JPH07260646A - Sample container - Google Patents

Abstract

PURPOSE:To provide a sample container in which an X-ray transmissive window is protected against bulging or fracture by preventing the air from being mixed with a sample in a hermetically sealed chamber defined within the sample container. CONSTITUTION:The sample container comprises a sample reservoir 21 and a cover 22 being applied thereto. A hermetically sealed chamber SC is defined between the sample reservoir 21 and the cover 22 with a pair of X-ray transmissive windows 8a, 9a being provided as the borders. The depth of the sample reservoir 21 is set such that all surfaces defining the hermetically sealed chamber SC come closer to the bottom side than the edge 21a of opening in the sample reservoir 21 when the cover 22 is applied thereto. The cover 22 is provided with a channel 221 communicating between the chamber SC and the outside. The channel 221 can be closed by a closing member 23.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sample container for an X-ray microscope used for observing biological samples.

[0002]

2. Description of the Related Art In a conventional high resolution electron microscope, cells,
The internal structure and functions of bacteria, sperm, chromosomes, mitochondria, flagella, etc. cannot be observed in the living body. In addition, conventional microscopes using visible light cannot perform observation with high resolution. Therefore, by using soft X-rays (wavelength λ = about 2 to 5 nm) instead of normal visible light (wavelength λ = about 400 to 800 nm) used by a visible light microscope, the resolution is higher than before and Development of an X-ray microscope that allows observation as a living body is underway.

FIG. 6 is a schematic configuration diagram of an X-ray microscope. As shown in the figure, the X-ray microscope has a configuration in which an illumination optical system 2, a sample container 3, a magnifying optical system 4, and an imaging device 5 are arranged in series on the output optical axis of the X-ray generator 1. It is housed in a vacuum container 6 having an exhaust device 7 in order to prevent absorption of In such an X-ray microscope, after setting a sample capsule (not shown) in the sample container 3, the inside of the vacuum container 6 is evacuated by the evacuation device 7. The soft X-ray beam emitted from the X-ray generator 1 is converged by the illumination optical system 2, and the sample container 3
Pass the sample in the sample capsule set to. The transmission image of the sample is magnified by the magnifying optical system 4, and the imaging device 5
Is imaged.

FIG. 7 is a sectional view of a conventional sample container. In this sample container, a spacer 10 is interposed between two chips 8 and 9 having X-ray transmission windows 8a and 9a, and a culture solution 11 containing an observation sample is loaded inside the spacer 10. The sample tank lid 12 and the sample tank 13 are fixed by screws 14, and press the chips 8 and 9 in opposite directions via an O-ring 15.
Further, the inside of the sample container is closed by the O-ring 16. As a result, the inside of the sample container is shut off from the vacuum, and the biological sample containing water can be observed even in the vacuum container 6. In the following, a combination of the chips 8 and 9 and the spacer 10 is particularly called a sample capsule CP. The X-ray transmission window material is formed of silicon nitride or the like, which has relatively low X-ray absorption and is excellent in film strength.

[0005]

In the sample container described above, after the chip 9 is installed in the sample tank 13, the sample tank 13 is
A culture solution containing a sample is dropped into the inside of the container, and the chip 8 and the sample tank lid 12 are stacked in this order to seal the inside of the sample container. However, since the chip 8 is exposed to the upper side of the liquid surface of the culture solution 11 when the sample tank lid 12 is stacked, air is mixed with the culture solution 11 in the sealed space inside the O-ring 16. Therefore, when the sample container is installed in the vacuum container 6 and vacuum exhaust is performed, the X-ray transmission windows 8a and 9a are inflated due to the atmospheric pressure difference between the atmospheric pressure and the vacuum of the vacuum container 6, and as a result, at the X-ray transmission window position. The absorption amount of soft X-rays increases, and the resolution of the X-ray image decreases. Also, to expand the observation area, X
When the X-ray transmission window is enlarged, the X-ray transmission window may be damaged because it cannot withstand the pressure difference between the internal pressure of the sample container and the vacuum container 6.

An object of the present invention is to provide a sample container which can prevent air from being mixed into a sealed chamber of a sample defined in the sample container and prevent expansion and breakage of the X-ray transmission window.

[0007]

1 to 3 showing an embodiment, the present invention is provided with a sample tank 21 and a sample tank lid 22 superposed on the sample tank 21, Between the sample tank 21 and the sample tank lid 22, it is applied to a sample container in which a sealed chamber SC for the sample having a pair of X-ray transmission windows 8a and 9a as a boundary with the outside is defined. The depth of the sample tank 21 is set so that all the surfaces that define the sealed chamber SC enter the bottom side of the opening edge 21a of the sample tank 21 when the sample tank 21 and the sample tank lid 22 are overlapped. The above-described object is achieved by forming the communication passage 221 that establishes communication between the sealed chamber SC and the external environment in the sample tank lid 22 and providing the closing member 23 that closes the communication passage 221. In the invention of claim 2, in the sample container of claim 1, the surfaces of the sample tank 21 and the sample tank lid 22 that define the sealed chamber SC are subjected to a hydrophilic treatment. Referring to FIG. 5, in the invention of claim 3, in the sample container of claim 1 or 2, the elastically deformable pipe member 24 is connected to the communication passage 221 and the communication member 221 is sandwiched to form the communication passage 221. The closing member 25 is configured to close.

[0008]

When the sample tank lid 22 is overlaid after the sample tank 21 is filled with a liquid such as a culture solution, the sealed chamber SC is defined at a position where the sample tank 21 is completely submerged in the liquid. Excess liquid when the sample tank lids 22 are stacked is discharged to the outside through the communication passage 221. After this, if the communication passage 221 is closed by the closing member 23, the outside world and the sealed chamber SC are completely cut off. In the invention of claim 2, since the liquid such as the culture liquid is adapted to the surfaces of the sample tank 21 and the sample tank lid 22 (the thick line portion in FIG. 4) which have been subjected to the hydrophilic treatment and spread uniformly, the sample tank 21 and the sample tank The time and effort to remove the air bubbles attached to the lid 22 are reduced. In the invention of claim 3, since the pipe member 24 is sandwiched by the closing member 25 from the outside to close the communication passage 221, the closing member 25 and the liquid in the communication passage 221 do not come into contact with each other, and the air adhering to the closing member 25 is prevented. Mixing into the communication passage 221 is prevented.

Incidentally, in the section of means and action for solving the above-mentioned problems for explaining the constitution of the present invention, the drawings of the embodiments are used to make the present invention easy to understand. It is not limited to.

[0010]

【Example】

-First Embodiment- A first embodiment of the present invention will be described with reference to Figs. The same parts as those of the conventional example shown in FIG. 7 described above are designated by the same reference numerals and the description thereof is omitted. FIG. 1 shows a cross section of the sample container of this embodiment, in which 21 is a sample tank and 22 is a sample tank lid.
The sample tank 21 is formed with a fitting hole 210 for fitting with the sample tank lid 22, a storage hole 211 for the sample capsule CP, and an X-ray passage hole 212 coaxial with the X-ray transmission windows 8a and 9b of the sample capsule CP. Depth d of fitting hole 210 and storage hole 211
1 and d2 will be described later. The bottom surfaces 210a and 211a of the fitting hole 210 and the storage hole 211 have O-rings 16,
15 is attached. The sample tank lid 22 is formed with a fitting protrusion 220 that fits into the fitting hole 210 of the sample tank 21, and the O-ring 15 is attached to the end surface 220a thereof.

The sample tank lid 22 has a pressure relief hole 221 having one end opened to the end face 220a and the other end opened to the outer peripheral face 22a.
Are formed. The opening position of the pressure relief hole 221 on the end face 220a side is set inside the contact position of the end face 220a with the O-ring 16. A nozzle 222 is screwed into an opening position of the pressure relief hole 221 on the outer peripheral surface 22a side. When the cap 23 is screwed into the tip of the nozzle 222, the pressure relief hole 221 is closed. Reference numeral 224 is an X-ray passage hole of the sample tank lid 22.

In order to seal the sample capsule CP in the above sample container, the chip 8 of the sample capsule CP is mounted in the storage hole 211 of the sample tank 21, and the fitting hole 210 and the storage hole 2 are attached.
After filling 11 with the culture solution, the spacer 10 and the chip 9 are overlapped. Then, the nozzle 22 of the sample tank lid 22
After removing the cap 23 from 2, the fitting protrusion 220
The sample tank lid 22 is placed on the sample tank 21 while fitting the fitting hole 210 with the fitting hole 210. At this time, as shown in FIGS. 1 and 2, the depths of the fitting hole 210 and the storage hole 211 are set so that the end surface 220a of the sample tank lid 22 enters the bottom surface 210a, 211a side of the opening edge 21a of the sample tank 21. d1, d2
Is set. Therefore, when the sample tank lids 22 are overlapped, the entire area below the end surface 220a is filled with the culture solution. Therefore, when the sample tank 21 and the sample tank lid 22 are tightened with bolts (not shown) until the O-rings 15 and 16 are sufficiently bent as shown in FIG. 3, air is mixed between the sample tank 21 and the sample tank lid 22. A sealed chamber SC is defined that does not have This prevents the X-ray transmission windows 8a and 9a from being deformed or damaged due to the pressure difference between the sealed chamber SC and the outside.

As is apparent from FIGS. 2 and 3, when the sample tank lid 22 is placed on the sample tank 21 and the two are tightened, the volume in the O-ring 16 is reduced and a residual culture solution is produced. The excess culture solution is discharged to the outside of the sample container through the pressure relief hole 221. This prevents the internal pressure of the sealed chamber SC from rising due to the closing of the extra culture solution. The air in the pressure relief hole 221 is also discharged to the outside of the sample container as the surplus culture solution is discharged. After the sample tank 21 and the sample tank lid 22 are completely tightened, the cap 23 is screwed in to close the pressure relief hole 221 and completely shut off the sealed chamber SC and the external environment.

-Second Embodiment- A second embodiment of the present invention will be described with reference to FIG. The same parts as those of the first embodiment described above are designated by the same reference numerals and the description thereof will be omitted. In this embodiment, portions of the sample tank 21 and the sample tank lid 22 indicated by thick lines in FIG. 4, that is, the opening edge 21 a of the sample tank 21, the fitting hole 210 and the storage hole 211, and the fitting projection of the sample tank lid 22 are shown. The end surface 220a of the portion 220 and the opening edge 21
The entire surface (including the mounting groove surfaces of the O-rings 15 and 16) of the facing portion 22b facing a is hydrophilized.

In the above-described sample container of the first embodiment, when the sample tank lid 22 is overlapped with the minute bubbles adhering to the surfaces of the end face 220a and the fitting hole 210, air is mixed in the sealed chamber SC. For this reason, it is necessary to carefully remove the air bubbles adhering to the sample tank 21 and the like prior to stacking the sample tank lids 22. In this respect, in this embodiment, the culture solution is the sample tank 21.
Since it fits in the sample tank lid 22 and spreads evenly, the time and effort for removing air bubbles are reduced.

In the present embodiment, the surfaces 21a and 22b outside the O-ring 16 are also subjected to the hydrophilic treatment, but the minimum limit is the wall surface that defines the sealed chamber SC, that is, the O-ring in the sample tank 21. The sample tank lid 22 may be hydrophilized from the mounting groove of 15 to the mounting groove of the O ring 16 and from the mounting groove of the O ring 15 to the contact position with the O ring 16. The portion of the sample capsule CP that comes into contact with the culture solution may be hydrophilically treated.

-Third Embodiment- A third embodiment of the present invention will be described with reference to FIG. The same parts as those of the first embodiment described above are designated by the same reference numerals and the description thereof will be omitted. In this embodiment, a rubber tube 24 is connected to the end portion of the pressure relief hole 221 on the outer peripheral surface 22a side, and the rubber tube 24 is sandwiched by clips 25 to close the pressure relief hole 221.
In such an example, when the pressure relief hole 221 is closed, the culture solution inside does not come into contact with the clip 25. Therefore, there is no possibility that the air attached to the clip 25 will flow into the pressure relief hole 221. In the first embodiment, the air attached to the cap 23 may flow into the pressure relief hole 221, so it is necessary to take measures to remove the air attached to the cap 23 by immersing the cap 23 in the culture solution. In place of the rubber pipe 24, various elastically deformable pipe materials such as a vinyl pipe and a nylon pipe may be used.

In the above embodiment, the pressure relief hole 221 constitutes the communication passage, the cap 23 and the clip 25 constitute the closing member, and the rubber tube 24 constitutes the pipe material.

[0019]

As described above, according to the present invention, the sealed chamber of the sample can be closed at the position where the sample is completely submerged in the liquid, and the excess liquid when the sealed chamber is closed is connected to the communication passage. After the excess fluid has been discharged, the communication passage can be closed by the closing member to completely shut off the external chamber from the sealed chamber, so that the sealed chamber can be formed without the increase of the internal pressure due to the inclusion of air or the sealing of the excess fluid. Thus, the biological sample can be observed with an X-ray microscope with high resolution. According to the invention of claim 2, since the liquid such as the culture solution spreads evenly on the surfaces of the sample tank and the sample tank lid that have been subjected to the hydrophilic treatment, it is troublesome to remove the air bubbles adhering to the sample tank and the sample tank lid. It will be reduced. In the invention of claim 3, when the communication passage is closed, the closing member and the liquid in the communication passage do not come into contact with each other, so that the air adhering to the closing member is prevented from mixing into the communication passage, and the air to the sealed chamber is prevented. Can be more reliably prevented.

[Brief description of drawings]

FIG. 1 is a sectional view of a sample container according to a first embodiment of the present invention.

FIG. 2 is a cross-sectional view showing a state in which a sample tank lid 22 is covered on the sample tank 21 of FIG.

3 shows a sample tank 21 and a sample tank lid 22 from the state of FIG.
The figure which shows the state which fastened in the axial direction.

FIG. 4 is a sectional view of a sample container according to a second embodiment of the present invention.

FIG. 5 is a sectional view of a sample container according to a third embodiment of the present invention.

FIG. 6 is a conceptual diagram of a conventional X-ray microscope.

FIG. 7 is a cross-sectional view of a conventional X-ray microscope sample container.

[Explanation of symbols]

 8a, 9a X-ray transmission window 21 sample tank 21a sample tank opening edge 22 sample tank lid 23 cap 24 rubber tube 25 clip 221 pressure relief hole (communication passage) SC sealed chamber for sample

Claims (3)

[Claims] 1. A sample tank and a sample tank lid which is superposed on the sample tank, and a sample is sealed between the sample tank and the sample tank lid with a pair of X-ray transmission windows as a boundary with the outside. In a sample container in which a chamber is defined, when the sample tank and the sample tank lid are superposed on each other, all surfaces defining the sealed chamber enter the bottom side of the opening edge of the sample tank. A sample container characterized in that the depth of the sample tank is set, a communication passage that connects the sealed chamber and the outside is formed in the sample tank lid, and a closing member that closes the communication passage is provided. 2. The sample container according to claim 1, wherein surfaces of the sample tank and the lid of the sample tank that define the sealed chamber are subjected to a hydrophilic treatment. 3. The sample container according to claim 1, wherein an elastically deformable pipe member is connected to the communication passage, and the closing member is configured to sandwich the pipe member to close the communication passage. Characteristic sample container.