JP6863267B2 - X-ray analyzer and abnormality detection method - Google Patents

Description

The present invention relates to an X-ray analyzer that performs analysis by detecting X-rays generated from a sample, and a method for detecting an abnormality in the X-ray analyzer.

As an example of an X-ray analyzer, by irradiating a sample with X-rays, X-rays (fluorescent X-rays) peculiar to the elements contained in the sample are generated, and the components in the sample are analyzed by detecting the X-rays. X-ray fluorescence analyzers are known (see, for example, Patent Document 1 below). The X-rays generated from the sample are separated by a spectroscope and then detected by a detector.

Some X-ray analyzers of this type can simultaneously analyze a plurality of types of elements by providing a spectroscope and a detector for each element to be analyzed (simultaneous fluorescent X-rays). Analysis equipment). Specifically, a detection unit is configured by integrally incorporating a spectroscope and a detector, and a plurality of detection units are arranged around a sample installation position. As a result, a plurality of detection units having substantially the same structure are installed close to each other.

The detector has, for example, a configuration in which a thin wire is inserted in a container filled with gas, and a high voltage is applied to the thin wire at the time of analysis. As a result, when X-rays from the sample are incident on the container, the gas in the container is ionized, and the current generated by the ionization is output from the detector as an output signal. The detector of each detection unit includes a container having a different shape depending on the type of the element to be analyzed, and the type of gas sealed in the container also differs depending on the type of the element to be analyzed. Therefore, the value of the high voltage applied to the detector is different for each detector.

On the other hand, the electric circuit to which each detector is connected has the same process of applying a high voltage to each detector to detect the current generated by ionization, so that the same electric circuit may be used. There are many. That is, the same electric circuit, which is difficult to distinguish from the outside, is detachably connected to each detection unit.

Jitsukaisho 60-49455 Gazette

When performing maintenance of the X-ray analyzer or replacing parts, the electric circuit may be removed from each detection unit and then reattached. At this time, if the electric circuits attached to each detection unit are exactly the same as described above, there is a possibility that the electric circuits not corresponding to each detection unit may be erroneously connected. In this case, when an unnecessarily high voltage is applied to the detector, a discharge may occur and the detector may be damaged.

Further, not only the electric circuit not corresponding to each detection unit may be erroneously connected as described above, but also the setting of the voltage applied to the detector may be erroneous. Even in such a case, a voltage higher than necessary may be applied to the detector, and the detector may be damaged.

The present invention has been made in view of the above circumstances, and an object of the present invention is to provide an X-ray analyzer and an abnormality detection method capable of preventing an unnecessarily high voltage from being applied to a detector. ..

(1) The X-ray analyzer according to the present invention is an X-ray analyzer that analyzes by detecting X-rays generated from a sample, and includes a plurality of detectors, a voltage application unit, and an abnormality detection processing unit. To be equipped. The plurality of detectors detect X-rays. The voltage application unit applies a voltage to the plurality of detectors. The abnormality detection processing unit applies X-rays generated from the sample to the plurality of detectors from the voltage application unit in a state where the samples are not detected by the plurality of detectors (for example, a state in which the sample is not irradiated with excited X-rays). The voltage is gradually increased, and the measured value based on the detection signals from the plurality of detectors at that time is compared with the threshold value to detect the abnormality.

According to such a configuration, the voltage applied to the plurality of detectors is gradually increased in a state where the X-rays generated from the sample are not detected by the plurality of detectors, based on the detection signals from the plurality of detectors. It is possible to detect an abnormality. In a state where X-rays generated from a sample are not detected by a plurality of detectors, normally, even if the voltage applied to the detectors is gradually increased, the detection signal from the detectors hardly changes. Nevertheless, when the measured value based on the detection signal from the detector exceeds a predetermined threshold value as the applied voltage to the detector rises, it is possible to detect that an abnormality has occurred. This makes it possible to prevent an unnecessarily high voltage from being applied to the detector.

(2) The X-ray analyzer may further include a voltage stop processing unit. When an abnormality is detected by the abnormality detection processing unit, the voltage stop processing unit stops application of a voltage from the voltage application unit to a detector whose measured value exceeds a threshold value.

According to such a configuration, when an abnormality is detected by the abnormality detection processing unit, at least the application of the voltage to the detector whose measured value exceeds the threshold value is stopped, so that it is more than necessary for the detector. It is possible to reliably prevent a high voltage from being applied to the surface.

(3) When an abnormality is detected by the abnormality detection processing unit, the voltage stop processing unit may stop only the application of the voltage from the voltage application unit to the detector whose measured value exceeds the threshold value. preferable. In this case, the abnormality detection processing unit gradually increases the voltage applied from the voltage application unit to the other detector even after the application of the voltage from the voltage application unit to any of the detectors is stopped. Therefore, the detection of the abnormality may be continued.

According to such a configuration, when an abnormality is detected by the abnormality detection processing unit, only the application of the voltage to the detector whose measured value exceeds the threshold value is stopped, and the applied voltage to the other detectors continues gradually. By increasing to, the detection of abnormality is continued. This makes it possible to continuously detect abnormalities related to other detectors, so that abnormalities can be detected more reliably.

(4) The X-ray analyzer may further include a notification processing unit. When an abnormality is detected by the abnormality detection processing unit, the notification processing unit notifies that fact.

According to such a configuration, when an abnormality is detected by the abnormality detection processing unit, the fact is notified, so that the user who confirms the notification can take appropriate measures. This makes it possible to more reliably prevent an unnecessarily high voltage from being applied to the detector.

(5) The voltage application unit may have a connection unit that can be individually attached to and detached from the plurality of detectors.

According to such a configuration, when a connection portion not corresponding to the detector is erroneously connected, an abnormality can be detected based on the detection signal from the detector. Therefore, it is possible to prevent an unnecessarily high voltage from being applied to the detector due to the connection portion being erroneously connected.

(6) The X-ray analyzer may further include a housing, an opening / closing door, and an opening / closing sensor. The housing accommodates the plurality of detectors, and a space for attaching / detaching the connection portion to / from the plurality of detectors is formed inside. The opening / closing door is provided in the housing and opens / closes the space. The open / close sensor detects the opening / closing of the opening / closing door. In this case, the abnormality detection processing unit gradually increases the voltage applied to the plurality of detectors from the voltage application unit only when the detector high voltage is applied immediately after the opening / closing sensor detects the opening / closing of the opening / closing door. Processing may be performed.

According to such a configuration, when there is no possibility that the connection portion is attached or detached, the time-consuming process of gradually increasing the voltage applied to the detector can be omitted.

(7) The abnormality detection method according to the present invention is an abnormality detection method of an X-ray analyzer that analyzes by detecting X-rays generated from a sample with a plurality of detectors to which a voltage is applied from a voltage application unit. , Includes anomaly detection steps. In the abnormality detection step, the voltage applied to the plurality of detectors from the voltage application unit is gradually increased in a state where the X-rays generated from the sample are not detected by the plurality of detectors, and the plurality of detections at that time are performed. Anomalies are detected by comparing the measured value based on the detection signal from the device with the threshold value.

(8) The abnormality detection method may further include a voltage stop step. In the voltage stop step, when an abnormality is detected by the abnormality detection step, the application of the voltage from the voltage application unit to the detector whose measured value exceeds the threshold value is stopped.

(9) In the voltage stop step, when an abnormality is detected by the abnormality detection step, it is preferable to stop the application of the voltage from the voltage application unit only to the detector whose measured value exceeds the threshold value. In this case, in the abnormality detection step, even after the application of the voltage from the voltage application unit to any of the detectors is stopped, the voltage applied from the voltage application unit to the other detector is gradually increased. Therefore, the detection of the abnormality may be continued.

(10) The abnormality detection method may further include a notification step. In the notification step, when an abnormality is detected by the abnormality detection step, a notification to that effect is given.

According to the present invention, when the measured value based on the detection signal from the detector exceeds a predetermined threshold value as the voltage applied to the detector rises, it is possible to detect that an abnormality has occurred, which is more than necessary. It is possible to prevent a high voltage from being applied to the detector.

It is the schematic which showed the structural example of the X-ray analyzer which concerns on one Embodiment of this invention. It is a block diagram which showed an example of the electric structure of the X-ray analyzer. It is a flowchart which showed the specific example of the abnormality detection performed by the abnormality detection processing unit.

1. 1. Overall Configuration of X-ray Analyzer FIG. 1 is a schematic view showing a configuration example of the X-ray analyzer 1 according to an embodiment of the present invention. This X-ray analyzer 1 generates X-rays (fluorescent X-rays) from the sample S by irradiating the sample S installed at the sample installation position with X-rays, and detects the X-rays for analysis. It is a fluorescent X-ray analyzer to perform. The X-ray analyzer 1 is provided with an X-ray source 2, a detection unit 3, an electric circuit 4, and the like.

The X-ray source 2 is composed of, for example, an X-ray tube. This type of X-ray source 2 includes, for example, filaments and targets (neither shown) that are spaced apart from each other. The target can be formed of, for example, Cu, Cr, Mo, Al, Ag or Au. Electric power is supplied to the X-ray source 2, and a high voltage is applied between the filament and the target. As a result, thermions are emitted from the filament toward the target, and the thermions collide with the target to generate X-rays. The X-rays generated from the X-ray source 2 irradiate the sample S.

From the sample S irradiated with X-rays, X-rays peculiar to the elements contained in the sample S are generated as fluorescent X-rays. The X-rays generated from the sample S are detected by the detection unit 3, and the detection signal is input to the electric circuit 4. The detection unit 3 is connected to the electric circuit 4 via the connection unit 5. The connection portion 5 is composed of, for example, a detachable connector, and connects the detection unit 3 and the electric circuit 4 in a detachable manner.

The detection unit 3 is configured as one component in which the spectroscope 31 and the detector 32 are integrally incorporated. The spectroscope 31 is composed of, for example, a spectroscopic crystal, and disperses the X-rays generated from the sample S. Then, the intensity of a specific wavelength can be measured by detecting the dispersed X-rays with the detector 32.

The detector 32 is composed of, for example, a proportional counter or a scintillation counter. The detector 32 has, for example, a configuration in which a thin wire is inserted in a container filled with gas, and a high voltage is applied to the thin wire at the time of analysis. As a result, when the X-ray from the sample S is incident on the container, the gas in the container is ionized, and the current generated by the ionization is output from the detector 32 as an output signal.

The electric circuit 4 includes a high voltage generator 41, an amplifier 42, a wave height analyzer 43, a counter 44, and the like. The high voltage generator 41, together with the connection unit 5, constitutes a voltage application unit that applies a high voltage to the detector 32. The amplifier 42 amplifies the output signal from the detector 32 and inputs it to the pulse height analyzer 43. The wave height analyzer 43 measures the wave height of the output signal (output pulse) from the detector 32 input from the amplifier 42. The counter 44 counts an output signal (output pulse) exceeding a predetermined crest value in the crest analyzer 43.

The X-ray analyzer 1 includes a hollow housing 12 having an internal space 11. The internal space 11 of the housing 12 houses an X-ray source 2, a detection unit 3, an electric circuit 4, and a connection portion 5. The housing 12 is provided with an opening / closing door 13 for opening / closing the internal space 11. Therefore, by opening the opening / closing door 13 to open the internal space 11, it is possible to attach / detach the connecting portion 5 to / from the detector 32 in the internal space 11.

2. Electrical configuration of the X-ray analyzer FIG. 2 is a block diagram showing an example of the electrical configuration of the X-ray analyzer 1. The X-ray analyzer 1 is provided with a control unit 6, an open / close sensor 7, a display unit 8, and the like, in addition to the detection unit 3, the electric circuit 4, and the connection unit 5 described above. The control unit 6 has a configuration including, for example, a CPU (Central Processing Unit), and functions as an abnormality detection processing unit 61, a voltage stop processing unit 62, a notification processing unit 63, and the like when the CPU executes a program.

As shown in FIG. 2, the X-ray analyzer 1 according to the present embodiment is provided with a plurality of detection units 3. The detector 32 provided in each detection unit 3 is for detecting a different element, has a container having a different shape depending on the type of the element to be analyzed, and has a different type in the container. Gas is sealed.

Each detection unit 3 has substantially the same structure, and is arranged around the installation position of the sample S. As a result, the plurality of detection units 3 are installed close to each other. At the time of analysis, by detecting X-rays peculiar to different elements in each detection unit 3, it is possible to analyze a plurality of types of elements at the same time.

An electric circuit 4 is connected to each detection unit 3 via a connection unit 5. That is, the X-ray analyzer 1 according to the present embodiment is provided with a plurality of sets of detection units 3 and electric circuits 4 connected to each other via a connection unit 5. Each connection portion 5 can be individually attached to and detached from each detection unit 3 and each electric circuit 4. As described above, each electric circuit 4 includes a high voltage generator 41, an amplifier 42, a wave height analyzer 43, a counter 44, and the like, and each has the same circuit configuration. Therefore, it is difficult to distinguish each electric circuit 4 from the appearance, and there is a possibility that different sets of detection units 3 and electric circuits 4 that do not correspond to each other are erroneously connected via the detachable connecting portion 5.

Therefore, in the present embodiment, the control of the control unit 6 is configured to prevent the electric circuit 4 that does not correspond to each detection unit 3 from being erroneously connected. Specifically, the abnormality detection processing unit 61 detects an abnormality based on the detection signal from the detector 32 of each detection unit 3. The "abnormality" includes a case where an electric circuit 4 not corresponding to each detection unit 3 is erroneously connected, a case where the voltage applied from the high voltage generator 41 to each detector 32 is set incorrectly, and the like. As described above, it is assumed that each detector 32 includes various states in which an unexpected voltage is applied.

The abnormality detection processing unit 61 applies a voltage applied from the high voltage generator 41 of each electric circuit 4 to the detector 32 of each detection unit 3 in a state where the sample S is not installed at the sample installation position of the X-ray analyzer 1. Gradually raise. At this time, the voltage applied to each detector 32 is controlled to increase continuously or stepwise until it reaches the voltage (set voltage) to be applied when the detector 32 is used.

When the abnormality detection processing unit 61 detects an abnormality, the sample S is not installed at the sample installation position. Therefore, if there is no abnormality, no detection signal is output from each detector 32, or the output is output. Even if it is done, it is very small. However, for example, when the electric circuit 4 which does not correspond to each detection unit 3 is erroneously connected, or when the setting of the voltage applied to each detector 32 is erroneous, the detection unit 32 is connected to any of the detectors 32. When an unexpected voltage is applied, the detector 32 may output a detection signal derived from the discharge.

Therefore, the abnormality detection processing unit 61 compares the measured value based on the detection signal from each detector 32 when the voltage applied to each detector 32 is gradually increased with the threshold value to obtain the above-mentioned abnormality. Is detected. That is, when the measured value based on the detection signal from any of the detectors 32 exceeds a predetermined threshold value, it can be determined that an abnormality has occurred in the detector 32. As the measured value, a counting rate (cps) can be exemplified, but the measured value is not limited to this.

The abnormality detection by the abnormality detection processing unit 61 should be performed at the timing of applying the detector high voltage, but in the present embodiment, the abnormality detection is started based on the presence / absence of opening / closing of the opening / closing door 13. There is. The X-ray analyzer 1 is provided with an opening / closing sensor 7 that mechanically or optically detects the opening / closing of the opening / closing door 13, for example. When the abnormality detection processing unit 61 detects the open state or the closed state of the open / close door 13 by the open / close sensor 7, the high voltage generator 41 of each electric circuit 4 to each detection unit 3 only when the detector high voltage is applied immediately after that. The process of gradually increasing the voltage applied to the detector 32 of the above is started. As a result, when there is no possibility that the connection portion 5 is attached or detached, the time-consuming process of gradually increasing the voltage applied to the detector can be omitted.

When an abnormality is detected by the abnormality detection processing unit 61, the voltage stop processing unit 62 stops the application of voltage to at least the detector 32 (detector 32 whose measured value exceeds the threshold value) in which the abnormality is detected. That is, the application of the voltage to all the detectors 32 may be stopped, but the application of the voltage to the detector 32 in which the abnormality is detected may be stopped, and the application of the voltage to the other detectors 32 may be continued. Good.

When the abnormality detection processing unit 61 detects an abnormality, the notification processing unit 63 notifies the user to that effect. In the present embodiment, the notification processing unit 63 controls the display on the display unit 8 to notify the user of the abnormality. The display unit 8 is composed of, for example, a liquid crystal display. However, the display is not limited to the display unit 8, and the abnormality may be notified by other means such as sound.

3. 3. Specific Example of Abnormality Detection FIG. 3 is a flowchart showing a specific example of abnormality detection performed by the abnormality detection processing unit 61. In the present embodiment, when the opening / closing sensor 7 detects the opening / closing of the opening / closing door 13 (Yes in step S101), the abnormality detection processing unit 61 starts the abnormality detection (steps S102, S103, S106: abnormality detection step). To.

Specifically, the voltage applied to each detector 32 is gradually increased (step S102), and the measured value (for example, counting rate) based on the detection signal from each detector 32 is compared with the threshold value (for example, 10 cps). (Step S103). In the process, if the measured value based on the detection signal from any of the detectors 32 exceeds the threshold value (Yes in step S103), only the application of the voltage to the detector 32 is stopped (step S104: Voltage stop step). Further, the fact that the abnormality has been detected is notified to the user by the display of the display unit 8 (step S105: notification step). At this time, information identifying the detector 32 in which the abnormality is detected may be notified.

As described above, even when the application of the voltage to any of the detectors 32 is stopped, the voltage is applied to the other detectors 32 until the abnormality detection process is completed (until the result becomes Yes in step S106). By gradually increasing the voltage to be applied (step S102), the detection of abnormality is continued. Then, when the measured value based on the detection signal from the other detector 32 exceeds the threshold value (Yes in step S103), the voltage stop step (step S104) and the notification step (step S105) are performed for the detector 32. Will be done.

4. Action effect (1) In the present embodiment, the voltage applied to the plurality of detectors 32 is gradually increased in a state where the X-rays generated from the sample S are not detected by the plurality of detectors 32 (step S102). The abnormality can be detected based on the detection signal from the detector 32 of the above (step S103). In the state where the X-rays generated from the sample S are not detected by the plurality of detectors 32, normally, even if the voltage applied to the detectors 32 is gradually increased, the detection signal from the detectors 32 hardly changes. .. Nevertheless, if the measured value based on the detection signal from the detector 32 exceeds a predetermined threshold value as the applied voltage to the detector 32 rises (Yes in step S103), an abnormality has occurred. Can be detected. This makes it possible to prevent an unnecessarily high voltage from being applied to the detector 32.

(2) Further, in the present embodiment, when an abnormality is detected by the abnormality detection processing unit 61 (Yes in step S103), the application of the voltage to the detector 32 whose measured value exceeds the threshold value is stopped. Therefore (step S104), it is possible to reliably prevent the detector 32 from being applied with an unnecessarily high voltage.

(3) In particular, in the present embodiment, when an abnormality is detected by the abnormality detection processing unit 61 (Yes in step S103), only the application of the voltage to the detector 32 whose measured value exceeds the threshold value is stopped (Yes). In step S104), the voltage applied to the other detector 32 is continuously gradually increased (step S102), so that the abnormality detection is continued. As a result, it becomes possible to continuously detect an abnormality related to the other detector 32, so that the abnormality can be detected more reliably.

(4) Further, in the present embodiment, when an abnormality is detected by the abnormality detection processing unit 61 (Yes in step S103), that fact is notified (step S105), so that the user who confirmed the notification Appropriate measures can be taken. As a result, it is possible to more reliably prevent an unnecessarily high voltage from being applied to the detector 32.

(5) In the present embodiment, each electric circuit 4 is connected to a plurality of detectors 32 via individually detachable connection portions 5. Therefore, when the connection unit 5 that does not correspond to the detector 32 is erroneously connected, the abnormality can be detected based on the detection signal from the detector 32. Therefore, it is possible to prevent an unnecessarily high voltage from being applied to the detector 32 due to the connection portion 5 being erroneously connected.

(6) Further, in the present embodiment, when the opening / closing door 13 is not opened / closed (No in step S101), the abnormality detection by the abnormality detection processing unit 61 is omitted. When the opening / closing door 13 is opened / closed, there is a possibility that the connecting portion 5 is attached / detached to / from the detector 32 housed in the housing 12. Therefore, when the opening / closing door 13 is opened / closed, it is necessary for the abnormality detection processing unit 61 to detect the abnormality, but if there is no possibility that the connection unit 5 is attached / detached, it is not necessary to waste time.

5. Deformation example Abnormality detection by the abnormality detection processing unit 61 may be performed in a state where the X-rays generated from the sample S are not detected by each detector 32, and is not limited to the state where the sample S is not installed at the sample installation position. Absent. That is, the abnormality detection may be performed in a state where the sample S installed at the sample installation position is not irradiated with X-rays from the X-ray source 2.

The timing at which the abnormality detection processing unit 61 starts abnormality detection is not limited to the case where the opening / closing door 13 is opened / closed. For example, it is possible to start the abnormality detection at any other timing, such as when the power of the X-ray analyzer 1 is turned on.

The present invention can be applied not only to a wavelength dispersive fluorescent X-ray analyzer but also to other X-ray analyzers such as an energy dispersive fluorescent X-ray analyzer.

1 X-ray analyzer 2 X-ray source 3 Detection unit 4 Electric circuit 5 Connection 6 Control 7 Open / close sensor 8 Display 11 Internal space 12 Housing 13 Open / close door 31 Spectrometer 32 Detector 41 High voltage generator 42 Amplifier 43 Wave height analyzer 44 Counter 61 Abnormality detection processing unit 62 Voltage stop processing unit 63 Notification processing unit

Claims (10)

An X-ray analyzer that performs analysis by detecting X-rays generated from a sample.
Multiple detectors that detect X-rays and
A voltage application unit that applies voltage to the plurality of detectors,
In a state where the X-rays generated from the sample are not detected by the plurality of detectors, the voltage applied to the plurality of detectors from the voltage application unit is gradually increased, and the detection signals from the plurality of detectors at that time are obtained. An X-ray analyzer comprising an abnormality detection processing unit that detects an abnormality by comparing a measured value based on the threshold value with a threshold value. When an abnormality is detected by the abnormality detection processing unit, a voltage stop processing unit for stopping the application of voltage from the voltage application unit to a detector whose measured value exceeds a threshold value is further provided. The X-ray analyzer according to claim 1. When an abnormality is detected by the abnormality detection processing unit, the voltage stop processing unit stops only the application of the voltage from the voltage application unit to the detector whose measured value exceeds the threshold value.
The abnormality detection processing unit gradually increases the voltage applied from the voltage application unit to the other detector even after the application of the voltage from the voltage application unit to any of the detectors is stopped. The X-ray analyzer according to claim 2, wherein the detection of an abnormality is continued. The X-ray analyzer according to any one of claims 1 to 3, further comprising a notification processing unit that notifies the abnormality when an abnormality is detected by the abnormality detection processing unit. The X-ray analyzer according to any one of claims 1 to 4, wherein the voltage application unit has a connection unit that can be individually attached to and detached from the plurality of detectors. A housing in which the plurality of detectors are housed and a space for attaching / detaching the connection portion to / from the plurality of detectors is formed inside.
An opening / closing door provided in the housing for opening / closing the space,
It is further equipped with an open / close sensor that detects the open / close of the open / close door.
When the opening / closing sensor detects the opening / closing of the opening / closing door, the abnormality detection processing unit gradually applies a voltage applied to the plurality of detectors from the voltage application unit only when a high voltage is applied to the detector immediately after that. The X-ray analyzer according to claim 5, wherein the raising process is performed. It is an abnormality detection method of an X-ray analyzer that analyzes by detecting X-rays generated from a sample with a plurality of detectors to which a voltage is applied from a voltage application unit.
In a state where the X-rays generated from the sample are not detected by the plurality of detectors, the voltage applied to the plurality of detectors from the voltage application unit is gradually increased, and the detection signals from the plurality of detectors at that time are obtained. An anomaly detection method comprising an anomaly detection step of detecting an anomaly by comparing a measured value based on the threshold value with a threshold value. The claim is further comprising a voltage stop step of stopping the application of a voltage from the voltage application unit to a detector whose measured value exceeds a threshold value when an abnormality is detected by the abnormality detection step. The abnormality detection method according to 7. In the voltage stop step, when an abnormality is detected by the abnormality detection step, the application of the voltage from the voltage application unit to only the detector whose measured value exceeds the threshold value is stopped.
In the abnormality detection step, even after the application of the voltage from the voltage application unit to any of the detectors is stopped, the voltage applied from the voltage application unit to the other detector is gradually increased to cause an abnormality. The abnormality detection method according to claim 8, wherein the detection of the above is continued. The abnormality detection method according to any one of claims 7 to 9, further comprising a notification step for notifying the fact when an abnormality is detected by the abnormality detection step.

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