JP2002162342A - Fixed cell for liquids - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a fixed cell for liquids which has highly efficient seal for liquid sample, and can precisely hold fixed space between window plates, and its stability for several matters is good, moreover it is taken environment into consideration. SOLUTION: This invention is related to the fixed cell for liquids which has a pair of window plates 130 and 131 located at both sides of spacer 134 and composed of material penetrating measuring light. Said spacer 134 is not crushed between said window plates 130 and 132, and it has base portion 170 which is hard to hold fixed space, adhesive portion 172 which is installed between said base portion 170 and a pair of window plates and are soft to be crushed to adhere to said window plates 130 and 132. The hardness of said adhesive portion is softer than said base portion.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a liquid fixed cell, and more particularly to an improvement in a spacer between window plates.

[0002]

2. Description of the Related Art Optical means are widely used for quantitative analysis of a predetermined component in a sample. In particular, since the absorbance of a sample is accurately proportional to the concentration of the component in the sample, the quantification by an absorption spectrophotometric method is required. Analysis is widely used. When the absorbance of a liquid sample is measured in this absorptiometry, for example, a liquid fixed cell is used to hold the liquid sample.
The liquid fixed cell containing the liquid sample is arranged at a predetermined position of an optical means such as a Fourier transform infrared spectrophotometer.

For example, in a Fourier transform infrared spectroscopy apparatus 10 as shown in FIG. 1, infrared light 14 from a light source 12 is incident on an interferometer 16, and the interferometer 16 generates an interference light 18. The interference light 18 is applied to the liquid sample 22 in the liquid fixed cell 20, and the transmitted light 24 is detected by the detector 26. The irradiation light data detected by the detector 26 is Fourier-transformed by the Fourier transformer 28 to obtain infrared absorption spectrum data.

In this liquid fixed cell 20, a pair of window plates 30 and 32 are opposed to each other in a portion where light is transmitted in a direction substantially orthogonal to the traveling direction of light so that light can be sufficiently transmitted. Has become. Spacers 3 are provided between the window plates 30 and 32 to secure a space between the window plates 30 and 32.
4 are provided. A hole 36 is provided substantially at the center of the spacer 34, and the space between the window plates 30 and 32 formed by the hole 36 is used as a cell inner chamber 38 to accommodate the liquid sample 22.

[0005]

By the way, it is important that the liquid fixed cell has a high sealing property in order to prevent leakage of the liquid sample. In addition, for example, when performing quantitative analysis using a liquid fixed cell having a fixed cell thickness, if there is an error in the cell thickness of each cell, the measurement conditions cannot be the same. It is also important to ensure the accuracy with this.

For this reason, in the liquid fixed cell, it is desired to ensure a further high sealing property for the liquid sample and a predetermined space between the window plates with high precision. Further, for example, there are various types of liquid samples that can be measured by optical means such as a Fourier transform infrared spectrometer, and the greater the number of types, the higher the possibility of deterioration of members such as spacers. It is desirable to have high stability for many substances.

Furthermore, recently, due to the high interest in the social environment, in addition to the above-mentioned demands on cell performance,
There is also a strong demand for the development of technologies that take environmental considerations into account, such as the natural environment and working environment. The present invention has been made in view of the above-mentioned problems of the related art, and has an object to have a high sealing property with respect to a liquid sample, and to ensure a predetermined space between window plates with high accuracy, and to use various materials. It is an object of the present invention to provide a liquid fixed cell which is excellent in stability and environmentally friendly.

[0008]

In order to achieve the above-mentioned object, a liquid fixed cell according to the present invention is provided so as to face a pair of spacers with a spacer interposed therebetween at a predetermined pressure and made of a material which transmits measurement light. In a liquid fixed cell used for detecting characteristics of a liquid sample inserted between the window plates, the spacer includes a base and a contact portion,
The hardness of the contact portion is softer than that of the base. Here, the spacer does not collapse when sandwiched between the window plates, and has a hardness to secure a predetermined space between the window plates.

The contact portion is provided on a surface of the base portion facing the window plate, and has a softness such that the base portion is crushed so as to be tightly attached to the window plate while being sandwiched between the window plates. In addition,
In the present invention, it is preferable that the spacer is made of a material that is stable with respect to the liquid sample, and the contact portion of the spacer has very low reactivity with various substances, that is, stability. It is particularly preferable that the metal is made of gold which has many advantages that are very excellent in environmental properties, such as excellent in adhesion and excellent in adhesion to the natural environment and not harmful to the working environment.

In the present invention, the thickness of the contact portion of the spacer is 0.1 μm or more and 20 μm or less, preferably 1 μm or more and 15 μm or less, more preferably 3 μm or less.
It is not less than 10 μm. That is, if the thickness of the contact portion of the spacer is less than 0.1 μm, sufficient adhesion to the window plate cannot be obtained, resulting in inferior sealability. If the thickness is more than 20 μm, the contact portion is not sufficiently crushed. This is because it may be difficult to accurately secure the space between the window plates at a desired interval.

For this reason, in the present invention, the thickness of the contact portion of the spacer is 0.1 μm or more in order to achieve both the sealing property of the liquid fixed cell and the securing of a predetermined space between the window plates.
The thickness is set to 0 μm or less. In order to achieve a higher level of both sealing performance and securing a space between window plates, the thickness of the contact portion of the spacer is 1 μm or more and 15 μm or less.
In order to achieve both a very high level of sealing performance and securing a space between window plates, the thickness of the contact portion of the spacer should be 3 μm.
m and 10 μm or less.

[0012]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS A preferred embodiment of the present invention will be described below with reference to the drawings. FIG. 2 is a front view of a schematic configuration of a liquid fixed cell according to an embodiment of the present invention, and FIG.
2A is a sectional view taken along line AA 'of the liquid fixed cell shown in FIG. 2, and FIG. 2B is a view of the same cell taken along line BB' from the side. I have. The portions corresponding to those of the above-described conventional technique are denoted by reference numeral 100, and description thereof is omitted.

The liquid fixed cell 120 shown in FIG. 1 includes a pair of window plates 130 and 132, a spacer 134, and a pair of cell bodies 150 and 152. Here, the window plate 1
30 and 132 are, for example, K transmitting infrared light (measurement light).
It is made of a material such as Br, and is opposed to each other with the spacer 134 interposed therebetween at a predetermined pressure.

The spacer 134 is made of a material that is stable with respect to the liquid sample. A hole 136 is provided in a substantially central portion of the spacer 134, and a space between the window plates 130 and 132 formed by the hole 136 is used as a cell inner chamber 138 to accommodate a liquid sample. The cell body 1
The holes 50 and 152 are provided with circular holes 154 and 156 for passing measurement light such as infrared light, for example, at substantially the center of each of the holes at approximately the same diameter as the hole 136 of the spacer 134.

The cell body 150 has a screw 162
(In FIG. 3B, only one is shown and the others have the same configuration.)
158 (in FIG. 3B, only one hole is shown and the other portions have the same configuration). On the other hand, the cell body 152 is provided with a thread groove 160 (in FIG. 3B, only one is shown and the others have the same configuration) for fitting with the screw 162.

Then, by inserting the screw 162 into the hole 158 of the cell body 150 and screwing the screw thread 164 of the screw 162 into the screw groove 160 of the cell body 152, the window plates 130, 132 hold the spacer 134 between them at a predetermined pressure. A pair of cell bodies 150 and 152 are fixed in a state of being sandwiched, and constitute a liquid fixed cell 120.

In this embodiment, the liquid fixed cell 120 has a filling port 166 and a discharge port 168. The liquid sample is filled into the cell inner chamber 138 through the filling port 166, and the measured liquid sample is discharged to the outside through the discharge port 167. In this embodiment, spacers 168 and 169 are provided between the window plate and the cell body.

By the way, although the spacer 134 between the window plates and the surface of the window plate usually have very slight irregularities, if the spacer 134 between the window plates is made of only a hard material such as lead, the spacer and the window plate may be formed. In some cases, a gap is formed in the gap, making it difficult to obtain a sealing property. In contrast, the spacer 13 between the window plates
If only 4 is made of a soft material, the spacer may be crushed more than a predetermined amount while sandwiched between the window plates, and a space between the window plates may not be secured at a desired interval with high accuracy.

Therefore, in this embodiment, FIGS.
As shown in FIG.
And a contact portion 172. FIG. 4 is an assembly view in which a window plate and a spacer part which are main parts of the liquid fixed cell according to the present embodiment are particularly enlarged, and FIG. 5 is a window plate which is a main part of the liquid fixed cell according to the present embodiment. FIG.

Here, the base 170 is provided with a window plate 130,
132 is not crushed in a state sandwiched by a predetermined pressure,
It is made of a material having hardness to secure a predetermined space between 0 and 132, for example, lead. The contact portion 1
72 is provided on the surface of the base 170 facing the window plates 130 and 132, and is a softness that is crushed so as to be tightly attached to the window plates 130 and 132 while being sandwiched between the window plates 130 and 132 with a predetermined pressure. It is composed of a material having

As described above, in the present embodiment, the spacer 134 between the window plates is provided by providing the soft contact portion 172 on the hard base 170, so that the base of the spacer, the surface of the window plates 130 and 132 can be used. Even if there are slight irregularities, the contact portion 172 fills the gap between the window plates 130 and 132 and the spacer 134 as described above, with the spacer 134 sandwiched between the window plates 130 and 132 at a predetermined pressure. Compared to the spacer 134 made of a hard material, the adhesion is greatly improved, and the liquid leakage is greatly reduced.

Moreover, in the present embodiment, the window plates 130, 1
32, with the spacer 134 sandwiched at a predetermined pressure,
70 maintains the predetermined thickness without being crushed, so that the space between the window plates 130 and 132 can be secured at a desired interval with high accuracy, as compared with the case where the spacer 134 between the window plates is made of one soft material. Can be.

Here, the spacer 1 between the window plates as described above is used.
For 34, attach a lead spacer as a base to mercury,
It is conceivable to use the amalgamated material as the contact portion. Since this amalgamated product is soft, it is easily crushed when sandwiched between window plates at a predetermined pressure, and the adhesion to the window plate can be improved. However, in this case, since mercury is used, sufficient facilities and care are required for disposal of the use environment and unnecessary products.

Therefore, in this embodiment, gold is used instead of mercury at the contact portion of the spacer, and a gold thin film is attached to the base made of lead. As a result, in the present embodiment, by using gold for the contact portion, the gold has a particularly low reactivity to various substances, that is, particularly excellent stability, and further does not pollute the natural environment. It has the advantage of being environmentally friendly, such as not being harmful to the environment.

In this embodiment, the thickness of the contact portion of the spacer is very important in order to ensure the sealing property and the space between the window plates with high accuracy. Therefore, for the purpose of verifying the preferable thickness of the contact portion used for the spacer of the present invention, the thickness of the gold thin film as the contact portion provided on the base made of lead is set as shown in Table 1 below. Instead of this, the sealing performance and the accuracy of securing a predetermined space between the window plates were evaluated.

[0026]Evaluation  ◎… very good ○… good △… normal ×… bad

[Table 1]  Thickness (μm) 0.05 0.1 1 3 5 10 15 20 50  Sealability × △ ○ ◎ ◎ ◎ ◎ ◎ ◎  Space accuracy ◎ ◎ ◎ ◎ ◎ ◎ ○ △ ×

As is clear from the table, when the thickness of the gold thin film is less than 0.1 μm, a space can be secured with a desired interval with high accuracy, but a high sealing property cannot be obtained. On the other hand, if it is thicker than 20 μm, the sealing property is improved, but it is difficult to secure spaces at desired intervals with high accuracy. Therefore, in the present embodiment, the thickness of the contact portion of the spacer is set to 0.1 in order to achieve both the sealing property and the space between the window plates with high accuracy.
It is not less than μm and not more than 20 μm.

As is clear from the table, when the thickness of the gold thin film is 1 μm or more and 15 μm or less, it is necessary to achieve both a higher level of sealing performance and a sufficient space between window plates. When the thickness of the gold thin film is 3 μm or more and 10 μm or less, it is possible to obtain both a very high level of sealing performance and to ensure a space between window plates with high accuracy.

Therefore, in this embodiment, in order to obtain a high sealing property and a space between the window plates with high precision, it is preferable to set the extremely high sealing property and the space between the window plates with a high precision of preferably 1 μm to 15 μm. In order to secure it, it is more preferably 3 μm or more and 10 μm or less. For this reason, in the present embodiment, a spacer is used in which the base is made of lead and the close contact portion is provided with a 5 μm thick gold thin film.

As described above, according to the liquid fixing cell according to the present embodiment, the spacer having the close contact portion made of a thin gold film on the base made of lead is sandwiched at a predetermined pressure between the window plates, so that the sealing performance is improved. And the space between the window boards can be sufficiently obtained. Further, in the present embodiment, as described above, the spacer 134 is deamalgamated and gold is used as the contact portion, so that the effect of the gold is excellent with respect to various substances and hardly deteriorated. As a result, the spacers and the like can be reused (recycled).
In addition, it does not pollute the natural environment of gold, or does not pollute the natural environment because of its very low possibility.
Alternatively, it is possible to provide a cell with very low possibility, and there is no harm to the working environment, so it is environmentally friendly.

In the present embodiment, the window plate 13
By improving the surface accuracy of the crystal 0, 132 by double-side polishing, the adhesion between the window plates 130, 132 and the spacer 134 can be further improved, so that the sealing performance can be further improved. For example, in order to improve the surface accuracy of a crystal substrate (window plate), the level of the Newton ring (NR) is usually 10 or less, and in the present embodiment, the flatness of the entire crystal substrate is reduced to 5 or less Newton rings. Raising.

In this embodiment, the surface of the base made of lead is smoothed by a roller or a press in order to reduce scratches on the surface, and the irregularities of minute parts are further reduced. In the present embodiment, examples of a method of providing gold as the adhesion portion on the base include a method of plating, vapor deposition, and sputtering, and a method of attaching a gold thin film to the base.

In this embodiment, an example using lead as the base has been described. However, the present invention is not limited to this, and any material may be used within the scope of the present invention. be able to. For example, aluminum or the like can be used for the base.

In this embodiment, the thickness of the base can be changed according to a desired cell thickness within the scope of the present invention. When the base is made of, for example, lead, the thickness of the base can be easily changed, that is, the bases having various thicknesses can be easily aligned, so that the cells having various cell thicknesses can be easily aligned.

Further, in the above-described configuration, the liquid fixed cell having a fixed cell thickness has been described as an example. However, any liquid cell in which a spacer is interposed between window plates may be used.
For example, the present invention can be applied to a flow cell and the like.

As described above, according to the liquid fixing cell according to the present invention, the base having the hardness for securing a predetermined space between the window plates without being crushed while being sandwiched between the window plates at a predetermined pressure. Since a spacer including a contact portion having a softness that is squashed so as to be tightly adhered to the window plate while being sandwiched between the window plates at a predetermined pressure is provided, the sealing property and the predetermined space between the window plates are reduced. You can get both. Further, in the present invention, the contact portion of the spacer is made of a material that is stable with respect to the liquid sample, particularly gold that is stable and environmentally friendly with respect to various substances, so that the spacer is significantly deteriorated. And is very environmentally friendly. Further, in the present invention, when the thickness of the contact portion of the spacer is 0.1 μm or more and 20 μm or less, it is possible to reliably obtain both sealing properties and securing a predetermined space between the window plates. Further, in the present invention, when the thickness of the contact portion is 1 μm or more and 15 μm or less, it is possible to obtain both a higher level of sealing performance and a predetermined space between window plates. Further, in the present invention, when the thickness of the contact portion of the spacer is 3 μm or more and 10 μm or less, it is possible to obtain both a sealing property at a very high level and a predetermined space between the window plates.

[Brief description of the drawings]

FIG. 1 is an explanatory diagram of a schematic configuration of a measuring device using a liquid fixed cell.

FIG. 2 is a front view of a schematic configuration of a liquid fixed cell according to an embodiment of the present invention.

3A is a cross-sectional view of a part of the liquid fixed cell shown in FIG. 2 when viewed from the side, and FIG. 3B is a cross-sectional view of a part of the same liquid fixed cell shown in FIG. FIG.

FIG. 4 is an enlarged view of an essential part of the liquid fixed cell according to the embodiment of the present invention.

FIG. 5 is an exploded view of a main part of the liquid fixed cell according to the embodiment of the present invention.

[Explanation of symbols]

 120 Fixed cell for liquid 130, 132 Window plate 136 Spacer 170 Base 172 Adhesive part

Claims (6)

[Claims] 1. A pair of window plates, which are opposed to each other with a spacer interposed therebetween at a predetermined pressure and made of a material that transmits measurement light, and detects characteristics of a liquid sample inserted between the window plates. In the liquid fixed cell used in the above, the spacer is not crushed while being sandwiched between the window plates,
A base having a hardness to secure a predetermined space between the window plates, provided on a surface of the base facing the window plate, so as to be tightly adhered to the window plate while being sandwiched between the window plates. A fixed portion having a softness to be crushed, wherein the hardness of the contact portion is softer than that of the base portion. 2. The liquid fixed cell according to claim 1, wherein the spacer is made of a material stable with respect to the liquid sample. 3. The liquid fixed cell according to claim 2, wherein the contact portion of the spacer is made of gold. 4. The liquid fixed cell according to claim 1, wherein the thickness of the contact portion of the spacer is 0.1 μm or more and 20 μm or more.
m or less. 5. The liquid fixed cell according to claim 4, wherein the thickness of the contact portion of the spacer is 1 μm or more and 15 μm or less. 6. The liquid fixed cell according to claim 5, wherein the thickness of the contact portion of the spacer is 3 μm or more and 10 μm or less.