JP2002328105A - X-ray analyzer improved in sealability for spare vacuum chamber - Google Patents

Abstract

PROBLEM TO BE SOLVED: To prolong a span for maintenance.inspection work and to realize efficient analytical work, by restraining deposit of a separated material separated from a sample S on a seal part 14 of a sample cup 10 for forming one portion of a spare chamber 3. SOLUTION: This X-ray analyzer 1 faced with the sample cup 10 for holding a sample holder H filled with the sample S, and for forming the one portion of the spare vacuum chamber 3 in a sample carrying-in port 22 is provided with a shielding member 9 for covering the seal part 14 in an upper end of the sample cup 10 and for preventing the separated material separated from the sample S from being deposited on the seal part 14.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an X-ray analyzer having improved sealability by preventing the detached material from a sample from adhering to a seal portion of a sample cup forming a part of a preliminary vacuum chamber. Things.

[0002]

2. Description of the Related Art Conventionally, an X-ray fluorescence spectrometer has been provided with a sample loading machine for unmanned operation, automation and labor saving. This sample loading machine includes a sample cup and a sample holder stored therein, and loads a sample prepared by the sample preparation machine into this holder. After the sample is loaded, the entire sample cup is carried to the analysis room of the X-ray analyzer, and the seal provided on the sample cup is pressed against a receiving portion having a shutter in the analysis room, and the receiving portions of these analysis chambers are pressed. In a state in which the preliminary vacuum chamber formed by the sample chamber and the preliminary vacuum chamber is kept airtight, the preliminary vacuum chamber is evacuated by a vacuum pump so as to have the same degree of vacuum as the analysis chamber. The sample loaded in is exposed to the analysis chamber, and the sample is irradiated with X-rays for analysis.

[0003]

If the sample is easily broken such as briquette obtained by solidifying powder such as ingot, glass, cement or slag and dust is easily scattered, the sample is loaded into the sample holder. At this time, the detached material from the sample easily adheres to the seal portion of the sample cup, and a defective vacuum may occur during sample analysis due to poor sealing due to the attached detached material. Therefore, in order to remove the detached material, it is necessary to perform maintenance and inspection work such as cleaning of the sample cup in a short span. In addition, since the sample loader is provided inside the X-ray analyzer (in the outer panel for blocking X-rays), the maintenance and maintenance of the sample cup is performed.
Inspection work needs to be performed inside the X-ray analyzer by turning off the X-ray source and shutting off the X-ray, opening the outer panel of the X-ray analyzer. However, once the X-rays are cut off, it takes time until the X-rays are turned on after the operation is completed and the X-ray intensity is stabilized. Furthermore, opening the outer panel destroys the constant temperature state in the analysis chamber, and after the work is completed, closes the outer panel and takes more time until the constant temperature state stabilizes. There was a problem that delayed work.

SUMMARY OF THE INVENTION The present invention solves such a problem and suppresses the detachment from the sample from adhering to the seal portion of the sample cup forming a part of the preliminary vacuum chamber, thereby improving the sealing performance of the preliminary vacuum chamber. It is an object of the present invention to provide an X-ray analyzer capable of maintaining a high level, maintaining a long span of maintenance and inspection work such as cleaning, and improving the efficiency of analysis work.

[0005]

In order to achieve the above object, an X-ray analyzer of the present invention has a sample holder in which a sample is loaded at a sample carry-in port, and a preliminary holder in the X-ray analyzer. An X-ray analyzer that faces a sample cup forming a part of a vacuum chamber, wherein the shielding member covers a seal portion at an upper end of the sample cup and prevents a substance detached from a sample from adhering to the seal portion. It has.

According to this structure, the seal provided at the upper end of the sample cup is covered by the shielding member.
The detached material from the sample is prevented from adhering to the seal portion. For this reason, the span of maintenance / inspection work such as cleaning of the sample cup is lengthened, and the efficiency of the analysis work can be improved.

In a preferred embodiment of the present invention, the shielding member includes a peripheral wall portion facing the seal portion from an inner peripheral side,
It is formed in an L-shaped cross section having an upper wall portion facing the seal portion from above. According to this configuration, at the time of loading the sample into the sample cup, the detachment from the sample is effectively suppressed from adhering to the seal portion.

In a preferred embodiment of the present invention, the space between the seal portion and an adjacent member adjacent above the seal portion is decompressed, or high-pressure air is blown into this space. Means are provided for preventing the detached material from entering the space. According to this configuration, at the time of loading the sample into the sample cup, the detachment from the sample is more effectively suppressed from adhering to the seal portion.

In a preferred embodiment of the present invention,
A sample loading machine that is arranged at the sample loading port and loads a sample into a sample holder housed in a sample cup forming a part of a preliminary vacuum chamber in the X-ray analyzer, wherein the sample loading machine is Transport means for transporting the sample to a sample holder,
And an unloading means for unloading the sample from the sample holder. According to this configuration, it is possible to suppress the detachment that is likely to occur when the sample is stored in the sample cup from adhering to the seal portion.

[0010]

Embodiments of the present invention will be described below with reference to the drawings. FIG. 1 shows a fluorescent X with a sample loader.
It is a longitudinal section showing the outline of a line analyzer. The X-ray fluorescence spectrometer 1 has an analysis chamber 2 inside an exterior panel 1A that covers the entire apparatus, and a sample carrying port 22 is provided in the exterior panel 1A. The work of carrying in the sample to be analyzed in the analysis chamber 2 and the work of taking out the analyzed sample to the outside from the carry-in port 22 are performed. A sample loading machine 20 for loading a sample into the sample loading port 22 and loading it into a sample cup 10 described later facing the loading port 22 is disposed outside the sample loading port 22. Below the sample loading port 22 in the exterior panel 1A,
A transport device 40 for transporting the sample cup 10 between the sample entrance 22 and the analysis chamber 2 is provided. This transport device 4
Numeral 0 is a well-known device constituted by an elevator (not shown) and a linear transfer device.

FIG. 2 is a sectional view showing a state in which a sample holder H housed in a sample cup 10 is set in the analysis chamber 2 and a sample analysis is performed. As shown in the figure, a cylindrical peripheral wall 4 that forms the outer periphery of the preliminary vacuum chamber 3 is fixed or integrally formed with the lower wall 5 of the analysis chamber below the analysis chamber 2. An X-ray tube 6 for irradiating the sample S with X-rays is attached to the upper wall of the analysis chamber 2, and a communication port 5 a between the analysis chamber 2 and the inside of the peripheral wall 4 is rotated or driven by a drive mechanism (not shown). A shutter 8 that moves linearly to open and close the communication port 5a is provided. In the analysis room 2, besides the X-ray tube 6,
A spectroscope, a detector, and the like (not shown) are provided, and the sample S in the analysis chamber 2 maintained at a predetermined degree of vacuum is irradiated with X-rays from the X-ray tube 6 to generate fluorescent X-rays generated from the sample S. Spectroscopy is performed and the intensity of the separated fluorescent X-rays is measured with a detector.
The sample S is analyzed.

FIG. 3 shows a sample loading machine 2 mounted on the sample holder H.
FIG. 9 is a cross-sectional view showing a state when a sample S is loaded according to 0. As shown in the figure, the sample holder H is a sample cup 1
A lower plate 71 supported on the 0 side, a plurality of columns 72 erected on the lower plate 71, and an upper plate 73 fixed to the upper end of the column 72
Supported vertically by the support column 72,
The tray includes a tray 74 for the sample S that moves up and down between the trays 1 and 73, and a coil spring 75 that applies an upward elastic force to the tray 74. A receiving hole 76 for receiving the sample S is formed in the upper plate 73.
A part of the upper surface of the sample S (analysis surface) is held down by suppressing the protrusion of the sample S.
A mask 77 having a hole 77a for exposing the mask 77 is mounted.

When the sample S is loaded into the receiving tray 74, the whole of the sample cup 10 is lifted upward by the elevating table 41 provided in the transfer device 40, and the positioning of the sample cup 10 is performed. The side contacts the lower surface of a movable ring 98 described later. The sample holder H supported by the sample cup 10 is provided with the shielding member 9.
Then, the sample S is loaded into the tray 74 in this protruding state.

A sample cup 1 for supporting the sample holder H
Numeral 0 is removably attached to a lifting table 41 which is placed on a transport device 40 and raised and lowered by an elevator. During sample analysis, the upper end of the sample cup 10 is connected to the peripheral wall 4 of the analysis chamber 2 as shown in FIG. To form a preliminary vacuum chamber 3 together with the peripheral wall 4. A sample table 12 on which a lower plate 71 of a sample holder H shown in FIG.
And a first spring 13 for applying an upward spring force to the sample table 12. This first spring body 13
2 urges the entire sample holder H upward through the table 12 during sample analysis, and the upper plate 73 is rotatably supported on the peripheral wall 4 of the preliminary vacuum chamber 3 in FIG. The sample S is pressed against the sample holder holder 79 so that the sample S faces the analysis chamber 2.

As shown in FIG. 3, the cup body 11
Is a cylindrical large-diameter receiving portion 11a having a bottom, and a small-diameter neck portion 11b provided therebelow and inserted and supported by the lift table 41.
And a cylindrical portion 11c formed concentrically inside the large-diameter receiving portion 11a. An annular groove 11d is formed in an upper outer peripheral portion of the receiving portion 11a, and a seal portion 14 made of rubber packing is attached to the annular groove 11d. When the sample is analyzed, the seal portion 14
Of the preliminary vacuum chamber 3 formed by the peripheral wall 4 and the sample cup 10 so as to be kept airtight to the outside.

A receiving portion 11a in the annular groove 11e shown in FIG.
On the side, an interior material 17 extending from the bottom surface of the annular groove 11e to the upper end of the receiving portion 11a is provided.

The sample table 12 has a circular shape having substantially the same outer diameter as the lower plate 71 of the sample holder H.
Motor 4 attached to the lower surface of the lifting platform 41
2, the sample holder H is rotated via the drive shaft 43 and is placed on the sample table 12, that is, the sample S
X-ray analysis is performed while rotating.

As shown in FIG. 2, the preliminary vacuum chamber 3 is provided with a vacuum pump 46 through a communication hole 45 formed in the peripheral wall 4 thereof.
The inside of the analysis chamber 2 and the preliminary vacuum chamber 3 is evacuated by the vacuum pump 46 via the on-off valves V1 and V2. When the degree of vacuum in the preliminary vacuum chamber 3 becomes equal to the degree of vacuum in the analysis chamber 2, the shutter 8 is opened to analyze the sample S. When the analysis of the sample S is completed, the shutter 8 is closed, the inside of the preliminary vacuum chamber 3 is returned to the atmospheric pressure, the sample cup 10 is detached from the lower end opening 44 of the peripheral wall 4, and the sample cup 10 is moved by the transfer device 40 to the sample. Loading port 2
Return to 2.

FIG. 4 shows an analysis chamber 2 inside the exterior panel 1A.
FIG. 3 is a perspective view schematically showing a sample loader 20 arranged on a side of the sample loading device. The sample loading machine 20 includes a transport unit 50 that transports the sample S to be analyzed to the sample holder H stored in the sample cup 10, an unloading unit 60 that unloads the sample S from the sample holder H, and the transport unit 50. A sample changer 80 is provided for loading the transported sample S into the sample holder H of the sample cup 10, removing the sample S after the analysis from the holder H, and discharging the sample S to the unloading means 60. Further, as shown in FIG. 3, the sample loading machine 20 covers a seal portion 14 provided on the upper outer periphery of the sample cup 10 at the time of loading the sample.
A shielding member 9 is provided on the seal portion 14 for preventing the detached material from the sample S from adhering.

The transport means 50 shown in FIG. 4 includes a carry-in belt 51 for carrying the sample S by running the belt, and a feed table 52 provided at a front portion of the carry-in belt 51 in the carrying direction. A stopper 53 for receiving the transported sample S and a pusher 54 for transporting the received sample S along the upper surface of the feed table 52 to the sample exchanger 80 are provided on the front side.

The sample exchange device 80 includes a feed table 52
The disk 82 is arranged on the front side in the sample transport direction, and is rotated by a motor 81, an elevating member 83 which is moved up and down by the rotation of the disk 82, and fixed on both sides in the width direction of the elevating member 83. And a pinion 8 supported below and engaged with the teeth of the rack 84.
A claw 87 is attached to the tip of a pinion shaft 86 extending laterally from the pinion 85 for pushing down a disc-shaped receiving tray 74 provided on the sample holder H at the time of sample replacement. The claw 87 is connected to the saucer 74 shown in FIG.
Is locked to a flange portion 74a on the outer periphery of.

On one side of the disk 82, a projection 82a is protruded at a radially outward position, while a vertically extending elongated hole 83a for receiving the projection 82a is formed above the elevating member 83. Projection 82a associated with the rotation of the disk 82.
The vertically moving member 83 is reciprocated up and down by the circular motion.
The claw 87 is swung by the rotation of the pinion 85 accompanying the vertical movement of the elevating member 83, and the claw 87 is pressed against the flange 74 a of the tray 74, and as shown by the solid line in FIG. While moving against the spring 75, the sample S is moved to a lower standby position that is substantially flush with the upper surface of the feed table 52, and the sample S sent by the advance of the pusher 54 is loaded on the tray 74. After the loading of the sample S onto the tray 74, the lifting member 83 is raised by the reverse rotation of the motor 81 in FIG. Thereby, the receiving tray 74 is raised to the set position indicated by the imaginary line in contact with the lower surface of the upper plate 73 by the pressing force of the coil spring 75 in FIG.

The unloading means 60 shown in FIG.
0, and a collection box 62 provided at the lower part of the tip of the unloading chute 61. The sample S taken out of the receiving tray 74 by the advance of the pusher 54 is transferred to the collection box 62 via the unloading chute 61. Discharge.

The shielding member 9 shown in FIG. 3 is attached to a lower portion of the sample entrance 22 in the outer panel 1A (FIG. 1). FIG. 5 is an exploded perspective view showing the shield member 9 and the sample cup 10. As shown in the figure, the shielding member 9 has a substantially donut shape in plan view, and has a peripheral wall portion 91 facing the seal portion 14 of the sample cup 10 shown in FIG. An upper wall 92 is formed integrally with an upper wall 91 and has an upper wall 92 opposed to the seal 14 from above.
A notch 93 (FIG. 5) for releasing the claw 87 of the sample exchanger 80 is formed on the upper surface side of the sample changer 80.

The feed table 52 and a transfer plate 94 located on the carry-out side are fixed to the exterior panel 1A (FIG. 1), and the shielding member 9 includes a plurality of mounting screws 95 shown in FIG.
, Are attached to the feed table 52 and the transfer plate 94. The sample entrance 22 (FIGS. 3 and 4) is formed by the feed table 52 and the transfer plate 94.

Further, at the time of loading the sample,
A movable ring 98 is fitted on the outer periphery of the peripheral wall portion 91 of the shielding member 9 as an adjacent member adjacent to the upper side of FIG.
A plurality of coil springs 97 are interposed between a and the upper wall portion 92 of the shielding member 9. The coil spring 97 elastically presses the movable ring 98 against the cup body 11 and the upper surface of the seal portion 14 shown in FIG. 3 when the sample is loaded, and prevents the detached material from the sample from entering the seal portion 14. Suppress.

Further, on the inner peripheral surface of the movable ring 98,
On the outer surface of the peripheral wall portion 91 of the shielding member 9 below the rib 98d, a locking ring 99 is fitted in a ring groove on the outer surface. 98 d and the locking ring 99 prevent the movable ring 98 from falling down from the shielding member 9. Thus, the movable ring (adjacent member) 9
Reference numeral 8 denotes a shielding member 9, a feed table 52, and a transfer plate 94.
Through the outer panel 1A of the X-ray analyzer 1 of FIG.

A notch 14a having a V-shaped cross section is formed on the inner peripheral side of the upper portion of the seal portion 14 shown in FIG.
A space 19 is formed between a and the outer peripheral surface of the movable ring 98, and a suction pipe (decompression means) 100 connected to a suction device such as a dust collector is connected to the outer peripheral portion of the movable ring 98. By reducing the pressure in the space 19 by the suction tube 100 and increasing the degree of sealing of the seal portion 14, the material detached from the sample S is prevented from entering the seal portion 14 and attaching thereto. Instead of the suction pipe 100, the space 1
A blowing pipe (blowing means) 100 for blowing high-pressure air into 9
A may be connected. In that case, high-pressure air is blown into the space 19 from the blowing pipe 100 to form a high-pressure air flow, so that the detached material from the sample S is prevented from entering the seal portion 14 and attaching thereto.

Next, a procedure for exchanging the sample S using the sample loading machine 20 will be described. First, the sample S prepared by the sample preparation machine is placed on the carry-in belt 51 of the transfer means 50 of the sample loading machine 20 shown in FIG. After being transported to the position of
Is transported on the feed table 52 to the position of the sample exchanger 80 by the advance of. On the other hand, on the sample exchanger 80 side, the sample cup 10 is lifted in advance via the elevating table 41 of the transfer device 40 shown in FIG. Is in contact with the lower surface of the movable ring 98 to position the sample cup 10. In this state, the upper end of the seal portion 14 is in contact with or close to the lower surface of the movable ring 98, and the sample holder H supported by the sample cup 10 projects upward from the inside of the shielding member 9. At the time of loading the sample, the tray 74 of the sample holder H is pushed down by the sample exchanger 80 of FIG. 4 and stands by at the standby position below the solid line in FIG. The sample S to be loaded is loaded.

When the sample S is loaded into the receiving tray 74, the receiving tray 74 is moved to a sample setting position indicated by a virtual line in FIG. It is inserted and set in the receiving hole 76 of 73.

At the time of loading the sample S into the sample holder H as described above, the separated material such as the sample powder separated from the sample S falls from the tray 74 toward the inside of the sample cup 10. The seal portion 14 provided on the outer periphery of the upper end of the sample cup 10 is entirely covered by the peripheral wall portion 91 and the upper wall portion 92 of the shielding member 9 facing the fall-off and separation object. The lower end surface is formed by a large diameter receiving portion 11 of the cup body 11 by a coil spring 97.
a, and the upper surface of the seal portion 14 is elastically pressed against the cut portion 14a of the seal portion 14, that is, the intrusion of the detached material from the sample S into the upper surface of the seal portion 14 is suppressed as much as possible.

Further, a sealing member 15 is disposed in the cup body 11 of the sample cup 10, and the upper end thereof is pressed against the lower end of the peripheral wall portion 91 of the shielding member 9 by the second spring 16. Further, the detachment from the sample S is more effectively prevented from adhering to the upper surface of the seal portion 14. Further, at the time of loading work of the sample S, the suction tube 100 connected to the outer peripheral portion of the movable ring 98
Movable ring 98, seal portion 14 and cup body 1
Since the pressure in the space 19 formed between the outer peripheral surface of the sample 1 and the outer peripheral surface of the sample S is reduced, the sealing performance of the seal portion 14 is improved, and the detachment of the sample S from the upper surface of the seal portion 14 is more effectively suppressed. Is done. Also, when the blowing tube 100A is provided in place of the suction tube 100, high-pressure air is blown into the space 19, and thus the high-pressure air flow causes the detached material from the sample S to adhere to the upper surface of the seal portion 14. Is more effectively suppressed. As a result, maintenance /
The span of inspection work can be lengthened, and the efficiency of analysis work can be increased.

As described above, the sample cup 10 shown in FIG.
After the sample S is loaded into the sample holder H, the entire sample cup 10 is taken out from the shielding member 9 by the lifting table 41 of the transfer device 40 and analyzed by the transfer device 40 of FIG. Transported to the lower side of the room 2
As shown in FIG. 2, the seal portion 14 of the sample cup 10 is pressed against the lower surface of the peripheral edge of the lower end opening 44 of the peripheral wall 4 of the analysis chamber 2 to be sealed, as shown in FIG. Preliminary vacuum chamber 3 formed by cup 10
Is kept airtight. At this time, since no detached material is attached to the upper surface of the seal portion 14, a large sealing force is secured.

When the analysis of the sample S is completed, the shutter 8 is closed and the inside of the preliminary vacuum chamber 3 is returned to the atmospheric pressure.
The sample cup 10 is lowered by the elevating table 41 of the transfer device 40 and is separated from the lower end opening 44 of the peripheral wall 4. Thereafter, the sample cup 10 is returned to the position facing the sample carrying-in port 22 in FIG. 1 by the transfer device 40, and the receiving tray 74 is moved to the lower standby position by the sample exchanger 80 in FIG. S is pushed out of the receiving tray 74 through the transfer plate 94 to the unloading chute 61 of the unloading means 60, and from the discharging chute 61 to the collection box 62.
Is discharged to After the sample S is taken out, a new sample S is loaded on the tray 74 as described above.

Although the above embodiment has been described with respect to the case where the apparatus has a sample loading machine for automatically loading a sample, the present invention provides a well-known rotary type in which a sample holder loaded with a sample in advance is provided at a sample loading port. (Refer to Japanese Patent Application No. 11-166821, for example) which is manually placed on a sample exchange table and transferred from the sample exchange table to a sample cup.

[0036]

As described above, according to the present invention, the detachment from the sample can be suppressed from adhering to the seal portion provided in the sample cup forming a part of the preliminary vacuum chamber. -The analysis work can be made more efficient by lengthening the span of inspection work.

[Brief description of the drawings]

FIG. 1 is a longitudinal sectional view schematically showing an X-ray analyzer according to one embodiment of the present invention.

FIG. 2 is a longitudinal sectional view showing a state where a sample analysis is performed by setting a sample holder of a sample cup in an analysis chamber of an X-ray analyzer.

FIG. 3 is a longitudinal sectional view showing a state where a sample is loaded into a sample holder of a sample cup by a sample loading machine.

FIG. 4 is a perspective view schematically showing a sample loading machine.

FIG. 5 is an exploded perspective view showing portions of a sample cup and a shielding member.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... X-ray analyzer, 1A ... exterior panel, 22 ... sample entrance, 3 ... preliminary vacuum chamber, 9 ... shielding member, 91 ... peripheral wall part, 9
2 ... top wall, 98 ... adjacent member (movable ring), 10 ... sample cup, 14 ... seal, 19 ... space, 50 ... transportation means, 60 ... unloading means, 80 ... sample exchange machine, 100 ... decompression means, 100A ... Blowing means, H ... Sample holder, S ... Sample

Claims (5)

[Claims] 1. An X-ray analyzer, wherein a sample holder for loading a sample is held at a sample inlet, and a sample cup forming a part of a preliminary vacuum chamber in the X-ray analyzer is exposed. An X-ray analyzer, comprising: a shielding member that covers a seal portion at an upper end of the sample cup and prevents a substance detached from a sample from adhering to the seal portion. 2. The device according to claim 1, wherein the shielding member has an L-shaped cross section having a peripheral wall portion facing the seal portion from the inner peripheral side and an upper wall portion facing the seal portion from above. X-ray analyzer. 3. The method according to claim 1, further comprising: reducing a pressure in a space between the seal portion and an adjacent member adjacent above the seal portion to prevent the detached material from entering the space. X-ray analyzer equipped with a decompression means for preventing. 4. The device according to claim 1, wherein high-pressure air is blown into a space between the seal portion and an adjacent member adjacent above the seal portion, and the detached material enters the space. An X-ray analyzer provided with a blowing means for preventing the occurrence of air. 5. The sample holder according to claim 1, further comprising a sample cup disposed at the sample entrance and forming a part of a preliminary vacuum chamber in the X-ray analyzer. An X-ray analyzer, comprising: a sample loader for loading a sample into the sample holder; the sample loader comprising: transport means for transporting the sample to a sample holder; and unloading means for unloading the sample from the sample holder.