JPH06186223A - Decantation device and thermal decomposition-infrared spectral analysis method for sample - Google Patents

Abstract

PURPOSE:To control the inclination operation of a container with the same amount of precision as manual operation by providing a retention arm and a rotary handle at the center of two large and small discs which are in contact with each other on the circumferential surface. CONSTITUTION:It is desirable that the ratio of diameter of a large disc E to that of a small disc F with extremely different radii of curvature should be 10:1-100:1. The discs E and F are in contact at the side surfaces with each other. Then, when a handle G at the center of the disc F is rotated to rotate the disc F, the disc E with a large diameter than that of the disc F gradually and smoothly rotates. The slow rotary motion is transferred to a container retention tool C which retains a container B being provided at the tip of a retention arm J by the retention arm J. Therefore, the rotation of the handle G causes the container B to be inclined slowly and smoothly and hence a supernatant liquid to flow out quietly and to be separated from a precipitate. Namely, arbitrary rotary control of the handle G enables the container B to be inclined at arbitrary speed and angle and hence achieving the same amount of decantation of a sample as that by manual operation.

Description

Detailed Description of the Invention

[0001]

[Industrial applications]

(First Invention) The first invention of the present invention relates to a decantation device for a sample used in a separation operation of a precipitate and a supernatant in a chemical analysis or a chemical synthesis. (Second invention) The second invention of the present invention relates to a thermal decomposition-infrared spectroscopic analysis method, and more specifically to improvement of a method for aggregating and collecting thermal decomposition products.

[0002]

[Prior art]

(First invention) At the time of chemical analysis or chemical synthesis, an operation of separating the precipitate from the supernatant without using a separating member such as filter paper may be performed. Conventionally, in such a case, hold a container such as a beaker in your hand, and gently tilt the container gently so as not to give vibration gently by hand.
An operation called so-called decantation is performed in which the precipitate and the supernatant are separated so that the supernatant and the precipitate are not mixed again. Until now, no decantation device or machine that can mechanically perform this tilting operation has been manufactured and sold, and the decantation device is exclusively operated by hand as described above. However, this manual operation has a problem that skill is required because interruption of the tilting operation and vibration must be minimized and difficulty in controlling the tilting speed and the tilting angle. Further, since it is necessary to perform the operation while gazing, the operator's face and the container are easily approached, and when handling harmful chemicals, there is a risk of inhaling the vapor. Further, there is also a problem that it is not efficient because only one person can process it manually.

(Second invention) Conventionally, the thermal decomposition-infrared spectroscopic analysis method is a method in which a polymer or the like is thermally decomposed and the decomposition product is analyzed by infrared spectroscopic method. The operation is carried out in a test tube. There is no lid on the test tube used for thermal decomposition, and the vapor generated by thermal decomposition is condensed on the tube wall, but in this case, the tube wall is not particularly cooled except by natural air cooling. . However, the above-mentioned conventional method has the following drawbacks. (1) In the conventional pyrolysis-infrared spectroscopy, the tube wall is
Since it is not cooled except for natural air cooling, it is extremely difficult to condense and collect trace substances that easily volatilize, and it is difficult to analyze these substances. Further, since the test tube for thermal decomposition used in the conventional method does not have a lid, it is more difficult to analyze a trace substance that easily volatilizes. (2) In conventional thermal decomposition-infrared spectroscopy, glass instruments such as test tubes are used as thermal decomposition vessels. For example, a low boiling point organic solvent is dripped into this and forcedly cooled. However, there is a problem that the glass is easily broken and only natural air cooling can be performed.

[0004]

[Problems to be Solved by the Invention]

(First Invention) Therefore, an object of the present invention is to solve these problems of the prior art, and to perform decantation of a sample capable of precisely controlling the tilting operation of a container as well as the conventional manual operation. A device is provided. (Second invention) Therefore, an object of the present invention is to solve the above-mentioned problems in the thermal decomposition process of a sample of the conventional method, and to provide a thermal decomposition-infrared spectroscopic analysis method with higher sensitivity than before. is there.

[0005]

[Means for Solving the Problems]

(First Invention) The object of the present invention is achieved by the following invention. That is, according to the present invention, two large and small discs and / or fan-shaped discs having circles with markedly different curvatures are in contact with each other on their circumferential surfaces, and a handle for rotating a small disc at the center of a small disc. Alternatively, a decantation of a sample, which has a motor and has a holding arm fixed to a rotation support portion provided at the center of a large board, and a container holder is installed at a tip of the holding arm. It is a device.

(Second Invention) The above object is achieved by the present invention described below. That is, according to the present invention, a sample is placed in a pyrolysis container with a lid and heated, and the pyrolysis vapor is cooled and collected using a cooling device or a coolant to form an aggregate, and then the condensate is subjected to infrared spectroscopy. It is a thermal decomposition-infrared spectroscopic analysis method characterized by being analyzed by an analyzer.

[0007]

[Action]

(First Invention) As a result of intensive studies to solve the above-mentioned problems of the prior art, the present inventor uses two elastic discs and / or fan-shaped discs of large and small rubbers having remarkably different curvatures. According to the present invention, it was found that a simple device capable of controlling the tilting speed and the angle of the container in the same manner as the manual operation can be obtained.

(Second Invention) As a result of intensive research to solve the above-mentioned problems of the prior art, the present inventor forcibly condenses and collects the pyrolysis vapor by using a cooling device or a coolant. The present invention has been completed by finding that it is possible to eliminate the drawbacks of the above-mentioned conventional methods (1) and (2) by efficiently aggregating and using this as an analysis sample. As a result, it becomes possible to analyze trace substances that easily volatilize, and it is possible to perform analysis with higher sensitivity than conventional methods.

[0009]

BEST MODE FOR CARRYING OUT THE INVENTION Next, the present invention will be described in detail with reference to preferred embodiments of the present invention. (First Invention) FIG. 1 is a schematic perspective view showing an example of the sample decantation apparatus of the present invention, and the present invention will be described based on this. In the figure, A is a sample, B is the container,
C is a container holder, D is a rotation support part, E is a large disk of elastic material such as rubber, F is a small disk made of rubber, G is a handle or electric motor for rotating the small disk, and H is Props,
Reference numeral I denotes a rubber stand for preventing vibration transmission, and J denotes a holding arm that connects the container holder C and the rotation support portion D. Both E and F are discs or fan-shaped discs made of an elastic material such as rubber, but the present invention is characterized in that their curvatures are significantly different. That is, the ratio of the diameters of the large disc of E and the small disc of F is preferably 1: 1 to 1
000: 1, more preferably 10: 1 to 100: 1. Further, as a material forming these disks, any material may be used as long as it can absorb vibration during rotation and can rotate smoothly. For example, in addition to various diene rubbers, non-diene rubbers such as urethane rubber and silicone rubber, or elastic bodies such as elastomers are preferably used. In the present invention, it is particularly preferable to use urethane rubber from the viewpoint of durability and economy.

As shown in FIG. 1, a handle G is provided at the center of the small disc F, and the handle G can be rotated at an arbitrary speed by rotating the handle G manually or by an electric motor. It can be configured. Moreover, FIG.
As shown in FIG. 2, the large disk E and the small disk F are in contact with each other at their side surfaces. As a result, first, when the small disc F is rotated by turning the handle G, the diameter of the large disc E is considerably larger than the diameter of the small disc F as described above. It will rotate.
For example, when the diameter ratio of the large disc E and the small disc F is 50: 1, when the small disc F makes one rotation, the large disc E becomes 0.02.
Rotate and spin slowly and smoothly.

Next, as shown in FIG. 1, a rotation support portion D is provided at the center of the large disc E, and the slow rotational movement of the large disc E is fixed to the rotation support portion D. It is transmitted to the container holder C provided at the tip of the holding arm J via the holding arm J. Further, the container B is firmly held on the container holder C. Therefore, when the large disc E is rotated slowly and smoothly by turning the handle G, the container B is slowly and smoothly inclined accordingly, and the supernatant liquid gently flows out to be separated into precipitates cleanly. That is, by arbitrarily controlling the rotation of the handle G, the container B can be tilted at an arbitrary speed and an arbitrary angle, so that the sample can be decanted in the same manner as the conventional manual operation. In a further preferred embodiment, if a vibration transmission preventing rubber base I is provided under the rotation support portion D so as to be connected to the rotation support portion D, vibration during rotation can be further prevented and the container can be gently tilted. Become.

(Second Invention) The present invention will be described in detail below with reference to preferred embodiments of the second invention of the present invention.
The present invention is characterized in that the pyrolysis vapor of a sample is forcibly cooled and collected by using a cooling device or a cooling agent, and then the condensate is analyzed by an infrared spectroscopic analysis device. As a method of thermal decomposition, a sample is put in a thermal decomposition container having a lid, and this is heated by a heating means to be thermally decomposed. As a thermal decomposition container for the sample used at this time, a heat-resistant container such as a porcelain, a metal, quartz, or hard glass with a lid is preferable. For example, it is possible to find useful containers in various types of commercially available crucibles, cells for spectrophotometers, and the like.

As a method for heating the sample, an electric heating device such as a hot plate, a high frequency induction heating device,
Any means such as infrared ray, laser beam, electron beam and X-ray can be used. For example, when a laser beam is used as the heating device, a minute portion of the sample can be thermally decomposed, so that effective analysis can be performed even in the case where only a small amount of sample can be sampled. A preferable decomposition temperature at the time of thermal decomposition varies depending on the sample to be analyzed, but heating is performed in the range of 100 to 2000 ° C.
The atmosphere for pyrolyzing the sample is appropriately selected from air, dry air, inert gas, etc., depending on the sample to be analyzed. The pressure at this time may be normal pressure, increased pressure, or reduced pressure.

In the present invention, at the time of pyrolysis, the lid or wall side of the pyrolysis vessel is cooled by an electronic cooling device, a coolant, etc., and the pyrolysis gas is forcibly condensed. As a method for cooling the lid or the wall side, a method using an electronic cooling device, a method of dropping a low boiling point solvent such as acetone on the lid and cooling by utilizing latent heat of vaporization is preferably used.

Next, scrape off the condensed agglomerates on a lid or the like,
Using this as a sample, ordinary infrared spectroscopic analysis such as a film method or a tablet method is performed. If the material of the lid reflects infrared light well, infrared spectroscopic analysis is performed as it is by various reflection methods such as ordinary reflection method, high sensitivity reflection method and multiple reflection method. Furthermore,
When an infrared transmitting material such as potassium bromide is used as the lid, it can be used as it is for infrared spectroscopic analysis by a transmission method.

[0016]

The present invention will be described in more detail with reference to the following preferred examples. <Embodiment 1> FIG. 2 shows another embodiment of the decantation apparatus of the present invention. Since such a device includes a plurality of container holders C, it is possible to gently and slowly incline a large number of containers at one time. As a result, a large amount of decantation can be performed at one time, and efficient separation processing can be performed.

<Embodiment 2> FIG. 3 shows another embodiment of the decantation apparatus of the present invention. As shown in FIG. 3, the apparatus has a fan-shaped large disc E. As a result, the rotation support portion D provided at the center of the large disc E differs from the apparatuses shown in FIGS. 1 and 2. Since it is located at the bottom of the device, the tilt fulcrum and the center of gravity of the container are lowered. As a result,
The transmission of vibrations to the precipitate is smaller and decantation is more complete. Also in this case, as shown in FIG. 3, if a vibration transmission preventing rubber base I is provided under the rotation support portion D so as to be connected to the rotation support portion D, vibration during rotation can be further prevented, and the container can be prevented. It is possible to tilt it quietly.

(Second invention) <Example 3> As a sample, a substance suspected of containing an amino group is placed in a porcelain crucible having a lid of 30 ml. Next, the magnetic crucible containing the sample is put on a hot plate for 200 to 60
The sample is pyrolyzed by heating to 0 ° C. Next, acetone is dropped as a cooling medium on the lid to cool it. As a result, the substance condensed on the back side of the lid is scraped off and subjected to infrared spectroscopic analysis by a usual transmission method. As a result, an acid amide was confirmed by a peak near 1675 cm ⁻¹ , which showed that the original sample contained an amino group.

[0019]

【The invention's effect】

(First invention) By configuring the decantation device as in the present invention as described above, it is possible to gently and slowly incline the container without transmitting vibration such as shaking of the hand. It is possible to perform a large amount of decantation quickly and safely.

(Second invention) As described above, according to the present invention, the pyrolysis vapor is efficiently aggregated and collected by cooling using a cooling device or a cooling agent, and this is used as an analysis sample in infrared rays. By performing the spectroscopic analysis, it is possible to detect a trace substance, which was easily volatilized by the conventional method, with high sensitivity and easily by the infrared spectroscopic analysis method. Furthermore, if a laser beam or the like is used as a heating method, it becomes possible to thermally decompose a minute portion of the sample and perform infrared spectroscopic analysis. Further, since the thermal decomposition container used in the present invention is a heat-resistant container such as a porcelain or a metal, there is no risk of damage even if a cooling agent such as a low boiling point solvent is dropped during cooling, and operational safety. It is also economical.

[Brief description of drawings]

FIG. 1 is a schematic perspective view of a decantation apparatus for a sample according to a first aspect of the present invention.

FIG. 2 is a schematic perspective view of a sample decantation apparatus according to another aspect of the first aspect of the present invention.

FIG. 3 is a schematic perspective view of a sample decantation apparatus according to another aspect of the first aspect of the present invention.

[Explanation of symbols]

 A: Sample B: Container C: Container holder D: Rotating support E: Large disk or fan disk F: Small disk G: Handle or motor H: Strut I: Vibration prevention rubber stand J: Holding arm

Claims (6)

[Claims] 1. Large and small 2 having circumferences having remarkably different curvatures
Two disks and / or fan-shaped disks are in contact with each other on their circumferential surfaces, and a handle or a motor for rotating the small disk is provided at the center of the small disk, and a rotation support provided at the center of the large disk A decantation device for a sample, wherein a holding arm is fixed to the part, and a container holder is installed at the tip of the holding arm. 2. Large and small 2 having circumferences having markedly different curvatures
The sample decanting device according to claim 1, wherein the one disk and / or the fan-shaped disk is made of an elastic material. 3. The decantation device for a sample according to claim 1, wherein the elastic body is rubber or elastomer. 4. The decantation device for a sample according to claim 1, wherein a rubber stand for preventing vibration transmission is provided below the rotation support part. 5. The sample is placed in a pyrolysis container with a lid and heated, the pyrolysis vapor is cooled and collected by a cooling device or a coolant to form an aggregate, and then the condensate is analyzed by infrared spectroscopy. Pyrolysis-infrared spectroscopy characterized by being analyzed by a device. 6. The thermal decomposition-infrared spectroscopic analysis method according to claim 4, wherein the acid amide group contained in the aggregate of the thermal decomposition vapor is analyzed to confirm the amino group.