JPH1123431A - Temperature regulating sample holder - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a temperature regulating sample holder excellent in temperature regulation performance and having a convenient structure. SOLUTION: The temperature regulating sample holder comprises a supporting member on the fixed side provided with a constant temperature water circulation channel, a supporting member 3 fixed movably or removable to the supporting member and provided with a constant temperature water circulation channel, and fixing members 3a, 3b and 2e for pressing both supporting members to support a sample between them. Since the sample is applied tightly to the constant temperature supporting members at least on two sides thereof, temperature difference is reduced between the sample and the supporting members 2, 3 and the sample can be subjected to more accurate temperature control.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for controlling the temperature by refluxing constant temperature water in a sample holder for a square cell, a square or flat solid sample used in a spectrophotometer or other analyzers. The present invention relates to the improvement of the temperature control performance.

[0002]

2. Description of the Related Art Physical and chemical properties of a substance, such as spectral properties, refractive index and other optical properties, dielectric constant, magnetic permeability and other electromagnetic properties, are affected by its temperature.
When measuring the characteristics, it is desirable to perform the measurement while controlling the sample to a predetermined temperature, and the holder for the measurement sample is often provided with a temperature adjusting function.

FIGS. 6 and 7 show a configuration example of a conventional sample holder in which a square cell is temperature-controlled (abbreviated as “temperature control”) by a constant-temperature water reflux method as a representative of a measurement sample.

[0006] In the method shown in FIGS. 6 and 7, a flow path for reflux is formed in one holder block 32, and refluxed water whose temperature has been adjusted from a reflux device outside the apparatus is passed through a constant temperature water tube to move the holder block 32. The temperature of the square cell 31 is adjusted by pressing the square cell 31 against one surface of the holder block 32 whose temperature has been adjusted by the spring 33 attached to the holder block 32.

[0005]

The method shown in FIGS. 6 and 7 is as follows.
In consideration of the convenience of detachment and attachment, the corner cell 31 is only pressed on one side of the temperature-controlled holder block by the spring mechanism 33 attached to the holder, and the other surface of the corner cell 31 Is in contact with the air, so that the square cell 31 is affected by the outside air temperature and has a lower temperature control accuracy than the holder block.

Further, when cells having different thicknesses are used, it is necessary to optimize the pressing force of the spring 33 for each cell, so that it is necessary to prepare a plurality of cells for each cell. In general, a spring formed of a thin plate has a small heat capacity, and one main surface of the cell is in contact with the spring.
The temperature difference between the block and the cell was caused by the influence of the outside air temperature, and the temperature control performance was deteriorated.

SUMMARY OF THE INVENTION It is an object of the present invention to provide a temperature-controllable sample holder having excellent temperature control performance and a simple configuration.

[0008]

In order to achieve the above object, a temperature-controlled sample holder of the present invention comprises a fixed-side support member having a constant-temperature water recirculation flow path and a fixed-side support member having a constant-temperature water recirculation flow path. A supporting member movable or removable with respect to the supporting member on the side, and a fixing member capable of supporting the sample between the two by pressing them.

Thus, regardless of the thickness of the cell, at least two surfaces of the cell are pressed and fixed to the temperature-controlled block with a certain pressing force or more, so that the temperature difference between the cell and the temperature-controlled block is reduced. This allows for more accurate temperature control.

In order to achieve the above object, a temperature-controlled sample holder according to a second aspect of the present invention is the temperature-controlled sample holder according to the first aspect, wherein the pressing force of the pressing means acts in two directions of the sample. .

Thus, three or more surfaces of the sample come into close contact with the constant temperature block, and the temperature control accuracy can be further improved.

[0012]

BEST MODE FOR CARRYING OUT THE INVENTION

(Embodiment 1) The temperature control type sample holder of the present example includes a fixed side temperature control block and a moving side temperature control block, and a flow path for constant temperature fluid recirculation is provided inside both of them.
It is connected to a constant temperature water recirculation device (not shown) outside the device, and is configured so that constant temperature water and the like can be recirculated in both blocks.
The two blocks are connected by a tube.

In the case of the present embodiment, the measurement object is preferably a thin cell. This cell is placed in the space formed by the fixed-side block, the moving-side block is fitted along a guide groove formed on the fixed side, and the cell is pressed rightward in FIG. Then, it is fixed with a fixing screw through a long hole provided on the fixed side. As a result, the cell is shown in FIG.
As shown in (2), at least two major surfaces having a large area are in contact with the temperature-controlled block, and a temperature difference from the block is less likely to occur as compared with the conventional method. Even if the cell thickness changes slightly, only adjusting how far the block on the moving side is pressed, without lowering the temperature control performance to cells of various thicknesses as long as the dimensions of the fixing mechanism with the fixing screw allow, Since it is possible to cope with the problem and the fixing is not performed by pressing the spring as in the related art, the necessity of preparing a plurality of holders according to the thickness of the cell is eliminated.

This embodiment is particularly suitable for a thin cell having a special shape, but can also be used as a temperature control holder for various fixed samples in addition to a normal square cell.

Hereinafter, a more specific description will be given with reference to the drawings.

FIG. 1 is a plan view showing a schematic configuration of a temperature-controlled sample holder according to an embodiment of the present invention. S is a sample, which may be a solid sample itself to be measured, but is usually a sample cell containing a sample. Reference numeral 1 denotes a temperature-controlled sample holder for holding the sample S at a predetermined temperature. 2
Is a constant temperature block main body (fixed side) constituting the main body of the sample holder 1 and has a U-shaped cross section, for example, to form a sample accommodating space. 3 presses the sample S from behind to the thermostatic block main body (fixed side) 2 side, and the sample holder 2
A fixing back plate (moving side) for fixing and holding the sample S between the constant temperature block bodies 3 with a sufficient pressing force, and causing at least two-sided contact between the constant temperature sample holder 1 and the sample S.
(A constant temperature block back plate), and is configured to be movable or detachable with respect to the constant temperature block main body (fixed side) 2.

The thermostatic block main body 2 and the fixing back plate 3 are formed with flow paths (not shown) for circulating a thermostatic fluid inside the respective blocks. For example, a constant temperature water tube 4 for circulating constant temperature water is connected. (Therefore, the constant temperature block main body 2 and the fixing back plate 3 are made of a material having good heat conductivity and being chemically stable to a constant temperature fluid, for example, a metal such as stainless steel, aluminum, or brass.) In the figure, is composed of a constant temperature water supply pipe 4a and a discharge pipe 4b to the constant temperature block main body 2, and a connecting pipe 4c between the constant temperature block main body 2 and the fixing back plate 3. Supply pipe 4a
One or both of the discharge pipes 4b may be provided on the side of the fixing back plate 3, but in this case, it is often necessary to attach and detach many pipes each time the fixing back plate 3 is attached and detached. It is preferable to install them on the constant temperature block 2 side as shown in FIG. The connecting pipe 4c is connected to the constant temperature block main body 2.
And the supply pipe 4a is connected to one of the fixing back plate 3 and
When the discharge pipe 4b is connected to the other end, the connecting pipe 4c
If only 4a and 4b are combined into one of the constant temperature block main body 2 and the fixing back plate 3, the connecting pipe 4c may be used.
Requires two round trips.

FIG. 2 is a perspective view of a more specific embodiment of the temperature-controlled sample holder, in which main elements are shown separated from each other, and the same symbols and numerals as in FIG. 1 represent the same elements. They have basically the same configuration. In FIG. 2, a constant temperature block main body (fixing side) 2 having a U-shaped cross section is fixed on a base 10 fixed to, for example, a fixing portion of a spectrophotometer by a fixing screw 10b. The thermostatic block main body 2 has a sample accommodating space 2b formed in a U-shape or the like. For example, the sample 1 is inserted in the direction of the arrow in FIG. 2 and can be accommodated in a predetermined state. . The fixing back plate (moving side) 3 is provided with a pair of screw holes 3a in the lateral width direction at the same height position on the left and right, while the constant temperature block body (fixing side) 2 has a pair of screw holes 3a. At a height position corresponding to the hole 3a, a pair of through holes 2e having an elongated width in the depth direction of the space 2b and extending in the width direction of the space 2b are provided. Thereby, when the sample cell S is inserted into the space 2b, the fixing back plate (moving side) 3 is moved in the direction of the arrow along a guide groove or the like provided in the constant temperature block main body 2 so that the sample cell S The sample cell S can be fixed at a predetermined position in the space 2b by the back plate fixing screw 3b in a state where both surfaces are sufficiently pressed by the constant temperature block 2 and the fixing back plate 3.

Reference numerals 4a and 4b denote thermostatic water tubes (supply pipes and discharge pipes) for circulating thermostatic water through the thermoregulated sample holder 1, one of which is connected to a recirculating flow path in the thermostatic block 2 and the other is connected to a recirculating flow path. Piping connection part 5 provided on front panel 11
a, 5b, and can be connected to a separately provided supply source of constant temperature water at a predetermined temperature and circulated.

With the above configuration, regardless of the thickness of the cell, at least two surfaces of the cell are pressed and fixed to the temperature-controlled thermostatic block by a pressing force of a certain level or more.
The temperature difference between the cell and the temperature-controlled block is reduced, and more accurate temperature control becomes possible. In the case of a sample holder for measuring optical characteristics such as a spectrophotometer, the following configuration is further provided.

The U-shaped constant temperature block main body 2 further has a shallow plate-like groove 2c on the side opposite to the space 2b, and the groove 2c is covered with a cover 2d. The cover 2d has a window 2a on the central axis through which the measurement light beam passes. Reference numeral 7 denotes a diaphragm plate for measuring light beam, which is provided with a light beam diaphragm 7a for limiting the amount of light passing through the measuring light beam. It is configured to be. Reference numeral 8 denotes an aperture plate for a reference light beam, which is provided with an aperture 8a for light amount balance and a screw 8b
Is fixed on the base 10.

(Embodiment 2) FIGS. 3 and 4 are plan views of a main part of a second embodiment of the present invention, and a base 10 similar to that of the first embodiment of FIGS. In the case where a constant-temperature water recirculation mechanism is provided and optical characteristics are measured by a spectrophotometer or the like, a light beam stop plate 7 and a light amount balance plate for a reference light beam are also provided.

In FIG. 3, reference numeral 12 denotes a constant temperature block main body (fixed side), which is formed in a quadrangular cylindrical shape, has a sufficient wall thickness, and is fixed on a base (FIG. 2). 13 is a constant temperature block back plate (moving side) (back plate block) formed in a rectangular parallelepiped shape and housed in the constant temperature block main body (fixed side).
The constant temperature block body 12 and the constant temperature block back plate 13
A constant temperature block assembly for supporting the sample S is constituted by the above. The constant temperature block main body 12 and the constant temperature block back plate 13 are each provided with a constant temperature water circulation channel, are detachably connected to a constant temperature water tube (not shown), and are connected to each other by a connection pipe (not shown). . The sample S includes one wall portion 12 a of the thermostatic block main body 12 and the thermostatic block back plate 1.
3 between. The thermostatic blocks 12 and 13 are made of the above-mentioned metal having good heat conductivity. Since the sample S and the constant temperature block back plate (moving side) 13 cannot be moved in and out laterally, the height of the sample S and the constant temperature block back plate 13 (moving side) is adjusted so that the sample S and the constant temperature block back plate 13 (moving side) can be easily moved in and out. It is preferable that the height is slightly higher (longer) than the height of the main body 12.

Reference numeral 9 denotes a pressing screw for pressing and fixing the constant temperature block back plate (moving side) 13 and the sample S to one wall 12a of the constant temperature block main body 12 on the side of the sample S. A portion 9a is provided. The pressing screw 9 is connected to the other wall 12 b of the thermostatic block main body 12 on the side opposite to the sample.
And is screwed on its central axis A. In this configuration, if the pressing screw 9 is adjusted,
The inner surface of the wall portion 12a and the constant temperature block back plate 13 can be fixedly supported by being brought into close contact with a sufficient pressure, respectively. A spring is provided at the tip of the pressing screw 9, one end is fixed to the tip of the screw 9, and the other end is brought into contact with the constant temperature block back plate 13,
It may be configured such that the pressing force of the pressing screw 9 elastically acts on the back plate 13.

According to the embodiment shown in FIG. 3, the structure is simple, the sample S and the constant temperature block back plate 13 (moving side) can be easily taken in and out, and the adjustment of the pressure on both sides of the sample S is very easy. In addition, it can sufficiently cope with a thin sample to a thick sample depending on the length of the screw 9. Further, since the back plate block 13 exists in the constant temperature block main body 12, the temperature control accuracy is higher than in the case of temperature control using only constant temperature water.

FIG. 4 is a modification of FIG. 3, and the basic configuration is exactly the same as that of FIG. 3, but the pressing force on the sample S and the constant temperature block back plate 13 (moving side) is changed to the constant temperature block main body 1.
3 is that the load is applied not in parallel to the central axis A but in an oblique direction (in the example shown in FIG. 4, in the downward right direction).
Is different from the embodiment.

As a mechanism for the pressing in the oblique direction,
In FIG. 4, the pressing screw 9 is disposed obliquely downward and to the right at a position shifted slightly above the axis A. However, the pressing screw 9 is provided in the same state as in FIG. 13, the left side may be formed as a sloping surface to the right as shown by a broken line B in FIG. In this case, if the pressing screw 9 is made longer, it can be adapted to a wider range from a thin sample to a thicker sample than the case where the pressing screw 9 is obliquely arranged. In some cases, the left slope of the constant temperature block back plate 13 (moving side) 13 may be used in combination with the arrangement of the pressing screw 9 obliquely downward to the right. With these configurations, in the case of FIG. 4, not only the left and right surfaces a and b of the sample S, but also
The constant temperature blocks 12, 1 are also used for the surface c perpendicular to the surface b.
In the state pressed from 3, it can be fixedly supported.

According to the embodiment shown in FIG. 4, the structure is simple, the sample S and the back plate block (moving side) 13 can be easily taken in and out, and the adjustment of the pressure on both sides of the sample S is very easy. Further, the sample S is placed in the thermostatic blocks 12 and 1.
3 can be brought into close contact with three surfaces, and the temperature control accuracy can be further improved as compared with FIG. 4 is also suitable for a relatively thick sample.

(Embodiment 3) FIG. 5 is a plan view of a main part of a third embodiment of the present invention, and shows a base 10, a constant temperature water circulating mechanism, and a light beam stop similar to those of the first embodiment. Although a plate 7 and a light amount balance plate for a reference light beam are also provided, their description is omitted because they are duplicated. FIG. 5 shows a configuration in which two (22, 23) constant temperature blocks having an L-shaped cross section are provided, for example, 22 is configured as a fixed side, 23 is configured as a movable side, and a sample S is arranged between them.
When the moving side 23 is moved and pressed in the upper right corner direction of the fixed side 22, the four side surfaces of the sample S are pressed against the corresponding inner side surfaces of the constant temperature block, and are brought into close contact with each other and fixedly supported. This pressing means can be formed by using two screw pressing mechanisms as shown in FIG. 3, but can also be simply constructed by using, for example, screw pressing tweezers or rubber rings. The configuration of FIG. 5 is also suitable for a sample having a certain thickness.

[0030]

As described above, according to the present invention, regardless of the thickness of the sample (sample cell), at least two surfaces thereof are pressed and fixed to the temperature-controlled block by a certain or more pressing force, As a result, the temperature difference between the sample (sample cell) and the temperature-controlled block is reduced, and more accurate temperature control of the sample becomes possible.

[Brief description of the drawings]

FIG. 1 is a plan view showing a configuration of a temperature-controlled sample holder according to an embodiment of the present invention.

FIG. 2 is a perspective view of a specific configuration of a temperature-controlled sample holder according to one embodiment of the present invention, showing a state where main elements are separated.

FIG. 3 is a plan view showing a configuration of a temperature-controlled sample holder according to a second embodiment of the present invention.

FIG. 4 is a plan view showing a configuration of a temperature-controlled sample holder according to a modification of the second embodiment of the present invention.

FIG. 5 is a plan view showing a configuration of a temperature-controlled sample holder according to a third embodiment of the present invention.

FIG. 6 is a perspective view showing a configuration example of a conventional temperature-controlled sample holder.

FIG. 7 is a plan view of the configuration of FIG. 6;

[Explanation of symbols]

 A: Central axis L: Measurement light beam R: Reference light beam S: Sample (sample cell) 1: Temperature-controlled sample holder 2: Constant temperature block (fixed side) 3: Fixed back plate (moving side) 3a: pressing fixing screw 4 (4a, 4b, 4c, 4d): constant temperature water tube 5 (5a, 5b): piping connection part 7: diaphragm plate for measuring beam 8: diaphragm plate for reference beam 9 ... Pressing screw 10 Base 11 Front panel 12 Constant temperature block main body 13 Constant temperature block back plate 22 Constant temperature block (fixed side) 23 Constant temperature block (moving side) 31 Square cell 32 ... constant temperature block 33 ... spring

Claims (2)

[Claims] 1. A fixed-side support member having a constant-temperature water recirculation flow path, a support member having a constant-temperature water recirculation flow path and movable or detachable with respect to the fixed-side support member, and both are pressed and fixed. A temperature-controllable sample holder, comprising a fixing member capable of supporting the sample between the two. 2. The temperature-controlled sample holder according to claim 1, wherein the pressing force of the pressing means acts on two surfaces of the sample.