JP2005345442A - Fluorescent x-ray analyzing liquid sample vessel - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a fluorescent X-ray analyzing liquid sample vessel, using an upper face irradiation, having a flat analysis window which does not have air in the inside, and being filled easily with the liquid sample so as to reduce the quantity of air as a whole within the vessel. <P>SOLUTION: The fluorescent X-ray analyzing liquid sample vessel is filled with the liquid sample 7, has primary X rays 11 irradiated from above, conducts fluorescent X-ray analysis, and is provided with a cylindrical body 1; an upper locking member 4 for detachably attaching the analysis window 3 comprising a film for transmitting the X-rays to the upper opening of the body 1, and a lower locking member 6 for detachably attaching a bottom 5 comprising a film to the lower opening of the body 1. The body 1 has a partition 2, provided centrally with a hole 2a, having a downward umbrella shape. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to a container for filling a liquid sample and irradiating primary X-rays from above to perform fluorescent X-ray analysis.

  X-ray fluorescence analysis includes upper surface irradiation that irradiates primary X-rays from above the sample and lower surface irradiation that irradiates primary X-rays from below the sample. In the case of upper surface irradiation, an X-ray tube is used. Because important parts such as detectors and other optical systems are above the sample, even if a sample that is powder or liquid spills during measurement, the damage and damage are not significant There is.

  As a first liquid sample container for X-ray fluorescence analysis by upper surface irradiation, there is the one shown in the cross-sectional view of FIG. 7 (for simplicity, hatching is applied only to the liquid sample. The same applies to other drawings). This container is filled with the liquid sample 7 as follows. First, as shown in FIG. 8, the liquid sample 7 is introduced from the opening of the bottomed cylindrical main body 21 to the edge of the opening. In order to remove bubbles, which will be described later, inside the main body 21, a partition portion 2 having a downward umbrella shape (conical side surface with the apex down) and a hole 2 a in the center is provided. As a result, a considerable amount of air 8b accumulates below the partition portion 2.

  Next, as shown in FIG. 9, the analysis window 3 made of a film that transmits X-rays can be detachably attached to the opening of the main body 21 using a ring-shaped locking member 4 that fits outside the main body 21. Install. That is, the analysis window 3 that is a circular film having a diameter slightly larger than the outer diameter of the main body 21 is placed so as to cover the opening of the main body 21, and the locking member 4 is fitted to the outside of the main body 21 from above. Thus, the peripheral portion 3 a of the analysis window 3 is sandwiched between the locking member 4 and the main body 21, and the analysis window 3 is attached to the opening of the main body 21. At this time, for the correct X-ray fluorescence analysis, the analysis window 3 should be flat (with no wrinkles, no bulges, no dents, and no tension), and attached so that there is no air inside. It is not easy, and some air bubbles (air) 8c often enter inside even if it is mounted flat.

  Therefore, as shown in FIG. 10, the container is turned upside down so that the bubbles 8c pass through the holes 2a of the partition part 2, and the container is slightly tilted to move the bubbles 8c upward along the inner surface of the bottom (in the direction of the arrow). 7 and integrated with the air 8b that has been under the partition 2, and the container is turned upside down again so that the air does not pass through the hole 2a, as shown in FIG. The entire air 8 is accumulated below the partition 2. If such an operation called bubble removal is performed, there is no air that attenuates the X-rays immediately below the analysis window 3, so that the fluorescent X-ray analysis by the upper surface irradiation can be performed correctly.

Further, Patent Document 1 discloses a second liquid sample container for fluorescent X-ray analysis by upper surface irradiation, which is different from this container.
JP 2001-255289 A

  However, in the first conventional liquid sample container, the air 8b tends to accumulate on the lower side of the partition part 2 when the liquid sample 7 is put (FIG. 8), and bubbles 8c also enter when the analysis window 3 is attached. Since it is easy (FIG. 9), the amount of the whole air 8 inside the container is large, and even if air bubbles are removed, it is not easy to collect the whole air 8 inside the container below the partition part 2. The amount of the entire air 8 inside the container may exceed the amount stored below the partition 2, and in such a case, air remains immediately below the analysis window 3 and correct analysis cannot be performed. Therefore, the filling operation must be repeated.

  Moreover, it is not easy even for a skilled person to attach the analysis window 3 flatly while keeping the liquid sample 7 as far as the edge of the opening as small as possible so that the bubbles 8c do not enter. Even if it is mounted flat, a considerable amount of air 8 accumulates on the lower side of the partition part 2 as described above, so that if it expands due to a rise in temperature during measurement, the analysis window 3 protrudes and becomes not flat. The distance between the detector and the liquid sample 7 is changed, so that the analysis becomes inaccurate, and there is a possibility that the detector bursts.

  On the other hand, in the conventional second liquid sample container, there is no space for storing air by escaping from just below the analysis window (X-ray transmission sheet). I have to start over.

  The present invention has been made in view of the above-described conventional problems. In a liquid sample container for fluorescent X-ray analysis by upper surface irradiation, the analysis window is flat and there is no air inside, and the total amount of air inside the container is also large. An object of the present invention is to provide a liquid sample that can be easily filled so that there are few.

  In order to achieve the above object, a first configuration of the present invention is a container for filling a liquid sample and irradiating primary X-rays from above to perform fluorescent X-ray analysis, which includes a cylindrical main body, An upper locking member for detachably attaching an analysis window made of a film that transmits X-rays to the upper opening of the main body, and a bottom made of film for detachably attaching to the lower opening of the main body A lower locking member. And the said main body has a partition part provided with the hole in the center in the shape of a downward umbrella.

  If the liquid sample container for X-ray fluorescence analysis of the 1st structure is used, after attaching an analysis window to an upper side opening part first, a main body can be turned upside down and a liquid sample can be put in from a lower side opening part. At this time, since the partition portion faces upward, air does not accumulate inside the container unlike the conventional first container. And when attaching a bottom part to a lower side opening part, since it is not necessary to attach flatly unlike an analysis window, since an operator can concentrate on only making it not enter a bubble, it is hard to enter a bubble. Even if air bubbles of the same degree as when the analysis window is attached to the first conventional container are entered, since there is no air accumulated in the container before that, the work of removing the air bubbles is performed easily and reliably. The amount of air that accumulates on the lower side of the partition is very small due to bubbles.

  In addition, the analysis window can be attached before the liquid sample is put, and in this case, since there is no problem of air bubbles mixing, the operator can concentrate on attaching it flatly, so it is easy to attach it flatly. As described above, according to the liquid sample container for fluorescent X-ray analysis of the first configuration, it is easy to prepare a liquid sample so that the analysis window is flat, there is no air inside, and the total amount of air inside the container is small. Can be filled.

  A second configuration of the present invention is a container for filling a liquid sample, irradiating primary X-rays from above and performing fluorescent X-ray analysis, and having a cylindrical main body and an upper opening of the main body, An upper locking member for detachably attaching an analysis window made of a film that transmits X-rays, and a detachable bottom portion at the lower opening of the main body. And the said main body has a partition part provided with the hole in the center in the shape of a downward umbrella. Also according to the second configuration of the present invention, the same effect as the first configuration can be obtained.

  Hereinafter, the liquid sample container of the first embodiment of the present invention will be described with reference to the drawings. As shown in FIG. 1, this container is filled with a liquid sample 7 and placed on a sample stage 9, and irradiated with primary X-rays 11 from an X-ray source 10 such as an upper X-ray tube, A container for analyzing fluorescent X-rays 12 generated by a detection means 13 such as a detector, from a film that transmits X-rays to a cylindrical main body 1 and an upper opening of the main body 1 An upper locking member 4 for detachably attaching the analysis window 3 and a lower locking member 6 for detachably attaching the bottom 5 made of a film to the lower opening of the main body 1 are provided. And the main body 1 has the partition part 2 by which the hole 2a was provided in the center in the downward umbrella shape.

  In the first embodiment and the second embodiment to be described later, the main body 1 includes a cylindrical outer side portion 1a and a cylindrical inner side portion 1b that fits inside the outer side portion 1a. The partition portion 2 is integrally formed on the inner side portion 1b. However, the present invention is not so limited, and for example, the entire main body including the partition portion may be integrally formed.

  The upper locking member 4 has a ring shape fitted to the outside of the main body 1, and the analysis window 3 is separated from the main body 1 by sandwiching the peripheral portion 3 a of the analysis window 3 between the upper locking member 4 and the main body 1. 1 is attached. Similarly, the lower locking member 6 has a ring shape that is fitted to the outside of the main body 1, and the peripheral portion 5 a of the bottom 5 is sandwiched between the lower locking member 6 and the main body 1, so that the bottom portion 5 is attached to the main body 1.

  The main body 1, the upper locking member 4, and the lower locking member 6 are made of, for example, polypropylene or polyethylene.

  The film used as the analysis window 3 has a material and a thickness selected according to the characteristics of the liquid sample 7 and the fluorescent X-ray to be measured. For example, the film is made of polyester, polypropylene, polyimide, or the like. The film used as the bottom part 5 does not need to consider the X-ray permeability, and is only required to have resistance to the liquid sample 7 and mechanical strength. May be.

  This container is filled with the liquid sample 7 as follows. First, as shown in FIG. 2, an analysis window 3, which is a circular film having a diameter slightly larger than the outer diameter of the main body 1, is placed so as to cover the upper opening of the main body 1. By fitting to the outside of the main body 1, the peripheral portion 3 a of the analysis window 3 is sandwiched between the upper locking member 4 and the main body 1, and the analysis window 3 is attached to the upper opening of the main body 1. At this time, it is before the liquid sample is put in, and there is no problem of air bubbles mixing, so the operator can concentrate on attaching it flatly (no wrinkles, no bulges, no dents, and no tension) The analysis window 3 can be easily mounted flat.

  Next, as shown in FIG. 3, the container is turned upside down, and the liquid sample 7 is inserted from the lower opening (located on the upper side in FIG. 3) to the edge of the lower opening. At this time, since the partition portion 2 faces upward, air does not accumulate inside the container unlike the conventional first container.

  Next, as shown in FIG. 4, the bottom portion is a circular film having a diameter slightly larger than the outer diameter of the main body 1 so as to cover the lower opening of the main body 1 (located on the upper side in FIG. 4). 5, and the lower locking member 6 is fitted to the outside of the main body 1 from above, so that the peripheral portion 5 a of the bottom 5 is sandwiched between the lower locking member 6 and the main body 1. Attach the bottom 5 to the lower opening. When attaching the bottom 5, unlike the analysis window 3, it is not necessary to attach it flat, so the operator can focus only on preventing bubbles from entering, so bubbles are difficult to enter, but bubbles 8 a still enter. In such a case, air bubbles can be removed as follows.

  As shown in FIG. 5, the container is slightly tilted upside down, and the bubbles 8a are moved upward (in the direction of the arrows) along the inner surface of the bottom 5 to collect them at the corners so that the air does not pass through the holes 2a. However, the container is turned upside down again, and the entire air 8 inside the container is accumulated below the partition 2 as shown in FIG. By removing the bubbles, there is no air that attenuates the X-rays immediately below the analysis window 3, so that the fluorescent X-ray analysis by the upper surface irradiation can be correctly performed.

  As described above with reference to FIG. 4, when the bottom portion 5 is attached to the lower opening of this container, bubbles are difficult to enter, but the same amount of bubbles as when the analysis window is attached to the first conventional container. Even if 8a enters, since there is no air accumulated in the container before that, the air bubble removal operation from the state of FIG. 5 to the state of FIG. 1 can be performed easily and reliably. Further, the air 8 that accumulates on the lower side of the partition portion 2 is also a very small amount corresponding to the bubbles 8a (FIGS. 4 and 5) that are entered when the bottom portion 5 is attached. However, the analysis window 3 hardly protrudes and is not flat. Therefore, the distance between the detection means 13 and the liquid sample 7 is not changed and the analysis is not inaccurate, and there is no possibility of rupture.

  As described above, according to the liquid sample container for X-ray fluorescence analysis of the first embodiment, the liquid is used so that the analysis window 3 is flat and there is no air inside, and the total amount of air 8 inside the container is small. The sample 7 can be easily filled. Although the analysis window 3 and the bottom 5 made of film are disposable, the main body 1, the upper locking member 4 and the lower locking member 6 constituting the container of the first embodiment can be repeatedly used by washing or the like. .

  Next, a liquid sample container according to a second embodiment of the present invention will be described. The container according to the first embodiment of FIG. 1 includes a lower locking member 6 for detachably attaching a bottom 5 made of a film to the lower opening of the main body 1, whereas the container according to the second embodiment As shown in FIG. 6, the difference is that a detachable cap-like bottom 15 is provided in the lower opening of the main body 1, but the other configurations are the same, so the same parts are denoted by the same reference numerals. Is omitted. The bottom portion 15 is made of, for example, polypropylene, polyethylene, etc., like the main body 1 and the upper locking member 4.

  In filling the liquid sample 7, in the container of the first embodiment of FIG. 4, the peripheral portion 5 a of the bottom portion 5 made of a film is sandwiched between the lower locking member 6 and the main body 1 to While the bottom 5 is attached to the side opening, the container of the second embodiment is different in that the cap-like bottom 15 (FIG. 6) is fitted to the lower opening of the main body 1, but the other procedures are the same. Yes, the same effect as the container of the first embodiment can be obtained. Although the analysis window 3 made of a film is disposable, the main body 1, the upper locking member 4 and the bottom 15 constituting the container of the second embodiment can be repeatedly used by washing.

It is a longitudinal cross-sectional view which shows the liquid sample container for fluorescent X-ray analysis of 1st Embodiment of this invention. It is a longitudinal cross-sectional view which shows the state at the time of attaching an analysis window to a main body in the container. It is a longitudinal cross-sectional view which shows the state at the time of putting a liquid sample in the container. It is a longitudinal cross-sectional view which shows the state at the time of attaching a bottom part to a main body in the container. It is a longitudinal cross-sectional view which shows the state at the time of performing bubble extraction in the container. It is a longitudinal cross-sectional view which shows the liquid sample container for fluorescent X-ray analysis of 2nd Embodiment of this invention. It is a longitudinal cross-sectional view which shows the conventional 1st liquid sample container for fluorescent X-ray analysis. It is a longitudinal cross-sectional view which shows the state at the time of putting a liquid sample in the container. It is a longitudinal cross-sectional view which shows the state at the time of attaching an analysis window to a main body in the container. It is a longitudinal cross-sectional view which shows the state at the time of performing bubble extraction in the container.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Main body 1a Outer side part 1b Inner side part 2 Partition part 2a Partition part hole 3 Analysis window 3a Analysis window peripheral part 4 Upper locking member 5,15 Bottom part 5a Bottom peripheral part 6 Lower locking member 7 Liquid sample 11 Primary X-ray

Claims (5)

A container for filling a liquid sample and irradiating primary X-rays from above to perform X-ray fluorescence analysis,
A cylindrical body;
An upper locking member for detachably attaching an analysis window made of a film that transmits X-rays to the upper opening of the main body,
A lower locking member for detachably attaching a bottom made of a film to the lower opening of the main body,
A liquid sample container for X-ray fluorescence analysis, wherein the main body has a partition portion having a downward umbrella shape and a hole in the center. A container for filling a liquid sample and irradiating primary X-rays from above to perform X-ray fluorescence analysis,
A cylindrical body;
An upper locking member for detachably attaching an analysis window made of a film that transmits X-rays to the upper opening of the main body,
A detachable bottom portion in the lower opening of the main body,
A liquid sample container for X-ray fluorescence analysis, wherein the main body has a partition portion having a downward umbrella shape and a hole in the center. In claim 1 or 2,
The upper locking member has a ring shape that fits to the outside of the main body, and the analysis window is attached to the main body by sandwiching a peripheral portion of the analysis window between the upper locking member and the main body. A liquid sample container for fluorescent X-ray analysis attached. In claim 1,
The lower locking member has a ring shape that fits to the outside of the main body, and the bottom portion is sandwiched between the lower locking member and the main body so that the bottom portion is attached to the main body. A liquid sample container for fluorescent X-ray analysis attached. In any one of Claims 1 thru | or 4,
The fluorescent X-ray in which the main body includes a cylindrical outer side portion and a cylindrical inner side portion fitted inside the outer side portion, and the partition portion is integrally formed on the inner side portion. Liquid sample container for analysis.

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