JPH11108863A - Fluorescent x-ray analyzer - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a fluorescent X-ray analyser reduced in the number of sample stands to be prepared and simple in structure as compared with a conventional analyser. SOLUTION: An operator designates the part where 'analysis of solid sample' is displayed on the display of a control apparatus 20 because a solid sample is set to a sample holder by a mouse. When this designation is performed, a switch control circuit 18 receiving a cover close signal from a reset circuit 19 turns a first exhaust switch 15 ON. Further, the operator turns the solid sample analyzing button 23 of an operation panel 22 ON. When the solid sample analyzing button 23 is turned ON, the switch control circuit 21 receiving the cover close signal from the reset circuit 19 turns a second exhaust switch 16 ON. When the exhaust switch 16 is turned ON, an exhaust apparatus power supply 17 is closed to be connected to an exhaust apparatus 14 to start the exhaustion of a sample chamber 4.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to an X-ray fluorescence analyzer.

[0002]

2. Description of the Related Art An X-ray fluorescence analyzer irradiates a sample with X-rays, and emits X-rays generated from the sample by the X-ray irradiation.
It is a device that detects a line and obtains the elements constituting the sample and their amounts from the detected fluorescent X-rays.

In this X-ray fluorescence spectrometer, when a solid sample is analyzed, the sample chamber is evacuated by a rotary pump in order to increase the analysis accuracy. On the other hand, if the sample chamber in which the liquid sample is disposed is evacuated, the liquid sample is discharged and the rotary pump is damaged, so that the sample chamber is not evacuated during the analysis of the liquid sample.

As described above, the sample chamber is evacuated during the analysis of a solid sample, and the sample chamber is not evacuated during the analysis of a liquid sample. However, the exhaust of the sample chamber is automatically performed based on the shape of the sample stage on which the sample holder is mounted. It is done on a regular basis. To explain this in detail, a conventional X-ray fluorescence spectrometer has, for example, a sample stage for solid sample analysis having an exhaust protrusion and to which a plurality of sample holders can be attached, and the protrusion. However, a sample stage for liquid sample analysis to which a plurality of sample holders can be attached is prepared.
Then, when the sample stage for solid sample analysis is attached to the sample stage receiver, the evacuation microswitch is turned on by the projection provided on the sample stage, and the sample chamber is exhausted. Further, when the sample stage for liquid sample analysis is mounted on the sample stage receiver, the microswitch is turned off and the sample chamber is not exhausted because the projection is not provided on the sample stage. The sample stage receiver is configured to rotate, and by this rotation, each sample holder attached to the sample stage is sequentially arranged at the X-ray irradiation position.

In a conventional X-ray fluorescence spectrometer, a sample stage for analyzing a large sample is prepared separately from the above-mentioned sample stage. This sample stage holds one large solid sample.
The sample stage for large-sized sample analysis has the projection for exhaust. Therefore, when the sample stage is mounted on the sample stage receiver, the sample chamber is evacuated.

The sample stage for analyzing a large sample has a rotation-preventing projection for preventing the sample stage receiver from rotating. When the sample stage is attached to the sample stage support, the rotation preventing microswitch is turned on by the rotation preventing projection, and the rotation of the sample stage support is inhibited. This is because, when the sample stage on which a large sample with a heavy weight is placed is rotated, the rotation drive unit of the sample stage receiver is damaged.

[0007]

As described above, in the conventional X-ray fluorescence spectrometer, the sample chamber for solid sample analysis and the liquid sample are automatically evacuated according to the sample. A sample stage for analysis must be prepared, and an exhaust microswitch must be provided on the sample stage receiver. Therefore, the cost of the apparatus increases. Further, rollers, shafts, O-rings, and the like are used in the drive section of the microswitch, but these parts wear out over time and must be replaced periodically.

Further, in the conventional X-ray fluorescence spectrometer, a sample stage for analyzing a large sample must be provided with a projection for exhausting and a projection for preventing rotation, and the sample stage receiver is provided with a projection for preventing rotation. A microswitch must be provided. Therefore, the cost of the apparatus also increases in this case. Also in this case, the drive unit of the microswitch must be periodically replaced.

The present invention has been made in view of the above points, and an object of the present invention is to provide a fluorescent X-ray analyzer having a simpler structure with a smaller number of sample stages than before. is there.

[0010]

Means for Solving the Problems To achieve this object, a first X-ray fluorescence spectrometer according to the present invention comprises: first exhaust instructing means for instructing an exhaust operation of an exhaust device connected to the sample chamber; Second exhaust instructing means for instructing the exhaust operation of the exhaust device, and exhaust control means for controlling the exhaust device based on output signals of the first exhaust instruction means and the second exhaust instruction means. It is characterized by. The X-ray fluorescence spectrometer according to the second aspect of the present invention includes a first rotation instructing unit for instructing a rotating operation of the rotating unit to which the sample stage is attached, and a second rotating instruction for instructing the rotating operation of the rotating unit. And rotation control means for controlling the rotation means based on output signals of the first rotation instruction means and the second rotation instruction means.

[0011]

Embodiments of the present invention will be described below with reference to the drawings.

FIG. 1 is a diagram showing an example of a fluorescent X-ray analyzer according to the present invention.

In FIG. 1, reference numeral 1 denotes a gantry, on which a cover 3 rotatable around an axis 2 perpendicular to the paper is attached. A motor 5 is arranged below the sample chamber 4 formed by the gantry 1 and the cover 3, and the motor 5 is connected to a rotating rod 6 serving as a sample holder. The motor 5 and the rotating rod 6 constitute a rotating means. A sample stage 7 for multi-sample analysis is attached to the tip of the rotating bar 6. The sample stage 7 has a turntable 9 in which holes 8 a to 8 f are formed and a frame 10 fixed on the turntable 9. It is composed of The frame 8 has the hole 8
Holes 11a to 11f slightly larger than a to 8f are formed. 12 is an X-ray source, and 13 is an X-ray detector.

The sample chamber 4 is connected to an exhaust device 14, which comprises a first exhaust switch 15, a second exhaust switch
Is connected to the exhaust device power supply 17 via the exhaust switch 16 of the first embodiment. The first exhaust switch 15 and the second exhaust switch 16 constitute exhaust control means. The first
Is connected to a switch control circuit 18. The switch control circuit 18 generates a cover close signal when the cover 3 is closed, and generates a cover open signal when the cover 3 is opened.
9 is connected. The switch control circuit 18
Is connected to the control device 20. The switch control circuit 18 and the control device 20 constitute first exhaust instruction means.

The second exhaust switch 16 is connected to a switch control circuit 21. The switch control circuit 21 is connected to the reset circuit 19 and a solid sample analysis button 23 on an operation panel 22. . The switch control circuit 21 and the operation panel 22 constitute a second exhaust instruction unit.

On the other hand, the motor 5 is connected to a motor power supply 2 via a first rotation switch 24 and a second rotation switch 25.
6 is connected. The first rotation switch 24 and the second rotation switch 25 constitute rotation control means. The first rotary switch 24 is a switch control circuit 2
The switch control circuit 27 is connected to the reset circuit 19 and the control device 20. The switch control circuit 27 and the control device 20 constitute first rotation instruction means.

The second rotary switch 25 is connected to a switch control circuit 28. The switch control circuit 28 is connected to the reset circuit 19 and the solid sample analysis button 29 of the operation panel 22. ing. The switch control circuit 28 and the operation panel 22 constitute second rotation instruction means.

The configuration of the apparatus shown in FIG. 1 has been described above. Next, the operation of this apparatus will be described.

First, when analyzing a plurality of solid samples, the operator opens the cover 3 and attaches the sample stage 7 for multi-sample analysis to the rotating rod 6 as shown in FIG. When the attachment of the sample table 7 to the rotating rod 6 is completed, the operator sets the sample holders in the holes 11a to 11f of the frame 10, respectively. FIG. 2 shows the sample holder, and a thin film 31 for supporting the sample is attached to one end of a cylindrical sample holder body 30. In this case, the solid sample 32 is received by the thin film 31. FIG. 3 is a sectional view when the sample holder is set in the hole of the frame 10. In addition, as the material of the thin film 31, a material having a small X-ray absorption and containing no analysis element is selected.

When the setting of the sample holder on the frame 10 is completed, the operator closes the cover 3. When the cover 3 is closed, the reset circuit 19 is turned on, and the cover close signal is transmitted to the switch control circuits 18, 21, 2,
7 and 28 respectively.

Next, since the solid sample is set in the sample holder, the operator designates a portion of the display of the control device 20 where "analyze solid sample" is displayed with a mouse. When this designation is performed, a solid sample designation signal is sent from the control device 20 to the switch control circuit 18. The switch control circuit 18 receives the cover close signal from the reset circuit 19 and the control device 20.
Is configured to turn on the first exhaust switch 15 when receiving the solid sample designation signal from the switch control circuit 18 which has already received the cover close signal.
Turns on the first exhaust switch 15 when receiving the solid sample designation signal from the control device 20.

Further, since the solid sample is set in the sample holder, the operator can operate the operation panel 22.
The solid sample analysis button 23 is turned on. When the solid sample analysis button 23 is turned on, a solid sample designation signal is sent from the operation panel 22 to the switch control circuit 21.
The switch control circuit 21 is configured to turn on the second exhaust switch 16 when it receives the cover close signal from the reset circuit 19 and the solid sample designation signal from the operation panel 22. The switch control circuit 21 receiving the close signal turns on the second exhaust switch 16 when receiving the solid sample designation signal from the operation panel 22. When the exhaust switch 16 is turned on, the exhaust device power supply 17, which is turned on, is connected to the exhaust device 14, and the exhaust of the sample chamber 4 starts.

Further, since a plurality of samples are set on the sample stage 7, the operator designates a portion of the display of the control device 20 which indicates "analyzing multiple samples" with a mouse. When this designation is performed, the multi-sample designation signal is sent from the control device 20 to the switch control circuit 27.
Sent to The switch control circuit 27 receives the cover close signal from the reset circuit 19 and the control device 20.
Is configured to turn on the first rotary switch 24 upon receipt of the multi-sample designation signal from the switch control circuit 27 that has already received the cover close signal.
When the multi-sample designation signal is received from the control device 20, the first rotation switch 24 is turned on.

Further, since a plurality of samples are set on the sample table 7, the operator operates the operation panel 22.
The multi-sample analysis button 29 is turned on. When the multi-sample analysis button 29 is turned on, a multi-sample designation signal is sent from the operation panel 22 to the switch control circuit 28. The switch control circuit 28 is configured to turn on the second rotary switch 25 when receiving the cover close signal from the reset circuit 19 and the multi-sample designation signal from the operation panel 22. When the switch control circuit 28 receiving the close signal receives the multi-sample designation signal from the operation panel 22, the switch control circuit 28
Turn 5 on. When the rotation switch 25 is turned on,
The powered motor power supply 26 is connected to the motor 5. Then, when the operator presses an analysis start switch (not shown), the motor 5 connected to the analysis start switch starts a predetermined rotation, rotates to a predetermined sample position and stops, and the X-rays The sample generated by the radiation source 12 is irradiated to the sample, and each sample attached to the sample stage 7 is analyzed in order.

When an analysis stop switch (not shown) is pressed, the rotation of the motor 5 is stopped and the X-ray irradiation is stopped. When the cover 3 is opened, the reset circuit 19 sends a cover open signal to the switch control circuits 18, 21, 27, 28, the control device 20 and the operation panel 22, respectively. The switches 21, 27 and 28 turn off the switches 15, 16, 24 and 25. Also,
The control device 20 that has received the cover open signal stops the signal supply to the switch control circuits 18 and 27,
The solid sample analysis button 23 and the multi-sample analysis button 29 on the operation panel 22 are turned off.

The case where the solid sample is set on the sample stage 7 for multi-sample analysis and the X-ray analysis is performed in the X-ray analyzer of FIG. 1 has been described above. The case where a plurality of liquid samples are subjected to X-ray analysis will be described.

First, when analyzing a plurality of liquid samples, the operator opens the cover 3 and attaches the sample stage 7 for multi-sample analysis to the rotating rod 6. Rotating rod 6 of sample stage 7
When the mounting on the frame 10 is completed, the operator inserts the sample holder shown in FIG.
1a to 11f are set respectively.

When the setting of the sample holder on the frame 10 is completed, the operator closes the cover 3. When the cover 3 is closed, the reset circuit 19 is turned on, and the cover close signal is transmitted to the switch control circuits 18, 21, 2,
7 and 28 respectively.

In this case, since the liquid sample is set in the sample holder, the operator does not designate a portion of the display of the control device 20 where "analyze solid sample" is displayed with a mouse. Therefore, the first exhaust switch 15 is not turned on.

Further, since the liquid sample is set in the sample holder, the operator does not turn on the solid sample analysis button 23 of the operation panel 22. Therefore, the second exhaust switch 16 is not turned on, and the exhaust device power supply 17 is not connected to the exhaust device 14. As a result, the sample chamber 4 is not exhausted.

Further, since a plurality of samples are set on the sample table 7, the operator designates a portion of the display of the control device 20 where "multi-sample analysis" is displayed with a mouse. When this designation is performed, the multi-sample designation signal is sent from the control device 20 to the switch control circuit 27.
Sent to The switch control circuit 27 which has already received the cover close signal turns on the first rotary switch 24 when receiving the multi-sample designation signal from the control device 20.

Further, since a plurality of samples are set on the sample table 7, the operator operates the operation panel 22.
The multi-sample analysis button 29 is turned on. When the multi-sample analysis button 29 is turned on, a multi-sample designation signal is sent from the operation panel 22 to the switch control circuit 28. Switch control circuit 28 already receiving cover close signal
Turns on the second rotation switch 25 when receiving the multi-sample designation signal from the operation panel 22. When the rotation switch 25 is turned on, the motor power supply 26, which is turned on, is connected to the motor 5. Then, when the operator presses the analysis start switch, the motor 5 connected to the analysis start switch starts a predetermined rotation, rotates to a predetermined sample position and stops, and X-rays are transmitted to the X-ray source 12.
Irradiates the sample, and each sample attached to the sample stage 7 is analyzed in turn.

Although the X-ray analysis of a plurality of solid samples and liquid samples in the X-ray analyzer of FIG. 1 has been described above, it is clear from the above description that the X-ray analyzer of the present invention has a plurality of samples. X-ray analysis of the solid sample and the liquid sample can be performed on one common sample stage. And
Since the X-ray analyzer of the present invention does not use a microswitch as in the prior art, the structure of the sample stage and its surroundings is considerably simple. In addition, since the evacuation device does not operate unless the two evacuation instruction means are instructed, the sample chamber is evacuated even if one evacuation instruction device is erroneously instructed when a liquid sample is set. Never.

Next, the case of analyzing a large solid sample with the X-ray analyzer of FIG. 1 will be described.

First, the operator opens the cover 3 and moves the sample stage 33 for large sample analysis shown in FIG.
Attach to The sample table 33 includes a turntable 35 having a hole 34 formed therein, and a frame 36 fixed on the turntable 35.
A slightly larger hole 37 is provided. When the attachment of the sample stage 33 to the rotating rod 6 is completed, the operator operates the frame 3
The solid sample is set in the hole 37 of No. 6 as it is. The sample table 33 is attached to the rotating rod 6 so that the solid sample is irradiated with X-rays generated by the X-ray source 12.

When the sample is set on the frame 36, the operator closes the cover 3. When the cover 3 is closed, the reset circuit 19 is turned on, and a cover close signal is sent to the switch control circuits 18, 21, 27, 28, respectively.

Next, since the solid sample is set on the sample table 33, the operator designates a portion of the display of the control device 20 where "analyze solid sample" is displayed with a mouse. When this designation is performed, the switch control circuit 18 turns on the first exhaust switch 15 as described above.

Further, since the solid sample is set in the sample holder, the operator can operate the operation panel 22.
The solid sample analysis button 23 is turned on. When the solid sample analysis button 23 is turned on, the switch control circuit 21 turns on the second exhaust switch 16 as described above. As a result, the exhaust of the sample chamber 4 starts.

In this case, since one solid sample is set on the sample stage 33, the operator designates a portion of the display of the control device 20 where "multiple sample analysis" is displayed with a mouse. do not do. Further, the operator does not turn on the multi-sample analysis button 29, and the motor power supply 26 is not connected to the motor 5. For this reason,
Even if the operator presses the analysis start switch, the motor 5 does not rotate, and the X-ray analysis of the large sample is performed with the rotation of the sample stage 33 stopped.

The X-ray analysis of a large solid sample in the X-ray analyzer of FIG. 1 has been described above.
In a line analyzer, even when analyzing a large solid sample, a microswitch or the like is not used, so that the structure of the sample stage and its surroundings is considerably simple. In addition, since the rotation means does not operate unless the two rotation instruction means are instructed, even if one rotation instruction means is erroneously instructed when a large sample is set, the rotation means is rotated. There is no.

Although the X-ray fluorescence analyzer of the present invention has been described above by way of example, the present invention is not limited to this.

For example, the display of the control device 20 displays two indications "analysis of solid sample", and when one of them is designated by a mouse, the switch control circuit 18 is displayed.
, A solid sample designation signal may be sent to the switch control circuit 21 when the other is designated by a mouse. Further, two indications "analyze multiple samples" are displayed on the display of the control device 20, and when one of them is designated by a mouse, a multiple sample designation signal is sent to the switch control circuit 27 and the other one is designated. May be configured to send a multi-sample designation signal to the switch control circuit 28 when designated by a mouse. Then, the operation panel 22 can be omitted.

Conversely, two buttons for analyzing a solid sample are provided on the operation panel 22. When one of the buttons is turned on, a solid sample designation signal is sent to the switch control circuit 18, and when the other is turned on, the switch control circuit 18 is turned on. The switch control circuit 21 may be configured to send a solid sample designation signal. Further, the operation panel 22 is provided with two buttons for multi-sample analysis,
When one of them is turned on, a multi-sample designation signal is sent to the switch control circuit 27, and when the other is turned on, a multi-sample designation signal may be sent to the switch control circuit 28. Then, the control device 20 can be omitted. In this way, if only the switch operation on the operation panel is performed, the switch can be instantaneously turned off when an erroneous operation is performed, and the exhaust of the sample chamber and the rotation of the sample holder can be stopped.

The exhaust instruction means and the rotation instruction means are
Instead of one, three or more may be provided.

[Brief description of the drawings]

FIG. 1 is a view for explaining an X-ray fluorescence analyzer of the present invention.

FIG. 2 is a view for explaining a sample holder.

FIG. 3 is a diagram showing a state when a sample holder is mounted on a sample stage.

FIG. 4 is a view showing a sample stage for analyzing a large sample.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... stand, 2 ... shaft, 3 ... cover, 4 ... sample room, 5 ... motor, 6 ... rotating rod, 7 ... sample stand, 8a-8f, 11a-1
1f, 34, 37: hole, 9, 35: turntable, 1
0, 36 ... frame, 12 ... X-ray source, 13 ... X-ray detector, 14
... exhaust device, 15 ... first exhaust switch, 16 ... second exhaust switch, 17 ... exhaust device power supply, 18, 21, 2
7, 28: switch control circuit, 19: reset circuit, 2
0: control device, 22: operation panel, 23: button for solid sample analysis, 24: first rotation switch, 25: second rotation switch, 26: motor power supply, 29: button for multi-sample analysis, 30: sample Holder, 31: thin film, 32: sample, 3
3 ... Sample stand for large sample analysis

Claims (3)

[Claims] 1. A sample placed in a sample chamber is irradiated with X-rays, fluorescent X-rays generated from the sample by the X-ray irradiation are detected, and elements contained in the sample are determined from the detected fluorescent X-rays. In the X-ray fluorescence spectrometer, first exhaust instruction means for instructing an exhaust operation of an exhaust device connected to the sample chamber; second exhaust instruction means for instructing an exhaust operation of the exhaust device; An X-ray fluorescence spectrometer, comprising: exhaust control means for controlling the exhaust device based on output signals of the exhaust instruction means and the second exhaust instruction means. 2. A sample placed in a sample chamber is irradiated with X-rays, fluorescent X-rays generated from the sample by the X-ray irradiation are detected, and elements contained in the sample are determined from the detected fluorescent X-rays. In the X-ray fluorescence spectrometer, first rotation instruction means for instructing a rotation operation of a rotation means to which a sample stage is attached; second rotation instruction means for instructing a rotation operation of the rotation means; An X-ray fluorescence analyzer comprising: a rotation control unit that controls the rotation unit based on an output signal of the instruction unit and a second rotation instruction unit. 3. A sample placed in a sample chamber is irradiated with X-rays, fluorescent X-rays generated from the sample by the X-ray irradiation are detected, and elements contained in the sample are determined from the detected fluorescent X-rays. In the X-ray fluorescence spectrometer, first exhaust instruction means for instructing an exhaust operation of an exhaust device connected to the sample chamber; second exhaust instruction means for instructing an exhaust operation of the exhaust device; Exhaust control means for controlling the exhaust device based on output signals of the exhaust instruction means and the second exhaust instruction means, first rotation instruction means for instructing the rotation of a rotating means to which a sample stage is attached, and A second rotation instructing means for instructing a rotating operation of the rotating means; and a rotation controlling means for controlling the rotating means based on output signals of the first rotation instructing means and the second rotation instructing means. X-ray fluorescence analyzer .