JP3088843B2 - High pressure substance observation device - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for observing a substance under a high pressure, and more particularly to a change in the state of a substance under a pressure load, and in particular, the physics of a crystal such as a crystal shape, a growth process and an annihilation process under a high pressure. The present invention relates to a high-pressure substance observation apparatus for observing a dynamic change.

[0002]

BACKGROUND OF THE INVENTION It is important to know the change in the state of a substance under a pressure load when producing or using the substance under pressure. In particular, it is important to understand the physical changes of the crystal such as the shape, growth process, and disappearance process of the crystal under the pressure load condition.
It is extremely important when producing or using chemicals under pressure.

[0003] For example, in a pressure crystallization method, which is attracting attention as a technique for separating and purifying a target component from a mixture, it is an essential requirement to grasp the physical change of the crystal as described above. The pressure crystallization method is a separation and purification technology that uses high pressure to separate out the target component crystals from a liquid or slurry-like mixture and separate them from other components to obtain high-purity products. Because there is. That is, it is necessary that the pressure for depositing and growing a crystal and the pressure condition for forming a good crystal be known in advance.

[0004] In order to grasp the physical change of the crystal under such a pressure load state, the crystal is observed under pressure.
An apparatus used for observing a change in the state of a substance under high pressure, such as crystal observation, is a high-pressure substance observation apparatus. FIG. 3 shows a typical example of a conventional high-pressure substance observation apparatus, which will be described below.

As shown in FIG. 3, a conventional high-pressure substance observation apparatus includes a pressure vessel 3 having optical windows 1 and 2 made of a light transmitting body on both upper and lower sides facing each other, and increasing the pressure in the pressure vessel 3. Pressure means 4 and a flange (i.e., peripheral edge of the small container) of the small container 10 having optical transparency and flexibility in the pressure-resistant container 3 and a peripheral edge of the end face of the optical window 1 and a small container holder. The sample S is formed by sandwiching the
Has a sealed sample chamber 9.

Here, the flange portion of the small container 10 is sandwiched by contacting the flange portion with the peripheral edge of the end surface of the optical window 1, screwing the small container holding member 11 to the screw portion of the mounting bracket 12, and rotating. This is done by tightening. As a result, the flange portion and the peripheral edge portion of the optical window 1 are in close contact with each other, and a liquid-tight sample chamber 9 is formed. Since the small container 10 requires flexibility, a container made of a soft synthetic resin such as a polyethylene resin is generally used.

According to the above high pressure substance observation apparatus, high pressure substance observation can be performed as follows. First, a sample S (object to be observed) is sealed and filled in the sample chamber 9 in advance, and then the pressure medium 15 is injected into the pressure-resistant container 3. While applying pressure, the light source 8 irradiates the optical window 2 with light. In this case, since the small container 10 forming the sample chamber 9 has flexibility, the pressure in the sample chamber 9 becomes equal to the pressure of the pressure medium 15, so that the sample S in the sample chamber 9 is moved to the predetermined pressure. The sample S can be depressurized to a predetermined pressure when the pressure is reduced to a predetermined pressure. On the other hand, the irradiated light passes through the optical window 2, passes through the light-transmitting small container 10, and irradiates the sample S. Therefore, the sample S is observed with the naked eye or a microscope from outside the optical window 1. obtain. Therefore, it is possible to observe the sample S in a state of being pressurized to a predetermined pressure, and observe the shape of the precipitated crystal, the crystal growth process when the pressure is increased, the crystal disappearing process when the pressure is reduced, the melting pressure, and the like. I can do it.

[0008]

However, in the conventional high-pressure substance observation apparatus, the flange of the small container 10 is brought into contact with the peripheral edge of the end face of the optical window 1 and the peripheral portion and the small container holder 11 are held together. Since the sample chamber 9 is formed by sandwiching the sample chamber 9, the liquid tightness (sealing property) of the sample chamber 9 depends on the surface roughness of the peripheral portion and the flange portion of the small container 10, and the sample chamber 9 is sealed by surface contact. Therefore, the pressure medium 15 in the pressure vessel 3 leaks into the sample chamber 9 and, conversely, the sample S from the sample chamber 9 into the pressure medium 15 in the pressure vessel 3 at the time of pressure reduction.
There is a problem that the leakage is likely to occur. In particular, when observing a substance under high pressure at a high temperature, the small container 10 is dented, which makes it more likely that the pressure medium 15 leaks into the sample chamber 9.

In addition, when the flange portion of the small container 10 is clamped, there is a drawback that a twisting force is applied to the flange portion due to the rotational tightening of the small container presser 11. This torsional force may cause problems such as deterioration of the sealing property of the sample chamber 9, difficulty in observing the sample S due to deformation of the sample chamber 9, and further, destruction of the sample chamber 9.

If the leakage occurs as described above, it is necessary to replenish the sample every time the substance is observed under high pressure, so that the handling is troublesome and extra time is required for switching. Furthermore, the sample to be observed under high pressure is naturally a new substance in many cases, and in that case, it is difficult to make a large amount of the sample. Therefore, it is a very serious problem that the leakage occurs as described above and the sample is wasted as a result. Note that when the sample S leaks into the pressure medium, the properties of the sample S may be unknown, and in an extreme case, there may be a problem that the pressure vessel 3 is corroded.

The present invention has been made in view of such circumstances, and has as its object to solve the above-mentioned problems, without impairing the advantages of the conventional high-pressure substance observation apparatus. As compared with the conventional apparatus, the sample chamber has excellent liquid tightness (sealability), and as a result, leakage between the pressure medium in the pressure-resistant container and the sample in the sample chamber can be prevented. It is an object of the present invention to provide a high-pressure substance observing apparatus in which a torsional force is hardly applied to the flange portion when clamping is performed, and as a result, occurrence of inconvenience due to torsion can be prevented.

[0012]

In order to achieve the above object, a high-pressure substance observation apparatus according to the present invention has the following configuration. That is, the high-pressure substance observation device according to claim 1 includes a pressure-resistant container having an optical window formed of a light transmitting body on a side surface, pressure increasing means for increasing the pressure in the pressure-resistant container, and light inside the pressure-resistant container. Observation of a substance under high pressure having a sample chamber which is formed by sandwiching a flange portion of a transparent and flexible small container between an end surface peripheral portion of the optical window and a small container holding member and in which a sample is sealed. An apparatus, wherein an O-ring is disposed between a peripheral edge portion of the optical window and a flange portion of the small container, and a patch plate is disposed between the flange portion and a holding member. It is a high-pressure substance observation device.

The high pressure substance observing apparatus according to the second aspect is the high pressure substance observing apparatus according to the first aspect, wherein an annular spacer for adjusting a contraction amount of the O-ring is arranged in the pressure container.

[0014]

As described above, the high-pressure substance observation apparatus according to the present invention comprises: a pressure-resistant container having an optical window made of a light-transmitting body on a side surface; a pressure-intensifying means for increasing the pressure in the pressure-resistant container; It has a sample chamber formed by sandwiching a flange portion of a light-transmitting and flexible small container in the container between the peripheral edge portion of the optical window and the small-vessel holding member and in which the sample is sealed. A substance observation apparatus under high pressure, wherein an O-ring is arranged between a peripheral edge portion of the optical window and a flange portion of the small container, and an abutment plate is arranged between the flange portion and a holding member. I have.

Therefore, the space between the peripheral edge of the optical window and the flange of the small container is sealed by the O-ring, and the O-ring is sealed by line contact.
It is clear that the sealing property is extremely improved, and therefore, the liquid tightness (sealing property) of the sample chamber is remarkably superior to that of the conventional device which is easily affected by the surface roughness of the sealing portion and is sealed by surface contact. As a result, leakage between the pressure medium in the pressure-resistant container and the sample in the sample chamber can be prevented.

Further, since the contact plate is arranged between the flange portion of the small container and the holding member, when the flange portion of the small container is pinched by the rotational tightening of the small container holding member, the torsion is caused by the contact plate. As a result, it becomes difficult to apply a twisting force to the flange portion, so that the flange portion is not twisted and can be uniformly tightened. As a result, inconvenience caused by the twisting can be prevented.

Therefore, the apparatus for observing a substance under high pressure according to the present invention does not impair the advantages of the conventional apparatus for observing a substance under high pressure, and the liquid tightness (sealing property) of the sample chamber is higher than that of the conventional apparatus. ), So that leakage between the pressure medium in the pressure vessel and the sample in the sample chamber can be prevented, and
When the flange portion of the small container is pinched, it is difficult for the torsion force to be applied to the flange portion, and as a result, inconvenience due to the torsion can be prevented.

It is preferable that an annular spacer for adjusting the amount of shrinkage of the O-ring is arranged in the pressure-resistant container. That is, when the flange of the small container is pinched by rotating and tightening the small container holder, excessive deformation of the O-ring can be avoided, and as a result, the O-ring is less likely to be damaged or deteriorated, and its life is extended. This is because, at the same time, excellent sealing properties can always be ensured.

In the apparatus for observing a substance under high pressure according to the present invention, the materials of the backing plate and the annular spacer are not particularly limited, as long as they have necessary heat resistance, chemical resistance and strength. . For example, metal, plastic, and the like can be used. Also, the number of O-rings and annular spacers is not particularly limited. On the other hand, as long as the small container has a light transmitting property and a flexibility, the material is not particularly limited, but the light transmitting property, the flexibility, the heat resistance, and the resistance It is desirable to use one having excellent chemical properties and the like.

[0020]

【Example】

(Embodiment 1) FIG. 1 is a sectional side view of a main part of a high-pressure substance observation apparatus according to Embodiment 1 of the present invention. This device basically has an optical window 1 made of a light transmitting body on opposing upper and lower sides.
2, a pressure-intensifying means for increasing the pressure in the pressure-resistant vessel 3 (similar to the pressure-intensifying means 4 shown in FIG. 3 and not shown), and A sample chamber formed by sandwiching a flange portion of a light-transmitting and flexible small container 28 between an end surface peripheral portion of the optical window 1 and the small container holding member 11 and sealing a sample S therein. 9. The high pressure substance observing apparatus having an O.D. 9 between the peripheral edge of the optical window 1 and the flange of the small container 28.
A ring 26 is provided, and a backing plate 27 is provided between the flange portion and the holding tool 11.

Here, the optical windows 1 and 2 are made of sapphire and are supported by an optical window support 29, which is screwed to the pressure-resistant container 3. Each optical window has a cylindrical shape, but the lower corner of the optical window 1 is tapered.
That is, the peripheral edge of the end surface of the optical window 1 in contact with the O-ring 26 is formed in a tapered shape over the entire circumference. The central portion of the optical window and its vicinity were formed flat. This is to enable the sample S to be more clearly observed.

The small container 28 is entirely made of a resin having light transmitting and flexibility. The sample chamber 9 is formed as follows. That is, the sample S is placed in the small container 28 and
The sample S is sealed by rotating the small container holder 11 through the contact plate 27 and tightening the flange after contacting the flange portion 28 with the peripheral edge (tapered portion) of the optical window 1 via the O-ring 26. A sample chamber 9 is formed. At this time, the annular spacer 7 for adjusting the contraction amount of the O-ring 26 is
Placed on the small container holder 11 in the
26 to prevent excessive deformation.

Using the above substance observation apparatus under high pressure, the sample S
Was sealed in a sample chamber 9, and crystal observation such as crystal precipitation and shape change under high pressure was performed as follows. That is, after sealing the sample S in the sample chamber 9, the pressure medium 15 is injected into the pressure-resistant container 3 and filled. Next, while the pressure medium 15 is pressurized by the pressure increasing means (similar to the pressure increasing means 4 in FIG. 3), the light source 8 irradiates the optical window 2 with light, and the sample S
Was observed from outside the optical window 1 with an optical microscope (not shown).

As a result, as the pressure increases, the small container
28 gradually shrinks, the state of crystal precipitation from the sample S can be clearly observed, and the melting state of the crystal accompanying the subsequent pressure reduction can also be clearly observed, and the pressure medium 15 leaks into the sample chamber 9. Thus, a series of crystal observations from the precipitation and growth of the crystal to the disappearance thereof could be performed without any intrusion or leakage of the sample S into the pressure medium 15. Further, the same crystal observation was repeated, but no leakage occurred between the pressure medium 15 and the sample S. When the precipitation pressure and the melting pressure of the crystals were measured, the measured values were the same as those measured by the conventional method without any inconvenience.

Further, when the flange portion of the small container 28 is clamped by the rotational tightening of the holding member 11 for forming the sample chamber 9 and sealing the sample S, the flange portion is not twisted at all and is uniformly tightened. And O-ring
26 could be tightened without excessive deformation.

(Embodiment 2) FIG. 2 is a sectional side view of a main part of a high-pressure substance observation apparatus according to Embodiment 2 of the present invention. In this device, the optical window 1 has a cylindrical shape and does not have a tapered lower corner, but has an O.D.
The ring 26 contacts and the small container 28 is in the form of a sheet. The sample (small container 28), the O-ring 26 and the optical window 1 form the sample chamber 9. Teflon and other light-transmitting and flexible resins were used for the sheet. Further, the annular spacer 7 is disposed inside the O-ring 26. Except for this point, it has a structure similar to that of the first embodiment. The arrangement of the annular spacer 7 also has the effect of reducing the substantial internal volume (space) of the sample chamber 9 and limiting the required amount of the sample S.

Using the above substance observation apparatus under high pressure, the same crystal observation was performed by the same method as in Example 1. As a result, as in the case of the first embodiment, the pressure medium 15
No crystal leakage occurred, and a series of crystal observations could be performed repeatedly. Further, at the time of clamping the flange portion of the small container 28, no inconvenience such as twisting of the flange portion occurred.

[0028]

The present invention has the above-described structure and functions. An O-ring is provided between the peripheral edge of the optical window and the flange of the small container. Since the backing plate is provided between the holder and the holder, the sample chamber formed by the optical window, the O-ring, and the small container has extremely excellent liquid tightness (sealability). When clamping the flange portion of the small container by tightening, twisting of the flange portion is extremely unlikely to occur. Therefore, the high-pressure substance observation apparatus according to the present invention has excellent liquid tightness (sealing property) of the sample chamber as compared with the conventional apparatus without impairing the advantages of the conventional high-pressure substance observation apparatus. It is possible to prevent leakage between the pressure medium in the pressure vessel and the sample in the sample chamber, and it is difficult for the torsion force to be applied to the flange portion when the flange portion of the small container is pinched. This has an effect that generation can be prevented.

[Brief description of the drawings]

FIG. 1 is a side sectional view showing a main part of a high-pressure substance observation apparatus according to a first embodiment.

FIG. 2 is a side sectional view showing a main part of a high-pressure substance observation apparatus according to a second embodiment.

FIG. 3 is a side sectional view showing an outline of a typical example of a conventional substance observation apparatus under high pressure.

[Explanation of symbols]

1—optical window, 2—optical window, 3—pressure vessel, 4—pressure booster, 5—temperature sensor, 6—pipe, 7—annular spacer,
8--light source, 9--sample chamber, 10--small container, 11--small container holder, 12--mounting bracket, 13--seal member, 14--side wall of pressure-resistant container, 15--pressure medium , 16-through hole, 17-piston, 18-piston large thread, 19-pressure gauge, 20-piston drive, 21-feed screw, 22-worm reducer, 23--Rotating means, 24--Packing, 25--Female thread of lead screw, 26--O
Ring, 27--backing plate, 28--small container, 29--optical window cradle, S
--sample.

──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-4-104998 (JP, A) JP-A-3-69583 (JP, A) JP-A-5-32499 (JP, A) JP-A-61- 140841 (JP, A) JP-A-63-9841 (JP, A) (58) Fields investigated (Int. Cl. ⁷ , DB name) G01N 21/00-21/61 C30B 1/00-35/00 JICST File (JOIS)

Claims (2)

(57) [Claims] 1. A pressure-resistant container having an optical window made of a light-transmitting body on a side surface, pressure-increasing means for increasing the pressure in the pressure-resistant container, and a light-transmitting and flexible small-sized container in the pressure-resistant container. A high-pressure substance observation device having a sample chamber in which a sample is sealed while being formed by sandwiching a flange portion of a container between an end surface peripheral portion of the optical window and a small container presser, wherein the optical window has An apparatus for observing a substance under high pressure, wherein an O-ring is provided between a peripheral portion of an end face and a flange portion of the small container, and a backing plate is provided between the flange portion and a holding member. 2. The high-pressure substance observation device according to claim 1, wherein an annular spacer for adjusting a contraction amount of the O-ring is disposed in the pressure-resistant container.