JPH0329746Y2 - - Google Patents

Description

[Detailed explanation of the invention] (a) Industrial application field The present invention relates to an evolved gas analyzer that analyzes evolved gases generated during a thermal analysis process. Analysis of gases generated during the entire process of gas analysis and thermal analysis,
The present invention relates to an evolved gas analyzer that can perform so-called total analysis with a single device.

(b) Prior art Generated gas analyzers are used to qualitatively and quantitatively quantify generated gases such as decomposed gases generated in the thermal analysis process, and make the results of thermal analysis more detailed and accurate. The gas analyzer has a structure in which a separation column for gas chromatography analysis is connected to the generated gas path of the thermal analyzer through a hexagonal tube equipped with a measuring tube. However, it was difficult to analyze each component of all gases generated in the entire temperature range of thermal analysis. Therefore, the analysis of each component of all generated gases generated in the entire temperature range of such thermal analysis is obtained by integrating the analysis results of each generated gas.

However, the result of integration in this way is
This tends to cause bias, and in order to obtain more accurate results, it is necessary to reduce the measurement temperature interval, which causes a problem in that the number of analyzes is increased more than necessary. Furthermore, for example, decomposed gas is generated over a relatively wide temperature range, making it difficult to detect trace components and causing analysis errors.

(C) Purpose The purpose of this invention is to solve the problems of conventional generated gas analyzers. The object of the present invention is to provide a generated gas analyzer that can analyze each component of generated gas at different temperatures and can quantify the total amount of each component of generated gas in the entire temperature range of thermal analysis.

(D) Structure The present invention focuses on the fact that by filling the column with an appropriate packing material, the components to be measured can be easily collected in the column from the gas generated in the entire temperature range of thermal analysis. This was achieved by connecting a measuring tube and a column filled with a suitable temperature-adjustable packing material to collect the component to be measured.

That is, the present invention provides a developed gas analyzer in which a chromatographic analyzer is connected to the generated gas path of the thermal analyzer, and one connection port of the Happo Kotsukku, which has four connection paths for flow path switching, is connected to the generated gas path of the thermal analyzer. Connect to the generated gas path, connect the two connection ports of the adjacent Happo Kotsu to the inlet and outlet of the metering tube, and connect the two connection ports of the adjacent Happo Kotuku to the collection column temperature setting device. It is characterized in that it is connected to the inlet and outlet of the collection column, and the remaining connection port of the Happo-kottoku is connected to the inlet of the separation column for gas chromatography analysis, the carrier gas flow path, and the gas discharge path. It is located in the generated gas analyzer.

In the present invention, the Happo Kotsuku has eight channels, and the connections between these channels can be changed as appropriate, and any Happo Kotsuku (including Happo valves) can be used as long as it can do this. can also be used. As the eight-way valve, various types of valves and valves such as rotary slide valves, linear slide valves, piston valves, etc. can be used. For rotary slide valve models, 8
The rotor has a stator having eight flow channels extending individually from eight connection ports, and a rotor having flow channels for appropriately switching and connecting these flow channels.

This Happo Kotuku is designed to prevent gases generated from decomposition gas, etc.
It is housed in a heat insulating tank to prevent condensation within this flow path.

The collection column is a collection column temperature setting device that can easily set the temperature so that at least one component in generated gas such as cracked gas can be easily and smoothly condensed and collected, and can also flow out easily and smoothly. placed within. The collection column is filled with a packing material to perform such gas collection.

To connect the connection port of the Happo Kotuku to the generated gas path, metering tube inlet and outlet, collection column inlet and outlet, separation column inlet for gas chromatography analysis, carrier gas flow path, and gas discharge path of the thermal analyzer. , it is preferable that the switching operations are connected in order, for example, according to the rotational direction of the rotor.

An embodiment of the present invention will be described below with reference to the accompanying drawings, but the technical scope of the present invention is not limited by this description.

(E) Embodiment The figure is a schematic explanatory diagram showing an embodiment of the generated gas analyzer of the present invention.

In this example, the generated gas analyzer includes a thermal analyzer 1, such as a differential thermal analyzer, an eight-way valve 2, a metering tube 3, a column 4 for collecting components to be measured in the generated gas,
It is formed by connecting a collection column temperature setting tank 5, a gas chromatograph 6, a heat insulating tank 7, a carrier gas for thermal analysis 8, a carrier gas passage 9, and a gas discharge passage 10.

The Happo valve 2 has connection ports 11, 12, 13,
A total of eight channels, 14, 15, 16, 17, and 18, are formed. Among these connection ports, connection port 11 connects to the generated gas path 19 of the thermal analyzer 1, connection port 12 connects to the inlet 20 of the metering tube 3, and connection port 13 connects the metering tube to the dashed line 27. ,27
1, 272, and 273, the generated gas of the thermal analyzer 1 in the constant-rate heating process is transferred from the generated gas path 19 to the connection port 11, the connection flow path 27, and the connection port 1.
3. Inlet 20 and outlet 21 of metering tube 3, connection port 1
2. Flow from the connection channel 271 and connection port 18 to the gas discharge channel 10. On the other hand, the carrier gas flows from the carrier gas flow path 9 to the connection port 17 and the connection flow path 27.
2, connection port 14, inlet 2 of the collection column 4
2 and outlet 23, connection port 15, connection flow path 273,
It flows from the connection port 16 to the analytical separation column 24 of the gas chromatograph.

When the temperature of the thermal analyzer 1 reaches a predetermined temperature, the rotor of the eight-way valve is turned clockwise so that the connection passage of the rotor is set as shown by the dotted line, and the carrier gas flows from the carrier gas passage 9 to the eight-way valve 2. It enters the connection port 17, passes through the connection channel 281 to the connection port 12, and enters the metering tube 3 from the inlet 20 of the metering tube 3.
The generated gas is metered into the metering tube 3 from the outlet 21 of the metering tube 3 to the connecting flow path 282 and the connecting port 1.
6, it flows into the analysis separation column 24 of the gas chromatograph 6 from the inlet 25, and the component concentration is detected by the detector 30. In this way, the dashed line 2
7, 271, 272 and 273 are connected, and the generated gas is metered into the metering tube 3, and then the dotted line connection channels 28, 281, 282 and 283 are connected to the outlet 21 of 3, and connected. The port 14 is connected to the inlet 22 of the column 4 for collecting the component to be measured in the generated gas.
In addition, the connection port 15 is connected to the outlet 23 of the column 4 for collection.
, the connection port 16 is connected to the inlet 25 of the analytical separation column 24 of the gas chromatograph, the connection port 17 is connected to the carrier gas flow path 9, and the connection port 1
8 is connected to a gas exhaust flow path 10. The connection flow path on the rotary side of the eight-way valve is the real line 26, 2.
61, 262 and 263, chain lines 27, 27
1,272 and 273 and dotted lines 28, 28
1,282,283, connection port 1
Between 1 and 18, connections can be made in at least three ways.

The gas chromatograph 6 is provided with a standard side column 29 alongside an analytical separation column 24, both of which are connected to an outflow path 31 via a detector 30.

Since the generated gas analyzer of this example is constructed as described above, the component analysis of the generated gas at each temperature is performed by switching the flow path for connecting the rotor of the eight-way valve. In this way, changes in the concentration of the generated gas can be measured.

When quantifying the total amount of each component of generated gas,
First, connect the rotor to the solid lines 26, 261, 2.
62 and 263. Generated gas generated during thermal analysis passes from the generated gas path 19 of the thermal analyzer 1 through the connection port 11, the connection flow path 261, and the connection port 14, and then enters the column 4 for collecting the measurement component in the generated gas from the inlet 22. The gas flows from the outlet 23 to the gas discharge path 10 via the connection port 15, the connection flow path 262, and the connection port 18.

A refrigerant such as liquid oxygen is appropriately placed in the collection column temperature setting tank 5 in which the column 4 for collecting the measurement component is accommodated, depending on the measurement component, and the collection column temperature setting tank 5 houses the column 4 for collecting the measurement component. The column 4 used for this purpose is cooled to a predetermined temperature. Further, the column 4 for collecting the component to be measured in the generated gas is filled with an appropriate filler depending on the component to be measured.

When the thermal analysis is completed, turn the rotor of the eight-way valve to connect the connecting channels to the dotted lines 28, 281, 28.
2 and 283. Components to be measured in gas generated during thermal analysis are collected in the column 4 for collecting the components to be measured. Therefore, the refrigerant is removed from the collection column temperature setting tank 5, and a suitable heating medium such as hot water or heating oil is added to heat the collection column 4 in which the measurement component is collected. When the column 4 for collecting the component to be measured is heated to the optimum temperature, the rotor of the eight-way valve is turned to switch from the dotted line connecting channels 28, 281, 282, and 283 to the one-dot chain line connecting channel. Therefore, the carrier gas enters from the carrier gas flow path 9, through the connection port 17, the connection flow path 272, and the connection port 14, into the column 4 for collecting the measurement component in the generated gas through its inlet 22, and the measurement component is also collected. The water flows all at once from the outlet 23 of the collection column 4, via the connection channel 273 and the connection port 16, into the analysis separation column 24 from its inlet, and is analyzed.

In this manner, in the present invention, it is possible to measure the concentration change of the generated gas in thermal analysis and the total amount of each component of the generated gas using a single generated gas analyzer.

(f) Effects In this invention, a collection column for collecting measurement components in the generated gas is provided in the collection column temperature setting device, and this collection column is attached to the switching unit of the generated gas analyzer. It is now possible to quantify the total amount of each component of the generated gas in thermal analysis by switching the flow path, so there is no need to integrate each component concentration change individually, as in the past. Since the bias in the sample does not double and trace components are concentrated, the measurement becomes more accurate and the reliability of the measured value is improved. Furthermore, in the present invention, a Happo Kotoku is used in the switching part of the generated gas analyzer, and a collection column for collecting the measured components in the generated gas is connected, as well as a measuring tube. With the simple operation of switching paths, and with a single device, it is possible to measure changes in the concentration of each component of the generated gas due to temperature changes in thermal analysis, as well as measure the total amount of each component of the generated gas. It is convenient to use because it can be

As described above, the generated gas analyzer of the present invention has many functional advantages over conventional devices, and its influence is significant.

[Brief explanation of drawings]

The figure is a schematic explanatory diagram showing one embodiment of the generated gas analyzer of the present invention. 1 is a thermal analysis device, 2 is a Happo Kotoku, 3 is a metering tube, 4 is a column for collecting measurement components in the generated gas,
5 is a column temperature setting tank, 6 is a gas chromatograph, 7 is a heat insulating tank, 8 and 9 are carrier gas channels, and 10 is a gas discharge channel.

Claims (1)

[Scope of utility model registration request] In a generated gas analyzer in which a chromatographic analyzer is connected to the generated gas path of the thermal analyzer, one connection port of the Happo Kotoku, which has four connection paths for flow path switching, is connected to the generated gas path of the thermal analyzer. , connect the two connection ports of the adjacent Happo Kotsu to the inlet and outlet of the measuring tube, and connect the two connection ports of the adjacent Happo Kotsu to the inlet and outlet of the collection column provided in the collection column temperature setting device. What is claimed is: 1. A generated gas analyzer, characterized in that an Happo kettle is provided by connecting the remaining Happo kettle to the inlet of a separation column for gas chromatography analysis, a carrier gas flow path, and a gas discharge path.