applied to the detector 3 by the detector high-voltage circuit 4 so that a position of the peak included in the data of the wave height distribution curve acquired in the data acquisition step by measuring the standard sample reaches a predetermined reference position are automatically performed, respectively. However, the present invention is not limited to this configuration, and at least 1 of the data acquisition step, the replacement time determination step, and the voltage adjustment step may be performed manually by a user.
The present invention is not limited to the wavelength dispersive fluorescent X-ray device, and can be applied to other X-ray analysis devices such as an X-ray diffraction device.
Symbol description
1X ray tube
2X ray high-voltage circuit
3. Detector for detecting a target object
4. Detector high-voltage circuit
5. Pre-amplifier
6 MCA
7. Control circuit
8. Data processing apparatus
9. Storage unit
81. Data acquisition unit
82. And a replacement time judging unit.

Claims (4)

1. An X-ray analysis apparatus comprising:
an X-ray source for irradiating X-rays onto a sample;
an X-ray detector that detects X-rays after the sample is irradiated;
a voltage applying unit that applies a voltage to the X-ray detector;
a data acquisition unit that acquires data having a wave height distribution curve of a peak inherent to a sample from a detection signal from the X-ray detector; and
a replacement time determination unit that determines a replacement time of the X-ray detector based on a peak included in the data of the wave height distribution curve acquired by the data acquisition unit by measuring the standard sample,
the replacement time determination unit determines the replacement time of the X-ray detector based on a change in an area value of a peak included in the data of the wave height distribution curve obtained by the data acquisition unit by measuring the standard sample.
2. The X-ray analysis apparatus according to claim 1, wherein,
the replacement time determination unit determines the replacement time of the X-ray detector by comparing the amount of change in the area value of the peak included in the data of the wave height distribution curve acquired by the data acquisition unit by measuring the standard sample with a threshold value.
3. The X-ray analysis apparatus according to claim 1, wherein,
further comprising a history storage unit for storing a history of area values within a predetermined section of a peak included in the data of the wave height distribution curve acquired by the data acquisition unit by measuring the standard sample,
the replacement time determination unit determines a replacement time of the X-ray detector based on the history of the area value of the peak stored in the history storage unit.
4. A method for determining a replacement time of an X-ray detector in an X-ray analysis apparatus including an X-ray source for irradiating an X-ray onto a sample, an X-ray detector for detecting the X-ray after the X-ray is irradiated onto the sample, and a voltage applying unit for applying a voltage to the X-ray detector, the method comprising:
a data acquisition step of acquiring data having a wave height distribution curve of a peak inherent to a sample from a detection signal from the X-ray detector; and
a replacement time determination step of determining a replacement time of the X-ray detector based on a peak included in the data of the wave height distribution curve acquired in the data acquisition step by measuring the standard sample,
in the replacement time determining step, the replacement time of the X-ray detector is determined based on a change in an area value of a peak included in the data of the wave height distribution curve acquired in the data acquiring step by measuring the standard sample in a certain section.
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