JPH04155246A - Crystal observation apparatus - Google Patents

Abstract

PURPOSE:To facilitate the maintaining of a constant pressure by a method wherein a liquid reservoir is arranged at a position high with respect of a loading start position of a mounting metal of a high pressure piping for a pressure medium chamber while a close valve at a position of equal level thereto, the close valve is opened when the mounting metal is loaded and closed when the loading ends. CONSTITUTION:A liquid reservoir 18 for overflow is arranged at an upper end of a high pressure piping 17 lifted higher than a loading start position A of a mounting metal 4 as connected to a pressure medium chamber 2 piercing a pressure resistance container 1 and a close valve 19 is arranged at a point of equal level to the position A in the course of the piping 17. The valve 9 is opened, the metal 4 is loaded to a sealing position B from the position A to clamp and a displacement of a pressure medium within the chamber 2 as generated here is stored into the liquid reservoir 8. Thereafter, the valve 9 is closed and after the end of pressurizing operation of a pressurizer 3 and observation of a crystal, the pressurizing operation is released and when the chamber 2 is returned to the normal pressure, the valve 19 is opened. This allows the omission of a tuning operation hard to adjust thereby achieving a maintaining of a constant pressure accurately and easily and also eliminates the mixing of an impure fluid thereby achieving certainty of the observation of the crystal.

Description

Detailed Description of the Invention (Industrial Application Field) The present invention relates to a crystal observation device, and in particular to a high-pressure crystal observation device for observing physical changes in crystals such as crystal shape, growth process, and disappearance process under high-pressure load conditions. Regarding observation equipment.

(Prior Art) It is extremely important to understand the physical changes of crystals, such as their shape, growth process, and extinction process, under pressure when producing or using chemical substances under pressure.

For example, in the pressure crystallization method, which is attracting attention as a separation and purification technology that uses high pressure to precipitate crystals of the target component from a mixture and obtain high-purity products, it is necessary to know in advance the pressure conditions for crystal precipitation and growth. This is an essential requirement.

In order to understand the physical changes in such crystals, crystal observation under pressure is performed.

A typical example of a crystal observation apparatus conventionally used for the above-mentioned crystal observation is shown in FIG. 3, and will be explained below based on this.

As shown in FIG. 3, a conventional crystal observation apparatus includes a pressure-resistant container (1) having optical windows (5) made of a light-transmitting material on both upper and lower opposing sides, and a pressure medium chamber ( 2), and a pressurizing device (3) for increasing the pressure of step 2).When observing crystals, the device is formed of a small container (6) that is transparent and stretchable, and the optical window (5). A sample (object to be observed) is filled in advance in the sample chamber (7).
The pressure medium α9 is transferred to the pressure medium chamber (
2), while the light source (8) illuminates the optical window (
5) Irradiate with light.

In this way, light passes through the optical window (5) and is irradiated onto the sample, and at the same time the sample is pressurized, allowing the crystal shape, growth process, etc. to be observed with the naked eye or with a microscope from outside the optical window (5). It is also possible to observe the disappearance process of crystals by reducing the pressure.

(Problem to be solved by the invention) By the way, the mounting bracket (4) having the sample chamber (7) and the optical window (5) integrally at the tip is attached to the mounting part αO of the pressure container (1).
) from above, the seal part αD provided at the end of the metal fitting (4), that is, the O-ring 0z mounting part, is inserted from the charging start position fal to the seal position (bl) by tightening. Pressure medium chamber (2) which is sealed when
Since the pressure medium α9 inside will naturally be compressed, it will be necessary to extract an amount commensurate with this.

Conventionally, a pressurizing device (3
) was operated to the depressurizing side, but since the mounting bracket (4) is not inserted, it is necessary to operate the depressurizing side.
Various operations must be performed at the same time (and these operations must be synchronized to maintain constant pressure).

If this synchronization is not performed, it is necessary to introduce air, which is a compressible fluid, into the pressure medium chamber (2).

Therefore, there were problems such as the tuning operation was not easy and the observation could not be performed accurately because a compressible fluid such as air was contained.

As a result of repeated studies to solve the above-mentioned problems, the present invention has been completed.The purpose of this invention is to be able to maintain a constant pressure accurately and omit difficult tuning operations. The objective is to achieve reliable crystal observation by easily realizing it and at the same time eliminating the mixture of impure fluids such as air.

(Means for Solving the Problems) In order to achieve the above object, the crystal observation apparatus according to the present invention has the following configuration.

That is, in the crystal observation apparatus according to claim 1, the mounting bracket having an integral optical window made of a light transmitting material at the tip is inserted into the mounting part of the pressure container from above, and is tightened from the charging start position to the sealing position. In a crystal observation apparatus in which a pressure medium chamber connected to a pressurizing device is formed in the pressure vessel by inserting a high pressure pipe into the pressure medium chamber, the high pressure pipe is connected to the pressure medium chamber and is raised higher than the charging start position. Connect the overflow reservoir to its upper end, and hold the valve closed after tightening the mounting bracket to the sole position at a point in the middle of this high-pressure piping that is at the same level as the charging start position. This crystal observation device is characterized by having a closing valve interposed therein.

The crystal observation apparatus according to claim 2 is a container in which the overflow liquid reservoir has a capacity sufficient to store the displacement amount of the pressure medium used for soil removal when the mounting fitting is tightened from the charging start position to the sealing position. The crystal observation apparatus according to claim 1.

(Function) As explained above, the crystal observation apparatus according to the present invention includes a high-pressure pipe connected to a pressure medium chamber, an overflow reservoir connected to the upper end of the pipe, and an intervening device at a predetermined point in the middle of the high-pressure pipe. It has a structure that allows the closure valve to be closed.

Therefore, before inserting the mounting bracket into the mounting portion of the pressure container, perform the following operations. That is, the pressure medium is put into the pressure medium chamber up to the charging start position, the closing valve is left open, and
Keep the pressurizing device stopped and inoperable. As the metal fittings to be removed are inserted and tightened, the pressure medium rises in the high-pressure piping and accumulates in the overflow reservoir.

Then, when the fitting is completely inserted into the sealing position and tightening is completed, the closing valve is closed.

Thus, while the fitting is being inserted, the pressure in the pressure medium chamber is maintained at normal pressure without increasing, and therefore no special operation is required to maintain the pressure. Then, after closing the closing valve, the pressurizing device may be pressurized.

In addition, the illustrated example is an apparatus in which the sample chamber and the pressure medium chamber are each independent, or the crystal observation apparatus according to the present invention is
In addition to this example, it is natural to include an apparatus having a structure in which a sample is injected into a pressure medium chamber and the chamber also serves as a sample chamber.

As described above, according to the present invention, there is no need to perform a depressurizing operation of the pressurizing device when inserting the mounting bracket, and there is no need for any air to be mixed into the pressure medium chamber.

(Example) An example of the present invention is shown in FIG.
A pressure vessel (1) and a pressure medium chamber (2) inside this vessel (1).
), and a pressure adjusting part to adjust the pressure inside the pressure medium chamber (2) during assembly.

Regarding the pressure container (1), (51, +51 is the container fil
There are optical windows made of sapphire installed on both the upper and lower sides of the camera. Both optical windows f5), f5) are hemispherical bodies, and a tapered cylindrical mounting bracket (4
) is integrally fixed to the tip of the tube by gluing or the like.

The mounting bracket (4) has a male thread carved on the outer circumferential surface of the maximum diameter part, and is screwed to a female thread carved in the mounting part αα of the pressure-resistant container (1), so that it can be installed at a predetermined sealing position (B ) is designed to be charged and fixed.

αD is a seal part that grows the O-ring O2, and in the state in the left half of the figure, the O-ring Gz comes into elastic contact with the inner wall of the pressure-resistant container (1), and the inside and outside of the container (1) is connected. It can be sealed off airtight.

It should be noted that the central part of the spherical surface of the hemisphere in the optical window (5) and its vicinity should be flat, since this will allow the sample to be observed more clearly.

(6) A small container (
It is a small container made of Norifun rubber), which is shaped like a plate, and its flange is in close contact with the periphery of the optical window (5) and the tip of the mounting bracket (4) that surrounds the periphery flush with the periphery. The state is firmly held by a small container presser G3 fitted to the tip of the mounting bracket (4).

In this way, an airtight sample chamber (7) is formed at the tip of the upper mounting bracket (4) between the small container (6) and the optical window (5). It is sealed with a small amount of sample for crystal observation.

Next, regarding the pressurizing device (3), a pressure-resistant pipe (9) for connecting the device ft +31 to the pressure medium chamber (2) and a pipe α4 for injecting the pressure medium Q9 are connected. There is. Note that Qe is a pressure gauge.

On the other hand, to explain the pressure regulating part, pressure medium chamber (2)
The high-pressure pipe 07) is connected to the pressure vessel (1) and taken out by liquid-tightly penetrating it, and is raised higher than the charging start position 1t (A) of the mounting bracket (4), and its raised upper end. The overflow reservoir qε connected to the section and the high pressure piping 1
A pressure regulating part is constituted by three members including a closing valve (191) interposed in the middle of 171 at the same level as the charging start position.

The above liquid reservoir q& is located at the charging start position (
Any container is sufficient as long as it has a capacity sufficient to store the amount of pressure medium displaced in the pressure medium chamber (2) tightened from A) to the sealing position (B), and strictly speaking, the liquid reservoir q8 The condition is that the volume in the high-pressure pipe 071 between the pump and the shutoff valve (191) can be stored at a minimum amount equal to the amount subtracted from the displacement amount.

In addition, the closing valve Q91 can be pressurized immediately after the mounting bracket (4) is inserted to the sealing position (B) and completely tightened. The valve is closed throughout the +31 pressurization operation and crystal observation, and after the observation is completed, the pressurization operation is canceled and the valve is opened when the pressure medium chamber (2) is returned to normal pressure.

Note that crystal observation using the apparatus of the example is performed as follows. That is, the installation of the mounting bracket (4) is completed and the closing valve (19
After the valve 1 is closed, the pressure medium 051 is injected into the pressurizing device t (3), and the pressure medium chamber (2) is filled with the pressure medium chamber (2) through the pressure-resistant piping (9) under an initial pressure. Meanwhile, the optical window (5) (lower optical window) is irradiated with light by the light source (8), and observation of the state of the sample in the sample chamber (7) is started. This observation is performed using an optical microscope (not shown) placed above the upper optical window (5).

Next, when the pressure device (3) pressurizes the pressure medium 05 to pressurize the sample, as the pressurization progresses, the small container (6)
gradually shrinks, resulting in changes such as precipitation of crystals from the liquid sample, and it is possible to observe changes in the crystal state.

(Effects of the Invention) The present invention has the above configuration and functions,
When charging the mounting bracket (4), the operation is very simple; just open and close the closing valve α9 and close it at the end of charging. There is no need for any troublesome measures such as not to reduce the pressure.

Furthermore, since the conventional operation that requires skill such as synchronizing two operations can be omitted, the operation is extremely simple and there is no inconvenience such as damage to the O-ring due to erroneous operation.

In addition, in the past, some compressible fluid such as air was used for compensation purposes when synchronization was not performed, and in the present invention, air or the like was not introduced into the pressure medium chamber at all, making it difficult to observe accurately. This has the effect of eliminating problems such as equipment deterioration due to oxidation.

[Brief explanation of the drawing]

FIG. 1 is a partially cutaway side view of one embodiment of the present invention, and FIG.
The figures are partially cutaway side views of a conventional device, in which the right half of both figures shows a state in which charging of the mounting bracket has started, and the left half shows a state in which charging has been completed. (1)-Pressure vessel (2) Pressure medium chamber (3
) - Pressure device (4) Mounting bracket (5) - Optical window GO) Mounting part αD/Seal part
0z O-ring G5 Pressure medium αη
-High pressure piping αg Overflow reservoir 09)
Shutoff valve (A) Charging start position (B)
Seal position patent applicant Kobe Steel Co., Ltd. Representative Patent attorney Akira Kanekagi

Claims (2)

[Claims] (1) Connect to the pressurizing device by inserting the mounting bracket, which has an integral optical window made of a light transmitting material at the tip, into the mounting part of the pressure container from above and tightening it from the charging start position to the sealing position. In the crystal observation apparatus in which a pressure medium chamber is formed in the pressure vessel, a high pressure pipe is connected to the pressure medium chamber and raised higher than the charging start position, and an overflow liquid reservoir is provided at the upper end of the high pressure pipe. At the same time, a closing valve is provided at a point in the middle of the high pressure piping at the same level as the charging start position to maintain the valve closed after the mounting bracket is tightened to the sealing position. crystal observation device. (2) The crystal observation apparatus according to claim 1, wherein the overflow reservoir is a container having a capacity sufficient to store the amount of pressure medium displaced when the mounting fitting is tightened from the charging start position to the sealing position. .