JP3247665B2 - Sample exchange in X-ray analyzer - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sample changer provided at a sample entrance of an X-ray analyzer for exchanging a sample.

[0002]

2. Description of the Related Art Conventionally, a preliminary exhaust chamber for carrying a sample from outside is provided adjacent to an analysis chamber for analyzing a sample under vacuum, and the inside of the preliminary exhaust chamber is evacuated by a vacuum pump, and then the preliminary vacuum exhaust is performed. The shutter that separates the chamber from the analysis chamber is opened, and the fluorescent X is transferred from the preliminary vacuum chamber to the analysis chamber.
Line analyzers are known.

[0003] The interior of such a pre-evacuation chamber is contaminated by powder of powder samples, fragments of glass beads or ingot samples due to repeated evacuation and leaking. Is performed.

A sample cup forming the lower half of the preliminary exhaust chamber is transported from a preliminary exhaust position below the analysis chamber to an exchange position facing the sample entrance, and a sample exchange provided at the sample entrance. Is sequentially replaced with a new sample.

[0005]

However, in the above-described conventional apparatus, since the sample exchanger cannot be removed from the sample entrance, maintenance / inspection such as cleaning of the sample cup is performed by temporarily removing the X-ray source. Turn off to block X-rays, X
The external panel of the X-ray analyzer was opened, and the analysis was performed inside the apparatus. However, once the X-rays are cut off, it takes time until the X-rays are turned on after the work is completed and the X-rays are stabilized.
In addition, when the exterior panel is opened, the temperature inside the analysis chamber is destroyed, and after the work is completed, the exterior panel is closed and it takes more time until the temperature becomes stable. There was a problem that delayed work.

The present invention solves such a problem, and can easily perform maintenance work on a sample cup forming a part of a preliminary exhaust chamber, thereby improving the efficiency of analysis work. It is intended to provide a line analyzer.

[0007]

In order to achieve the above object, a sample exchanger according to the present invention is provided at a sample inlet of an X-ray analyzer, and has a sample holder having an exchange hole and holding a sample. A sample exchange device for delivering a sample holder which is formed from the exchange hole to a sample cup forming a part of a preliminary vacuum chamber in an X-ray analyzer and receiving a sample holder led out from the sample cup through the exchange hole; It is set movably to open and close the mouth. According to this configuration,
By moving the sample exchanger, maintenance and inspection of the sample cup can be easily performed from the sample entrance that opens.

[0008] In a preferred embodiment of the present invention, the sample exchanger comprises a base plate having the exchange hole, and a moving plate which is set movably with respect to the base plate and moves a plurality of sample holders on the base plate. A driving device for driving the moving plate to move the sample holder to a position corresponding to the exchange hole.

In a preferred embodiment of the present invention, X
X-ray analyzer, a sample cup supporting the sample holder, a preliminary exhaust position forming a part of a preliminary exhaust chamber adjacent to the analysis chamber that performs X-ray irradiation on the sample, and an exchange position facing the sample carry-in port. The sample cup is provided detachably with respect to the transport means. According to this configuration, the sample cup can be detached from the transfer means and taken out from the sample loading port, so that the maintenance and inspection work of the sample cup is further facilitated. Also, if a plurality of sample cups are prepared, the next analysis operation can be performed without interrupting the analysis work by exchanging the sample cups. Therefore, there is no interruption time of the analysis work due to the maintenance / inspection work, and the work efficiency is improved.

[0010]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Preferred embodiments in which the present invention is applied to a fluorescent X-ray analyzer will be described below in detail with reference to the drawings. In FIG. 1, the X-ray fluorescence analyzer has an analysis chamber 2 provided inside an exterior panel 1 and a preliminary exhaust chamber 3 provided below the analysis chamber 2. The peripheral wall 4 of the preliminary exhaust chamber 3 is fixed or integrally formed with the lower wall 5 of the analysis chamber. 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 51 between the analysis chamber 2 and the preliminary exhaust chamber 3 is rotated or linearly moved by a driving mechanism (not shown). The shutter 8 is opened and closed.

A sample entrance 20 formed in the exterior panel 1
Is provided with a sample exchanger 9, and a sample cup 10, which will be described later, is provided in the exterior panel 1.
A transfer means 40 is provided for transferring between an exchange position below the pre-exhaust position and a preliminary exhaust position forming the lower part of the preliminary exhaust chamber 3. The transporting means 40 is a known one comprising an elevator (not shown) and a linear transporter.

In the analysis chamber 2, in addition to the X-ray tube 6,
A spectroscope and a detector (not shown) are provided, and the sample S in the analysis chamber 2 maintained at a predetermined vacuum degree is irradiated with X-rays from the X-ray tube 6 to spectrally separate the fluorescent X-rays generated from the sample S. Spectroscopy with a detector, measure the intensity of the separated fluorescent X-rays with a detector,
The sample S is analyzed.

As shown in FIG. 6, the sample S is a sample holder H
The sample holder H is held in the sample cup 10
It is supported by. The sample holder S is a cylindrical container having a bottom and has a coil spring 53 for applying an upward elastic force to the sample S, a part of the upper surface (analysis surface) of the sample S being exposed to cover other portions, and And a mask 54 for suppressing the protrusion of S, and a through hole 55 is provided in a peripheral wall thereof. The through hole 55 is for making the degree of vacuum in the sample holder H the same as the degree of vacuum in the preliminary exhaust chamber 3.

A sample cup 1 for supporting the sample holder H
0 is pressed against the open lower end of the peripheral wall 4 of the preliminary exhaust chamber 3 to form the preliminary exhaust chamber 3 together with the peripheral wall 4. The sample cup 10 is removably attached to an elevating table 41 which is placed on the transporting means 40 and raised and lowered by an elevating device. As shown in FIG. A sample table 12 to be placed, a ring-shaped guide body 13 into which the outer peripheral portion of the lower end of the sample holder H is fitted to regulate the position of the sample holder H in the radial direction, and A first spring body 14 for applying a spring force is mounted. The cup main body 11 is detachably attached to the lift table 41 by a screw body 66.

The cup body 11 has a bottomed cylindrical large-diameter receiving portion 11a, a small-diameter neck portion 11b therebelow, a flange portion 11c, and a shaft supporting portion 11d formed concentrically inside the receiving portion 11a. , And an upper contact portion 11f and a lower spring receiver 11g. A sealing member 16 made of rubber packing is fitted into a groove 15 formed on the outer diameter side of the receiving portion 11a, and the floating bearing 1
7 is supported movably in the axial direction. This bearing 1
7 has a pair of bearings 17a, 17a and a holder 17b for holding them, and is upwardly moved by a second spring body 24 interposed between the holder 17b and the lower spring receiver 11g. A spring force is applied and the spring is pressed against the contact portion 11f. Therefore, the sample table 12 moves axially downward together with the bearing 17 in accordance with the load. An annular groove 18 formed between the shaft support 11d and the receiving part 11a and opening upward has the guide body 13 and the first
A spring body 14 is fitted.

The sample table 12 has a circular shape having substantially the same outer diameter as the bottom surface of the sample holder H, and a rotating shaft 61 is connected to the center of the lower surface. The rotating shaft 61 includes a fixed portion 61a fixed to the sample table 12, and a swing portion 61c that is swingably connected to the fixed portion 61a by a pin 61b. The fixed portion 61a of the rotating shaft 61 is supported by the bearing 17, and a connecting groove 62 extending in the radial direction is formed at the lower end of the swinging portion 61c, as shown in FIG. 4B. The bearing 17 moves in the axial direction together with the rotating shaft 61 according to the load applied to the sample table 12.

The neck 11b shown in FIG. 4 (a) has a substantially cylindrical shape, and has an outer diameter smaller than that of the receiving portion 11a, and is fitted into a fitting hole 11e provided on the inner diameter side thereof.
a is inserted and the center of the lift table 41 is aligned.
The flange portion 11c has a disk shape, has an outer diameter larger than that of the receiving portion 11a, and as shown in FIG.
Are formed at two point symmetric positions. On the other hand, a screw body 66 is attached to a mounting hole 41b formed in the elevating table 41 of the transport means 40 at two point symmetric positions, and a large diameter retaining portion 66a (see FIG. 4 (a))
Is attached. With the retaining portion 66a and the screw head 66b, the screw body 66 is not completely detached from the elevator 41. The attachment / detachment hole 65 has a substantially circular large-diameter penetrating portion 65a having a size to penetrate the head 66b of the screw member 66, and a smaller diameter than the large-diameter penetrating portion 65a.
6 and a long groove fastening portion 65b having a width slightly larger than the threaded portion 66c and extending in the circumferential direction of the flange portion 11c.

The elevating table 41 of the conveying means 40 has a rectangular plate shape, the fitting projection 41a is formed at the center thereof, and the spin motor 42 is mounted on the lower surface thereof, and its drive shaft is provided. 43 protrudes upward from the center of the fitting protrusion 41a on the upper surface. A connection protrusion 44 extending in the radial direction is formed on the upper end surface of the drive shaft 43. The connecting projections 44 together with the connecting grooves 62 constitute a detachable connecting means.

Opening the shutter 8 shown in FIG.
By driving the spin motor 42 fixed to the lower surface of the lift table 41 in a state where the sample S is desired inside,
The X-ray analysis is performed while rotating the sample table 12 in the sample cup 10 and rotating the sample holder H mounted on the sample table 12, that is, the sample S.

The seal member 16 of the sample cup 10 contacts the lower end of the peripheral wall 4 of the preliminary exhaust chamber 3 to keep the interior of the preliminary exhaust chamber 3 airtight. A sample holder retainer 56, which is a stopper for positioning the sample holder H in the height direction, is rotatably supported by a bearing 58 above the inner diameter surface of the peripheral wall 4, and the sample holder retainer 56 is Hold down so as not to hinder rotation during analysis.

The preliminary exhaust chamber 3 is connected to a vacuum pump 50 through a communication hole 49 formed in the peripheral wall 4 thereof.
The interior of the analysis chamber 2 and the preliminary exhaust chamber 3 is evacuated by the vacuum pump 50 via the on-off valves V1 and V2. When the degree of vacuum in the preliminary exhaust chamber 3 becomes equal to the degree of vacuum in the analysis chamber 2, the shutter 8 is opened and the sample S is analyzed. When the analysis of the sample S is completed, the shutter 8 is closed, the inside of the preliminary exhaust chamber 3 is returned to the atmospheric pressure, and the peripheral wall 4 of the preliminary exhaust chamber 3 is opened.
The sample cup 10 is separated from the sample cup, and the sample cup 10 is transported to the sample entrance 20 (see FIG. 1) by the transport means 40.

Next, the sample changer 9 will be described with reference to FIGS. As shown in FIG. 1, the sample exchanger 9 includes an upper wall 31 of a hood (a part of the outer panel) 31 provided so as to cover an inlet 19 formed in the outer panel 1.
The sample carrying port 20 is formed in the upper wall 31a. The inside of the hood 31 forms a sample exchange chamber 35. The sample entrance 20 is connected to the sample exchange 9
It is opened and closed by moving. Sample exchange chamber 35
Is a sample cup 10 between the sample exchanger 9 and the inlet 19.
Has a height such that the whole of the can be accommodated.

As shown in FIG. 3, the sample changer 9 includes a base plate 21 and a movable plate 23 supported by a slide member 22 so as to be rotatable relative to the base plate 21. The sliding member 22 is an annular plate member fixed to the upper surface of the base plate 21 and having a portion corresponding to a later-described replacement port 21a cut out. The moving plate 23 is fixed to a shaft 33 rotatably supported by a bearing 32 attached to the center of the base plate 21. The base plate 21 has a slightly larger outer shape than the sample carrying port 20, and is rotatably attached to the hood 31 by a hinge 26 to open and close the sample carrying port 20. The hinge 26 is a hinge pin 26a.
And a fixed plate 26 which relatively rotates about a hinge pin 26a.
b and the rotating plate 26c. The fixing plate 26b is a hood 3
The rotating plate 26 c is fixed to the back surface of the upper wall 31 a and is attached to a support frame 27 fixed to the base plate 21. This support frame 27 is provided as a pair of left and right (FIG. 2).
reference).

As shown in FIG. 2, the base plate 21 has
In the moving plate 23, a plurality of (six in the illustrated example) fitting holes 23a are provided in the moving plate 23. The size of the exchange port 21a and the fitting hole 23a is slightly larger than the outer diameter of the sample holder S, and the sample holder S is held on the base plate 21 through the fitting hole 23a. Is carried to the exchange port 21a of the base plate 21 with the rotational movement of. As shown by the two-dot chain line in FIG.
It is lifted by the elevating table 41 of the transport means 40 and stands by. In a state where the sample cup 10 is on standby, the guide body 13 shown in FIG. 4 is pressed against the periphery of the exchange port 21 a on the lower surface of the base plate 21, so that the first spring body 14 is formed.
Retreats downward against the spring force of
The upper surface of the sample table 12 is substantially in agreement with the upper surface of the base plate 21. Therefore, the sample table 12 can easily receive the sample holder H sliding on the base plate 21.

The knob 3 provided at the upper end of the shaft 33
4 protrudes upward from the movable plate 23 via the neck 34a, and has a hexagonal shape having an outer diameter larger than that of the neck 34a. At the time of maintenance and inspection of the sample cup 10, the knob 34
The sample changer 9 is pivoted upward by pulling and lifting the sample, and the sample entrance 20 is opened. A large-diameter driven gear 36 provided at the lower end of the shaft 33 meshes with a driving gear 39 of a replacement driving device 38 composed of a motor fixed to a lower surface of the base plate 21 by a mounting bracket 37, and Under the control of the driving device 38 by 70, the moving plate 23 is rotated to move the sample holder H to a position corresponding to the exchange hole 21a. Sample holder H that has reached the exchange hole 21a
Move onto the sample table 12 of the sample cup 10 waiting at the exchange position facing the exchange hole 21a, and
By 0, it is conveyed to the preliminary exhaust chamber 3.

When the measurement of the sample S is completed, the sample holder H holding the sample S is supported by the sample cup 10 and transported by the transport means 40, enters the sample exchange chamber 31 through the introduction port 19, and moves to the base. The sample holder H is pushed up from the exchange hole 21a of the plate 21 and the fitting hole 23a of the moving plate 23. At this time, as described above, the upper surface of the sample table 12 is substantially coincident with the upper surface of the base plate 21, and the movable plate 23 is rotated by the driving device 38,
The measured sample holder H is smoothly moved to a position outside the exchange hole 21a.

In the above-described configuration, the sample holder H holding the sample S shown in FIG. Is transported to and from a preliminary exhaust position that forms the lower part of The new sample S, which is held in the sample holder H, is placed on the sample exchanger 9 by manual or automatic transfer so as to be fitted into the fitting hole 23a of the moving plate 23 of the sample exchanger 9, and In operation, they are sequentially delivered to the sample cup 10 and carried to the preliminary exhaust chamber 3. The sample holder H holding the measured sample S is supported by the sample cup 10, and the sample exchange 9
Through the exchange hole 21a.

The sample cup 10 from which the sample holder H has been drawn out
When the maintenance / inspection is performed, the knob 34 of the sample exchanger 9 shown in FIG. 3 is pinched, and the sample exchanger 9 is rotated as shown by a two-dot chain line to open the sample entrance 20. At this time, the rotation driving mechanism including the driving device 38 for rotating the moving plate 23 also rotates upward together with the base plate 21, so that a large space is created inside the sample exchange chamber 35. In this state, the sample cup 10 shown in FIG.
5 is loosened, and the sample cup 10 is rotated about the vertical axis on the elevating table 41 by hand, so that the large-diameter through-hole 65a of the attaching / detaching hole 65 shown in FIG. Withdraw the sample cup 10 upward. The sample cup 10 thus removed is cleaned outside the apparatus. The cleaning may be performed while the sample cup 10 is attached to the elevating table 41. As described above, since the sample exchange 9 can be moved to open the sample carry-in port 20, the maintenance and inspection of the sample cup 10 becomes easy.

The cleaned sample cup 10 is placed on the lift 41
4A, the fitting groove 11e of the sample cup 10 is fitted to the movable table 41 while the connecting groove 62 of the rotating shaft 61 shown in FIG. Fit into the joint projection 41a. Thus, sample cup 1
0 with the cup body 1
5 is rotated about the vertical axis, the large-diameter through-hole 65 a of the mounting hole 65 shown in FIG. 5 is inserted through the head 66 b of the screw body 66, and the sample cup 10 is placed on the movable table 41. Further, the sample cup 10 is rotated so that the screw body 66 is inserted into the narrow narrow groove fastening portion 65b, and the screw body 66 is tightened with a tool to fix the sample cup 10 to the lift table 41.

Here, if a plurality of sample cups 10 are prepared and the sample cups 10 are replaced at the time of maintenance and inspection, the next analysis operation can be performed without interrupting the analysis work. Therefore, there is no interruption time of the analysis work due to the maintenance / inspection work, and the work efficiency is further improved.

In the above embodiment, the X-ray fluorescence analyzer has been described.
It can be used for other X-ray analyzers such as a X-ray analyzer.

[0032]

According to the first aspect of the present invention,
Since the sample entrance is opened by moving the sample exchanger, maintenance and inspection of the sample cup can be easily performed. If the sample cup is made detachable with respect to the transport means, maintenance and maintenance should be performed with the sample cup removed.
Inspection work can be performed more easily.

[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 plan view showing a sample exchanger of the X-ray analyzer.

FIG. 3 is a sectional view taken along line III-III in FIG. 2;

FIG. 4 is a cross-sectional view showing a state where the sample cup of the X-ray analyzer is mounted on a lifting table.

FIG. 5 is a perspective view of a main part showing a connection structure between the sample cup and a lift table.

FIG. 6 is a sectional view showing an analysis chamber and a preliminary exhaust chamber of the X-ray analyzer.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... Exterior panel, 2 ... Analysis room, 3 ... Preliminary exhaust room, 6 ... X
Wire tube, 9 ... Sample exchange machine, 10 ... Sample cup, 20 ... Sample entrance, 21 ... Base plate, 21a ... Exchange hole, 23 ... Movement plate, 38 ... Driver for exchange, 40 ... Transportation means, 41 ... Table, 42 ... Spin motor, H ... Sample holder, S ... Sample

Claims (3)

(57) [Claims] 1. A sample holder which is arranged at a sample carrying-in port of an X-ray analyzer and has an exchange hole and holds a sample, forms a part of a preliminary vacuum chamber in the X-ray analyzer from the exchange hole. A sample exchange device that receives a sample holder drawn out of the sample cup through the exchange hole while transferring the sample holder to the sample cup, wherein the sample in the X-ray analyzer is movably set to open and close the sample loading port. switch. 2. The method according to claim 1, wherein the base plate having the exchange hole, a movable plate that is set to be movable with respect to the base plate and moves a plurality of sample holders on the base plate, And a drive for driving the sample holder to a position corresponding to the exchange hole. 3. The X-ray analyzer according to claim 1, wherein the sample cup supporting the sample holder forms a part of a preliminary exhaust chamber adjacent to an analysis chamber for irradiating the sample with X-rays. X is provided with a transport unit for transporting between an exhaust position and an exchange position facing the sample loading port, wherein the sample cup is detachably set to the transport unit.
Sample changer in X-ray analyzer.