JP2009053037A - Fluorescent x-ray analyzer - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an inexpensive fluorescent X-ray analyzer allowing a filter to be simply and easily replaced manually. <P>SOLUTION: This fluorescent X-ray analyzer 100 comprises an X-ray tube 1, a sample chamber 3 having a lid 2, a sample chamber leak valve 41, a spectroscopy chamber 5 having a detecting means 4 for detecting fluorescent X-rays 12, a spectroscopy chamber leak valve 51, a vacuum shutter 6 for opening and closing an opening 10 between the sample chamber 3 and the spectroscopy chamber 5, a filter moving means to which a filter 7 for filtering primary X-rays 11 is attached replaceably, a sample replacing machine 20, and a controlling means 30 for controlling the X-ray tube 1, the lid 2, a vacuum pump 9, the sample chamber leak valve 41, the spectroscopy chamber leak valve 51, the vacuum shutter 6, the filter moving means 8, and the sample replacing machine 20. The controlling means 30 executes a filter replacement preparing procedure in response to a first command, and executes an initializing procedure of returning the state to the state before the execution of the procedure in response to a second command. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  In the present invention, a sample is irradiated with primary X-rays filtered from an X-ray source such as an X-ray tube, and the intensity of the generated fluorescent X-rays is measured by a detection means such as a detector. The present invention relates to a fluorescent X-ray analyzer capable of easily exchanging a filter in fluorescent X-ray analysis for analyzing the content rate, film thickness, and the like of the liquid.

Conventionally, in fluorescent X-ray analysis, a sample is analyzed by selecting a filter that filters an appropriate primary X-ray according to the purpose of analysis. Are equipped with a fluorescent X-ray analyzer (see Patent Document 1). However, in such a fluorescent X-ray analyzer having an automatic filter exchanger that can automatically replace a plurality of filters, the volume occupied by the automatic filter exchanger increases, and the vacuum chamber that is a spectroscopic chamber that accommodates the filter increases. Becomes larger and more expensive. Furthermore, it takes a long time to evacuate the spectroscopic chamber. Therefore, as a simple and inexpensive apparatus for analysis that does not require frequent filter replacement, there is an X-ray fluorescence analyzer that can replace a filter manually without providing an automatic filter exchanger.
JP 2001-349851 A

  However, in a conventional fluorescent X-ray analysis apparatus in which the filter can be manually replaced, the filter housed in the spectral chamber being evacuated is removed from the opening of a vacuum shutter provided as a partition between the sample chamber and the spectral chamber. In order for the operator to manually replace the X-ray tube, the X-ray tube is turned off, the sample chamber and the spectroscopic chamber are evacuated and exhausted, the transport arm for transporting the sample, the lid of the sample chamber and the opening and closing of the vacuum shutter, etc. Each step operation must be performed by the operator by instructing the input means of the apparatus for each step, and the operation is complicated, and if the operation step is inadvertently specified, the apparatus is caused by interference or overload of each component of the apparatus. May be damaged.

  As described above, in the conventional simple and inexpensive fluorescent X-ray analyzer, the manual filter replacement operation is complicated and cannot be easily and easily replaced.

  The present invention has been made in view of the above-described conventional problems, and an object thereof is to provide an inexpensive X-ray fluorescence analyzer capable of easily and easily replacing a filter manually.

  In order to achieve the above object, an X-ray fluorescence analyzer of the present invention has an X-ray tube for irradiating a sample with primary X-rays and a lid that can be opened and closed, and is vacuumed by a vacuum pump when the lid is closed. Detect the intensity of fluorescent X-rays generated from the sample by evacuating the sample chamber, opening the sample chamber leak valve that opens and connects the sample chamber to the atmosphere, and irradiating the primary X-ray from the X-ray tube A spectroscopic chamber that is housed and is evacuated by the vacuum pump, a spectroscopic chamber leak valve that opens and connects the spectroscopic chamber to the atmosphere, and a partition wall between the sample chamber and the spectroscopic chamber A vacuum shutter that opens and closes the provided opening and a filter that filters primary X-rays from the X-ray tube are interchangeably attached, and the filter is connected to the primary X-ray between the X-ray tube and the sample. To advance and retreat into the aisle Sample advancement / retraction means, a turret on which a sample is placed, a sample exchanger having a transfer arm for transferring the sample from the turret to the sample chamber, the X-ray tube, a lid, a vacuum pump, a sample chamber leak valve, a spectroscopic chamber A fluorescent X-ray analyzer having a leak valve, a vacuum shutter, a filter advance / retreat means, and a control means for controlling the sample exchanger.

  Further, in the fluorescent X-ray analysis apparatus of the present invention, the control means stops the irradiation of the primary X-ray to the X-ray tube according to the first instruction of the operator, and the transfer arm from the opening. A procedure for evacuating the sample chamber, a procedure for bringing the sample chamber to atmospheric pressure by stopping the vacuum pump and opening the sample chamber leak valve, and a step for stopping the vacuum pump and opening the spectroscopic chamber leak valve. Move the filter to the filter advancing / retreating means just below the opening after the procedure for setting the pressure, the procedure for opening the lid after the procedure for setting the sample chamber to atmospheric pressure, and the procedure for retracting the transfer arm And a filter replacement preparation procedure including a procedure for opening the vacuum shutter, and in response to a second instruction from an operator, It performs an initialization procedure for returning to the state before data exchange preparing procedure execution.

  According to the present invention, the control means is configured to stop the irradiation of the primary X-rays to the X-ray tube according to the first instruction from the input means by the operator, and retract the transfer arm from the opening. A procedure for bringing the sample chamber to atmospheric pressure by stopping the vacuum pump and opening the sample chamber leak valve; and bringing the spectral chamber to atmospheric pressure by stopping the vacuum pump and opening the spectrum chamber leak valve. A procedure for opening the lid after a procedure for setting the inside of the sample chamber to atmospheric pressure, and a procedure for moving the filter to the filter advancing / retreating means immediately below the opening after a procedure for retracting the transfer arm. And a procedure for preparing the filter replacement including the procedure for opening the vacuum shutter, the operator must input an instruction with the input means of the apparatus for each step. Rather, without damaging the apparatus due to interference or overload of the components of the device, the spectral indoor filter being evacuated can easily be exchanged manually from the opening of the vacuum shutter. Then, according to the second instruction from the input means by the operator, the X-ray fluorescence analyzer is initialized to the state before the execution of the filter replacement preparation procedure, so that the measurement of the sample S can be started immediately.

  Hereinafter, a fluorescent X-ray analyzer according to an embodiment of the present invention will be described. As shown in FIGS. 1A and 1B, a fluorescent X-ray analyzer 100 includes an X-ray tube 1 that irradiates a sample S placed in a sample holder SH with a primary X-ray 11 from below, and a lid 2 that can be freely opened and closed. The sample chamber 3 evacuated by the vacuum pump 9 when the lid 2 is closed, the sample chamber leak valve 41 for communicating the sample chamber 3 with the atmosphere, the spectroscopic chamber 5 evacuated by the vacuum pump 9, and the spectroscopic chamber A spectroscopic chamber leak valve 51 for communicating 5 with the atmosphere, a vacuum shutter 6 for opening and closing an opening 10 provided as a partition between the sample chamber 3 and the spectroscopic chamber 5, and primary X-rays 11 from the X-ray tube 1. A primary filter 7 for filtering the filter 7 is attached in a replaceable manner, a filter advance / retreat means 8 for moving the filter 7 back and forth in the path of the primary X-ray 11, and a turret 21 for placing a sample holder SH containing the sample S; Sample holder SH A sample changer 20 having a transfer arm 22 for transferring it from the chamber 21 to the sample chamber 3, an X-ray tube 1, a lid 2, a vacuum pump 9, a sample chamber leak valve 41, a spectroscopic chamber leak valve 51, a vacuum shutter 6, and a filter advance / retreat. Means 8 and control means 30 for controlling the sample changer 20 are provided.

  In response to a first instruction from the input means 31 by the operator, the control means 30 stops the irradiation of the primary X-ray 11 to the X-ray tube 1, retreats the transfer arm 22 from the opening 10, vacuum A procedure for bringing the inside of the sample chamber 3 to atmospheric pressure by stopping the pump 9 and opening the sample chamber leak valve 41; and a procedure for bringing the inside of the spectroscopic chamber 5 to atmospheric pressure by stopping the vacuum pump 9 and opening the spectroscopic chamber leak valve 51. A procedure for opening the lid 2 after a procedure for setting the inside of the sample chamber 3 to atmospheric pressure, a procedure for moving the filter 7 to the filter advance / retreat means 8 to a position immediately below the opening 10 after a procedure for retracting the transfer arm 22; A filter replacement preparation procedure including a procedure for opening the vacuum shutter 6 is executed. After the filter 7 is replaced, an initialization procedure for returning the X-ray fluorescence spectrometer 100 to a state before the filter replacement preparation procedure is executed is executed in accordance with a second instruction from the input means 31 by the operator.

  The sample chamber 3 is a vacuum chamber formed when the vacuum shutter 6 is closed and the lid 2 is closed. When the sample holder SH is inserted, air is introduced into the sample chamber 3 by the sample chamber leak valve 41. The lid 2 is opened upward after communicating with the atmosphere. After the sample holder SH is inserted, the lid 2 and the sample chamber leak valve 41 are closed and evacuated by the vacuum pump 9 to be kept in vacuum.

  The spectroscopic chamber 5 communicates with the sample chamber 3 through an opening 10 of a vacuum shutter 6 provided as a partition wall between the sample chamber 3 and the spectroscopic chamber 5. As shown in FIG. 2, the spectroscopic chamber 5 houses detection means 4 that detects the intensity of fluorescent X-rays 12 generated from the sample S when the primary X-ray 11 from the X-ray tube 1 is irradiated. The detection means 4 has a divergence slit 41 that collimates the secondary X-ray 12 that is a fluorescent X-ray, a spectroscopic element 42 that splits the secondary X-ray parallelized by the divergence slit 41, and the spectroscopic element 42 splits the light. A light receiving slit 43 that parallelizes the secondary X-ray and a detector that detects the secondary X-ray 12 parallelized by the light receiving slit 43, for example, a scintillation counter 44 are included. The spectroscopic chamber 5 also houses the X-ray tube 1 and the filter advancing / retreating means 8, and the vacuum shutter 6 and the spectroscopic chamber leak valve 51 are closed, and the vacuum pump 9 exhausts the vacuum chamber and maintains the vacuum. When the spectroscopic chamber 5 communicates with the atmosphere, the spectroscopic chamber leak valve 51 leaks air.

  The filter 7 is formed of a foil or a thin plate of aluminum, iron, vanadium or the like, for example, and is used to reduce intrinsic X-rays, impurity lines and background of the target material emitted from the X-ray tube 1. As shown in FIG. 3, the filter 7 is attached to the filter advance / retreat means 8. When the sample S is measured, the filter advancing / retreating means 8 is controlled by the control means 30 so that the filter 7 enters the passage of the primary X-ray 11 when filtering the primary X-ray 11 and retreats when not filtering. The When the filter 7 is replaced, the filter advance / retreat means 8 is controlled by the control means 30 so that the filter 7 moves to the position of the opening 10 of the vacuum shutter 6. The X-ray fluorescence analyzer 100 is a bottom surface irradiation type and wavelength dispersion type X-ray fluorescence analyzer.

  Next, the operation of the fluorescent X-ray analysis apparatus 100 according to the embodiment of the present invention will be described according to the steps of the flowchart shown in FIG. FIG. 4 is a flowchart when the sample holder SH is not accommodated in the sample chamber 3. In step S <b> 1, the operator inputs a first instruction to prepare for replacement of the filter 7 from the input unit 31 of the control unit 30. When the first instruction is input, the power of the X-ray tube 1 is turned off in step S2. In step S3, the transfer arm 22 of the sample changer 20 moves to the retracted position. In step S4, the vacuum pump 9 is stopped. In step S5, the inside of the sample chamber 3 maintained at a predetermined vacuum pressure is leaked by the sample chamber leak valve 41 to the atmospheric pressure. In step S6, the inside of the spectroscopic chamber 5 maintained at a predetermined vacuum pressure is leaked by the spectroscopic chamber leak valve 51 to the atmospheric pressure. When the sample chamber 3 and the spectroscopic chamber 5 are at atmospheric pressure, the process proceeds to step S7. In step S7, the lid 2 of the sample chamber 3 is opened, and the sample chamber 3 is opened. In step S <b> 8, the filter 7 is moved by the filter advancing / retreating means 8 to a position immediately below the opening 10 of the vacuum shutter 6. In step S9, the vacuum shutter 6 is opened.

  At this time, the lid 2 and the transfer arm 22 are retracted from the opening 10 of the vacuum shutter, and the vacuum shutter 6 is also opened. In step S10, the operator opens an apparatus cover (not shown) covering the outside of the lid 2 and fixes the filter cover 8 to the filter advance / retreat means 8 shown in FIG. Look at the filter 7, put a hand in the opening 10, remove the fixing screw 71, remove the used filter 7, fix the filter 7 to be used next to the filter advancing / retreating means 8 with the fixing screw 71, and attach the device cover. Close and close. In step S <b> 11, the operator inputs a second instruction to the effect that the fluorescent X-ray analysis apparatus 100 should be initialized from the input unit 31. When the second instruction is input, in step S12, “Initializing” is displayed on the display unit 32 of the control device 30, the X-ray fluorescence analyzer 100 is initialized, and before the first instruction is input. The state, that is, the state before starting the measurement of the sample S is set.

  According to the fluorescent X-ray analysis apparatus 100 of the present embodiment, the control unit 30 stops the irradiation of the primary X-ray 11 on the X-ray tube 1 in response to the first instruction from the input unit 31 by the operator. A procedure for retracting the transfer arm 22 from the opening 10; a procedure for stopping the vacuum pump 9 and opening the sample chamber leak valve 41 to bring the inside of the sample chamber 3 to atmospheric pressure; and a procedure for stopping the vacuum pump 9 and the spectroscopic chamber leak valve. Filter opening / retracting means after opening the lid 51 after opening the chamber 51 by opening 51, opening the lid 2 after opening the sample chamber 3 at atmospheric pressure, and retracting the transfer arm 22 8, the filter replacement preparation procedure including the procedure of moving the filter 7 to the position immediately below the opening 10 and the procedure of opening the vacuum shutter 6 is executed. Therefore, the operator inputs the input means 3 of the apparatus for each step. The filter 7 in the spectroscopic chamber 5 that has been evacuated without damaging the fluorescent X-ray analyzer due to interference or overload of each component of the fluorescent X-ray analyzer 100 can be used. It can be easily replaced manually from the opening 10 of the vacuum shutter 6. Then, according to the second instruction from the input means 31 by the operator, the X-ray fluorescence analyzer 100 is initialized to the state before the execution of the filter replacement preparation procedure, so that the measurement of the sample S can be started immediately.

  In the present embodiment, the bottom-illuminated and wavelength-dispersed X-ray fluorescence analyzer has been described, but the top-illuminated type or the energy-dispersed type may be used. The operation flow when the sample holder SH is not accommodated in the sample chamber 3 has been described. However, when the sample holder SH is accommodated in the sample chamber 3, the sample holder SH is discharged from the sample chamber 3. After performing the operation to be performed, the operation flow of this embodiment may be performed.

1 is a schematic front view of a fluorescent X-ray analyzer according to an embodiment of the present invention. It is a schematic plan view of the apparatus. It is a schematic side view of the spectroscopic chamber of the apparatus. It is a top view of the filter advance / retreat means of the same apparatus. It is an operation | movement flowchart of the same apparatus.

Explanation of symbols

1 X-ray tube 2 Lid 3 Sample chamber 4 Detection means 5 Spectroscopic chamber
6 Vacuum shutter 7 Filter 8 Filter advance / retreat means 9 Vacuum pump 10 Vacuum shutter opening 11 Primary X-ray 12 Fluorescent X-ray Secondary X-ray 20 Sample exchanger 21 Turret 22 Transfer arm 30 Control means 31 Input means 41 Sample chamber leak valve 51 Spectroscopic leak valve 100 X-ray fluorescence analyzer S Sample

Claims (1)

An X-ray tube that irradiates the sample with primary X-rays;
A sample chamber having an openable / closable lid, and evacuated by a vacuum pump when the lid is closed;
A sample chamber leak valve for communicating the sample chamber to the atmosphere by being opened; and
A spectroscopic chamber in which detection means for detecting the intensity of fluorescent X-rays generated from the sample by irradiation of primary X-rays from the X-ray tube is housed and evacuated by the vacuum pump;
A spectroscopic chamber leak valve that is opened to communicate the spectroscopic chamber to the atmosphere;
A vacuum shutter that opens and closes an opening provided in a partition wall between the sample chamber and the spectroscopic chamber;
A filter advancing and retracting means for exchanging a primary X-ray from the X-ray tube in a replaceable manner, and advancing and retracting the filter in a primary X-ray path between the X-ray tube and the sample;
A sample changer having a turret on which a sample is placed, and a transfer arm for transferring the sample from the turret to the sample chamber;
Control means for controlling the X-ray tube, lid, vacuum pump, sample chamber leak valve, spectroscopic chamber leak valve, vacuum shutter, filter advance / retreat means, and sample exchanger;
A fluorescent X-ray analysis apparatus comprising:
In accordance with a first instruction from an operator, the control means stops the irradiation of the primary X-rays to the X-ray tube, retracts the transfer arm from the opening, stops the vacuum pump; A procedure for bringing the sample chamber to atmospheric pressure by opening the sample chamber leak valve; a procedure for stopping the vacuum pump and opening the spectroscopic chamber leak valve; and A procedure for opening the lid after a procedure for making, a procedure for moving the filter to just below the opening in the filter advance / retreat means after a procedure for retracting the transfer arm, and a procedure for opening the vacuum shutter In response to the operator's second instruction, the X-ray fluorescence analyzer is first returned to the state before the filter replacement preparation procedure is executed. X-ray fluorescence spectrometer to perform the procedure.

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