JPH0694701A - Device for collecting thermally decomposed object - Google Patents

Abstract

PURPOSE:To provide a device for collecting a thermally decomposed product of an organic compound efficiently with a relatively simple configuration and without requiring any complex operation. CONSTITUTION:This device is provided with a heat-resistance transparent container body 1 whose one edge is sealed and which is heated from an outer- periphery surface side, a removable close-down body 2 sealing the other edge opening of the transparent container body 1 airtightly, and an infrared ray transmission type substrate 3 for capturing a thermally decomposed product which is fitted to and laid out at the upper-side space part inside the transparent container body 1 so that it can be removed. Further it is provided with an atmosphere switching means 6 for switching the atmosphere inside the transparent container body 1 while it is fitted to the close-down body airtightly, a sample 5 to be thermally decomposed which is fitted to the close-down body 2 airtightly and stays inside the transparent container body 1, and an insertion/ delivery part 7 for inserting and delivering a thermally decomposed residue.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a thermal decomposition product collector, and more particularly to a thermal decomposition product collector suitable for preparing a sample for infrared absorption spectrum analysis.

[0002]

2. Description of the Related Art For example, an organic compound having a molecular weight of tens of thousands or more, which is difficult to extract even by an extraction operation with an organic solvent such as a cross-linked / cured resin, and a filler such as calcium carbonate or glass fiber are formed. The existing molded body is widely put to practical use as a structural material, an insulator, and the like. The separation and analysis of organic compounds (resins and rubbers) in the molded body are generally performed for the purpose of improving the usage and characteristics or functions of these molded bodies. As a means for separating and analyzing only the organic compound in the molded body,
The following thermal decomposition methods are known. In other words, after removing relatively low molecular weight components from the sample to be thermally decomposed in advance by Soxhlet extraction that requires several hours, the components (sample) that remain unextracted can be extracted, for example, in test tubes or containers of similar shape. The sample is housed inside and a test tube or the like is heated by, for example, a gas burner to decompose the high molecular weight organic compound in the sample. That is, the molecular chain of the high molecular weight organic compound is cut by heating to form a low boiling point decomposition component in a low molecular state, cooled and condensed on the inner wall surface of a test tube, and the condensate condensed on the inner wall surface is Samples are collected with a collection tool such as a spatula, applied to and deposited on the surface of a KBr collection substrate, and then subjected to infrared spectroscopic analysis and other analysis devices.

[0003]

However, in the case of the means for separating and analyzing the organic compounds (resins and rubbers), there are the following practical problems. First, since a relatively low molecular weight component is removed as a pretreatment by Soxhlet extraction which requires several hours, there are disadvantages that the operation is complicated and it takes a long time. Further, when the condensate condensed on the inner wall surface of the test tube or a container having a similar shape by thermal decomposition is collected by a collecting tool such as a spatula, an amount necessary for analysis depending on the state of the condensate or the amount of condensation,
For example, it is often impossible to collect an amount of several mg. In other words, due to the fact that condensate condenses over a wide area on the inner wall surface of the container, and the amount of it that adheres to and remains on the inner wall surface of the container and the spatula is relatively large, only a part of it can be sampled and used. It may not be possible to perform an analysis.

Although there is a means for recovering the condensate by dissolving it in an organic solvent for the difficulty of collecting the condensate, it is not practical because the operation is complicated and the efficiency is poor. In any case, in the case of a means for thermally decomposing the organic compound and collecting the decomposition products, the condensate is condensed in a wide range on the inner wall surface of the container, or adheres to the inner wall surface of the container or a spatula. Considering the residual amount, it can be said that it is not suitable for the preparation of this kind of analytical sample, because a few gr of condensate is required to secure the required sample amount (about several mg or more) for analysis.

The present invention has been made in view of such circumstances, and has a relatively simple structure and efficiently collects a thermal decomposition product of an organic compound without requiring complicated operations. An object of the present invention is to provide a device for collecting a thermal decomposition product that can be used.

[0006]

A thermal decomposition product collector according to the present invention comprises a heat-resistant transparent container body having one end sealed and heated from the outer peripheral surface side, and the other end of the transparent container body. A detachable closure that hermetically seals the opening, an infrared transmissive thermal decomposition product collection substrate that is detachably mounted and arranged in the upper space of the transparent container body, and the closure is Atmosphere switching means that is airtightly attached and switches the atmosphere inside the transparent container body, and an insertion / exhaust part that is airtightly attached to the closure body and that inserts / discharges the thermally decomposed sample and the thermal decomposition residue into the transparent container body. It is characterized by comprising.

The infrared transmission type substrate for collecting thermal decomposition products is, for example, a plate made of KBr, Si, ZnSe or the like, which is transparent to infrared light and interferes with the analysis and measurement of the collected thermal decomposition products. A material that does not invite is selected. The shape of the substrate for collecting the thermal decomposition products. The size of the transparent container body and the device used for analysis and measurement. Although appropriately set in consideration of the size and the like, the mounting / arrangement in the transparent container main body is a region of a relatively low temperature above the sample to be thermally decomposed to be inserted and arranged and at the time of the thermal decomposition operation.

[0008]

In the device for collecting thermal decomposition products according to the present invention,
Since the substrate for collecting thermal decomposition products is mounted and placed in a relatively low temperature area inside the transparent container body that thermally decomposes organic compounds, the products generated by thermal decomposition are the surfaces of the substrate for collecting thermal decomposition products. Preferentially condense. That is, since the thermal decomposition products are condensed on the inner surface of the transparent container body having a relatively large area and directly attached to the analyzer, the thermal decomposition products are condensed on the surface of the collecting substrate having a relatively small area. Even when the thermal decomposition product (condensable substance) does not reach several gr, it is possible to reliably achieve the condensation and securing of several mg of the thermal decomposition product required for analysis and measurement. More specifically, the amount of adhesion / remaining on the inner wall surface of the transparent container body can be reduced, while the adhesion / remaining on the spatula etc. can be eliminated / avoided, so that the efficient condensation and securing of the thermal decomposition products can be achieved. This makes it possible to sufficiently perform infrared spectroscopic analysis (infrared spectroscopic measurement) of an organic polymer compound by a thermal decomposition product, which has been difficult or practically difficult in the past.

[0009]

Embodiments of the present invention will be described below with reference to FIGS. 1, 2, 3 (a), 3 (b) and 4.

Example 1 FIG. 1 is a cross-sectional view showing the main part of a constitutional example of a thermal decomposition product collecting apparatus according to the present invention, in which one end is sealed and heated from the outer peripheral surface side. A heat-resistant transparent container body, for example, an outer diameter 15 mm, an inner diameter 12 mm, and a length 100 mm, which is a sealed glass tube at one end, and 2 is a removable closure body for hermetically sealing the other end opening of the transparent container body 1, For example, it is a closing body (sealing tool) made of acrylic resin. Further, 3 is the transparent container body 1
Infrared transmission type pyrolysis product collection substrate that is removably mounted and placed in the upper space inside, such as KBr, Si, ZnSe
It is a disc made of mm in diameter. The substrate 3 for collecting thermal decomposition products is slidably inserted and arranged in the closing body 2 and is mounted on the tip end side of the support operation rod 4, and the thermally decomposed sample 5 to be enclosed is arranged. It is configured so that it can be placed above. Further, 6 is an atmosphere switching means that is airtightly attached to the closure body 2 and switches the atmosphere inside the transparent container body 1.
Prior to the thermal decomposition operation of the sample to be thermally decomposed 5, the transparent container body 1 is filled with, for example, a dry inert gas (N ₂ or the like), or the inside of the transparent container body 1 is evacuated to generate the thermal decomposition product. The atmosphere is switched so as to prevent adhesion of an undesired substance to the object collecting substrate 3 or erosion by moisture. Furthermore, 7 is an insertion / exhaust portion which is also airtightly attached to the closure body 2 for inserting the sample to be pyrolyzed 5 into the transparent container body 1 and discharging the pyrolysis residue. Therefore, in this thermal decomposition product collecting device, the transparent operating device 4 is integrated with the closing body 2 such as the supporting operation rod 4 of the substrate 3 for collecting the thermal decomposition products with respect to the transparent container body 1, the atmosphere switching means 6, and the inserting / discharging part 7. The transparent container body 1 is separated by attaching and detaching the closing body 2.

Next, an example of use of the heat decomposition product collecting device having the above-mentioned structure will be described.

First, the transparent container body 1 is filled with dry N ₂ gas, and a KBr disk 3 as a substrate for collecting pyrolysis products 3 is supported and mounted on the tip side of the supporting operation rod 4. Two
Is attached to the opening on the other end and hermetically sealed. On the other hand, 2 mg of polyvinyl chloride resin is inserted as the sample 5 to be decomposed into heat from the inserting / exhausting part 7 for inserting the sample 5 to be decomposed into the closure 2 and discharging the decomposition residue to make the transparent container body 1 substantially horizontal. While being held, the portion where the sample 5 to be pyrolyzed was arranged was heated from the outside by a gas burner to thermally decompose the polyvinyl chloride resin 5. By this thermal decomposition operation, a low molecular weight product due to the thermal decomposition of the polyvinyl chloride resin 5 was easily condensed and deposited on the surface of the KBr disk 3.

After that, the atmosphere switching means 6 is activated to switch the atmosphere in the transparent container body 1 and then the closing member 2 is closed.
On the other hand, the KBr disk 3 on which the pyrolysis products were condensed and adhered was removed, and the KBr disk 3 was attached to an infrared spectrophotometer and infrared spectroscopic analysis was performed. An infrared spectrum was obtained.

Embodiment 2 FIGS. 3 (a) and 3 (b) are cross-sectional views showing the main parts of another structural example of the thermal decomposition product collecting apparatus according to the present invention, wherein 8 is sealed at one end. And a heat-resistant transparent container body that is heated from the outer peripheral surface side, for example, a one-end sealed rectangular glass tube having an outer diameter of 15 × 15 mm, an inner diameter of 12 × 12 mm, and a length of 100 mm, 9 is the transparent container body 8 Is a detachable closing body that hermetically seals the other end opening, for example, an acrylic resin closing body (sealing tool). Reference numeral 10 denotes an infrared ray transmissive type pyrolysis product collecting substrate which is detachably mounted and arranged in the upper space of the transparent container body 8, for example, a side of 13 × 2 mm made of KBr, Si, ZnSe. It is a plate. Then, the substrate 10 for collecting the thermal decomposition products,
The transparent container main body 8 is slidably mounted on the surface of the supporting portion 11 which also functions as a guide and is formed by protruding a part of the opposite sides of the transparent container main body 8 inwardly. It is configured to be possible. Further, 6 is an atmosphere switching means that is airtightly attached to the closure body 9 and switches the atmosphere in the transparent container body 8, and in the transparent container body 8 prior to the thermal decomposition operation of the thermally decomposed sample 5. For example, it is filled with a dry inert gas (N ₂ etc.) or the inside of the transparent container body 8 is evacuated to prevent adhesion of an undesired substance to the thermal decomposition product collecting substrate 10 or erosion prevention by water. Switch the atmosphere as you would. Furthermore, 7 is an insertion / exhaust portion which is also airtightly attached to the closure body 9 for inserting the sample to be pyrolyzed 5 into the transparent container body 1 and discharging the pyrolysis residue. Therefore, in this thermal decomposition product collecting device, the transparent container body 8 and the supporting portion 11 of the substrate 10 for collecting thermal decomposition products are integrated, and the transparent container body 8
The atmosphere switching means 6 and the inserting / discharging portion 7 are integrated with the closing body 2.

Also in the case of this heat decomposition product collecting apparatus, it is used in accordance with the use and operation of the above-mentioned Example 1, and 2 mg of polyvinyl chloride resin is inserted into the transparent container body 8 as the sample 5 to be decomposed by heat. The polyvinyl chloride resin 5 was thermally decomposed by heating the portion where the sample to be pyrolyzed 5 was placed from the outside with a gas burner in a state where the transparent container body 8 was mounted and held substantially horizontally. By this thermal decomposition operation, a low molecular weight product resulting from the thermal decomposition of the polyvinyl chloride resin 5 was easily condensed and deposited on the lower surface of the KBr square plate 10.

Thereafter, the atmosphere switching means 6 is activated to switch the atmosphere in the transparent container body 8, and then the closing member 9 is closed.
On the other hand, the KBr square plate 10 on which the pyrolysis products are condensed and adhered is removed, and the KBr square plate 10 is attached to the infrared spectrophotometer to perform infrared spectroscopic analysis. An infrared spectrum was obtained.

As can be seen from the above examples, according to the thermal decomposition product collecting apparatus of the present invention, even if a sample to be decomposed by heat of about several mg, which has been practically impossible to collect, Since the thermal decomposition products capable of performing the required infrared spectroscopic analysis can be condensed / deposited or collected (collected), infrared spectroscopic analysis of this type of polymer organic compound can be easily performed.

[0018]

EFFECTS OF THE INVENTION According to the thermal decomposition product collecting apparatus of the present invention, compared with the conventional thermal decomposition product collecting and collecting means, even if the sample to be decomposed by heat is about 1/10, It is possible to directly collect (condensate / deposit) the condensate (product) of (1) on the surface of the collection substrate, and to perform required infrared spectroscopic analysis and the like. And, it is enough that the sample to be decomposed by heat is as small as a few mg.
It is possible to shorten the time required for condensation by heat decomposition and collection of products by heat decomposition on the surface of the substrate or collection (collection) on the substrate surface, such as sample preparation such as infrared spectroscopic analysis of high molecular weight organic compounds. Can bring many advantages in.

[Brief description of drawings]

FIG. 1 is a cross-sectional view showing a main part of a configuration example of a thermal decomposition product collecting apparatus according to the present invention.

FIG. 2 is an infrared spectrum diagram showing an infrared spectrum example of a condensate collected on a collection substrate surface by the thermal decomposition product collection device shown in FIG.

3A and 3B show essential parts of another configuration example of the thermal decomposition product trapping apparatus according to the present invention, in which FIG. 3A is a horizontal sectional view and FIG. 3B is a vertical sectional view.

FIG. 4 is an infrared spectrum diagram showing an infrared spectrum example of a condensate collected on a collection substrate surface by the thermal decomposition product collection device shown in FIG.

[Explanation of symbols]

1, 8 ... Heat-resistant transparent container body 2, 9 ... Closure body (sealing tool) 3, 10 ... Infrared transmission type thermal decomposition product collection substrate 4 ... Collection substrate supporting operation rod 5 ... Heat Decomposition sample 6 ... Atmosphere switching means 7 ... Insertion of a sample to be decomposed by heat and discharge of pyrolysis residue 11 ... Supporting part for collecting substrate

Front page continuation (72) Inventor Kimito Sakai 1 Komukai Toshiba-cho, Sachi-ku, Kawasaki-shi, Kanagawa Stock company Toshiba Research Institute

Claims (1)

[Claims] 1. A heat-resistant transparent container body having one end sealed and heated from the outer peripheral surface side, a removable closure body hermetically sealing the other end opening of the transparent container body, and the transparent container body. An infrared-transmissive thermal decomposition product collection substrate detachably mounted and arranged in the upper space of the inside, and an atmosphere switching means that is airtightly attached to the closing body to switch the atmosphere inside the transparent container body, An apparatus for collecting a thermal decomposition product, comprising: an insertion / exhaust portion that is airtightly attached to the closure and inserts / exhausts a sample to be thermally decomposed into the transparent container body and a thermal decomposition residue.