JP3268977B2 - X-ray fluorescence analyzer - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an X-ray analysis for irradiating a sample with primary X-rays to detect fluorescent X-rays generated from the sample, and to appropriately maintain the temperature during detection in accordance with the sample. Accordingly, the present invention relates to an X-ray analyzer capable of performing more accurate analysis.

[0002]

2. Description of the Related Art A conventional X-ray fluorescence spectrometer has no means for maintaining the temperature during the detection of a sample, and is irradiated with primary X-rays during the detection. , For example, about 50 degrees (Centigrade, hereinafter the same).

[0003]

However, the inventor of the present invention, when detecting the fluorescent X-ray intensity of a specific element generated from a certain alloy while heating the sample and measuring the temperature, obtains the normal temperature (26 degrees). It was found that the strength decreased with increasing temperature, and the strength was not stabilized until the temperature reached about 72 degrees. This is presumed to be due to a change in the state of the crystal structure and the like of the sample from room temperature to about 72 degrees .

[0004] ie, the sample is said to as certain <br/> alloy, the temperature rise in the detection, fluorescent X-ray intensity changes that occur. Therefore, in a conventional X-ray fluorescence spectrometer that does not control the temperature of a sample during detection, comparison between samples cannot be performed, and accurate quantitative analysis cannot be performed.

SUMMARY OF THE INVENTION The present invention has been made in view of the above-mentioned conventional problems. In an X-ray analysis for irradiating a sample with primary X-rays and detecting secondary X-rays generated from the sample, detection is performed according to the sample. An object of the present invention is to provide an X-ray analyzer capable of performing more accurate analysis by appropriately maintaining the temperature inside.

[0006]

In order to achieve the above object, an X-ray fluorescence spectrometer according to claim 1 comprises a heating means for heating a sample before detection, and a method for setting the temperature of the sample during detection to a predetermined temperature or higher. so as to maintain, and a control means for controlling the heating means.

According to the first aspect of the present invention, the sample is heated before the detection so that the temperature of the sample being detected is maintained at an appropriate predetermined temperature or higher in accordance with the sample. The line intensity is stable, and more accurate analysis can be performed .

The X-ray fluorescence analyzer according to claim 1 is a
Airtight sample chamber where the sample is irradiated with primary X-rays, and the sample chamber
Selection means for selecting a sample to be carried into the
The heating means faces the sample placed on the selection means.
It is provided in the place.

According to the first aspect of the present invention, the intensity of the generated fluorescent X-rays is stabilized without much complicated structure, and more accurate analysis can be performed.

[0010]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, an X-ray fluorescence analyzer according to one embodiment of the present invention will be described with reference to the drawings. First,
The loading and unloading of a sample by the X-ray fluorescence analyzer will be described. In FIG. 1, a plurality of sample cups (transported objects) 11 are placed on a table 10 on the left side of the drawing, and by rotating the table 10, the sample cup at the stock position P1 is rotated.
11 is transferred to the loading / unloading position P2. A sample 12 is built in the sample cup 11 as shown by a broken line. That is, the table 10 is a selecting means 10 for selecting the sample 12 to be carried into the sample chamber 15 described later. The first transfer device 13 on the right side of the table 10 is provided with first lids 18 at the ends of two arms 13a, respectively. Inside the first lid 18, a handling unit 14 for gripping the sample cup 11 is provided. The first transfer device 13 transfers the sample cup 11 between the carry-in / out position P2 and a preliminary vacuum chamber 20, which will be described later, when the arm 13a is driven to move up and down and pivot.

A sample chamber 15 is provided on the right side of the first transfer device 13, and further on the right side of the sample chamber 15 is a sample chamber.
A spectroscopic chamber 31 in communication with 15 is provided adjacent to the spectroscopic chamber. The sample chamber 15 and the spectroscopic chamber 31 are formed by a vacuum vessel 16 and are airtight vacuum chambers.

A loading / unloading port 17 for loading / unloading the sample cup 11 into / from the sample chamber 15 is formed in the upper left portion of the sample chamber 15. Below the loading / unloading port 17, a second lid 19 is provided which opens and closes the loading / unloading port 17 by moving up and down. The first and second lids 18 and 19 are pressed against the outer surface and the inner surface of the vacuum vessel 16 around the carry-in / out port 17 to form a preliminary vacuum chamber 20.

In the lower part of the sample chamber 15, a second transfer device
23 includes a pair of second lids 19, a pair of elevating rods 22,
And a turret 21. The second lid 19 constitutes a saucer-shaped handling unit that places the sample cup 11 and transfers the sample cup 11. The turret 21 has a mounting portion 21a on which the pair of second lids 19 are mounted, and a through hole (not shown) is formed in the center of the mounting portion 21a. The lifting rod 22 vertically penetrates through the through holes of the vacuum vessel 16 and the turret 21 to move the second lid 19 up and down. A vacuum seal is provided on the contact surface between the lids 18 and 19 and the vacuum container 16.

An X-ray tube 30 as an X-ray source has its tip inserted into the sample chamber 15 and emits primary X-rays B1 toward the sample 12. The incident primary X-ray B1 excites atoms of the sample 12 to generate fluorescent X-rays B2 unique to the element. The fluorescent X-rays B2 from the sample 12 pass through a solar slit 32 in an analysis chamber 31, are then separated by a spectroscope 33, are incident on a detector 34, and are detected. Based on this detected value, as is well known, the sample 12
Is subjected to elemental analysis.

Next, the loading operation of the sample cup 11 will be described. In advance, the second lid 19 is set in a state in which the sample cup 11 is not placed, and
Is pressed against the inner surface of the surrounding area. As a result, the loading / unloading port 17
Is closed, and the sample chamber 15 is kept in a vacuum state.

The sample cup 12 is transferred from the stock position P1 to the carry-in / out position P2 by turning the table 10. Thereafter, the arm 13a of the first transfer device 13 descends,
After gripping the sample cup 11 with the handling unit 14, the arm
The sample cup 11 is raised, turned, and lowered, and the sample cup 11 is carried into the preliminary vacuum chamber 20. At the same time, the first lid 18 is
As a result, the preliminary vacuum chamber 20 is closed as shown in FIG.

Thereafter, the inside of the preliminary vacuum chamber 20 is evacuated, and the first lid 18 releases the gripping of the sample cup 11 and
The sample cup 11 is transferred onto the second lid 19.

Thereafter, the left lifting rod 22 descends,
The second lid 19 is placed on the turret 21. After this placement, the turret 21 turns, the right elevating rod 22 rises, and the sample cup 11 is transferred together with the second lid 19 to the analysis position P3. That is, the turret 21 is a moving unit 21 that moves the sample 12 in the sample chamber 15 in the horizontal direction. After the transfer, a predetermined elemental analysis is performed. Note that the carry-out operation is performed simultaneously with the carry-in operation, but is similar to the carry-in operation, and a detailed description thereof will be omitted.

In the X-ray fluorescence analyzer of this embodiment, before the detection of the fluorescent X-rays B2 from the sample 12 by the detector 34, that is, the sample cup 11 and the second lid 19 are still in the turret 21. When it is on the top, the heating means 1 such as an infrared lamp, a nichrome wire or a ribbon heater for heating the sample 12
, For example, as shown on the left side of FIG.
Auto sample changers (13, 18, 14, 10, etc.)
It is provided inside the lid 7 . Further, a control means for controlling the heating means 1 before detection so that the temperature of the sample 12 being detected (at the analysis position P3) is maintained at a predetermined temperature or higher.
Step 5 is provided. The control means may include a temperature sensor or the like for measuring the temperature of the sample 12 being heated .

According to the X-ray fluorescence spectrometer of this embodiment, the sample 12 is heated before detection so that the temperature of the sample 12 being detected is maintained at an appropriate predetermined temperature or higher in accordance with the sample 12. Therefore, even in the case of the sample 12 whose intensity is not stabilized until the temperature reaches a predetermined temperature, such as the above-mentioned kind of alloy, the intensity of the generated fluorescent X-ray is stabilized, and accurate analysis can be performed .

[0021]

As the following description, according to the present invention, the apparatus according to the appended claims 1, depending on the sample, so that the temperature of the sample in the detection is maintained above the appropriate predetermined temperature, the sample prior to detection Is heated, the intensity of the generated fluorescent X-rays is stabilized, and more accurate analysis can be performed .

Further, without significant complicating structure, the fluorescent X-ray intensity generated is stabilized, it is possible to perform a more accurate analysis.

[Brief description of the drawings]

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

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... Heating means, 5 ... Control means, 10 ... Selection means (table), 11 ... Sample cup, 12 ... Sample, 15 ... Sample chamber, 21 ... Transfer means (turret), 30 ... X-ray source, 34 ... Detector , B1…
Primary X-ray, B2 ... X-ray fluorescence.

────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Hisayuki Kono 14-8 Akaoji-cho, Takatsuki-shi, Osaka Rigaku Denki Kogyo Co., Ltd. (56) References JP-A-5-157711 (JP, A) JP-A-8-54358 (JP, A) JP-A-1-296149 (JP, A) JP-A 61-40646 (JP, U) JP-A 63-188553 (JP, U) Int.Cl. ⁷ , DB name) G01N 23/00-23/227 G01N 1/00-1/44

Claims (1)

(57) [Claims] And 1. A X-ray source for incident primary X-ray to the sample, a fluorescent X-ray analysis apparatus provided with a detector for detecting the fluorescent X-ray generated from the sample, the sample prior to the detection heating means for heating to maintain the temperature of the sample in the detection above a predetermined temperature, and control means for controlling the heating means, and gas-tight sample chamber sample is irradiated with the primary X-rays, Selecting means for selecting a sample to be carried into the sample chamber;
Wherein the heating means, facing the placed sample to the selection means
X-ray fluorescence analyzer provided at the position .