JPS6046449A - Volatile product gas trap device for thermogravimetric measuring device - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a trap device for vaporized gas used in a thermogravimetric measuring device, and in particular, it traps vaporized gas generated by heating a sample during thermogravimetric measurement.
The present invention relates to a trap device for a thermogravimetric measuring device that captures only volatile components having a boiling point above a preset temperature and discharges volatile components below that boiling point as gas.

(Prior art) A thermogravimetric measuring device heats a sample while changing the temperature at a constant rate, measures the quality of the sample as a function of temperature, and detects dehydration from the sample during heating, acid reduction due to thermal decomposition reaction, etc. , which measures the increase in mass due to adsorption and oxidation reactions, and is particularly widely used to determine the state of polymeric substances.

When this thermogravimetric measuring device is used to measure samples such as synthetic polymer substances or coal as a thermal decomposition reaction, volatile components with a boiling point corresponding to the temperature added to these samples become gas and volatilize. When introducing this volatilized gas into an analysis device such as a gas chromatograph device through an introduction tube such as a vinyl tube, the temperature of the introduction tube is lower than the sample heating temperature, so the volatilized gas is generated inside the introduction tube. The gas will condense. This reduces the cross-sectional area of the gas flow path in the introduction pipe, causing fluctuations in the gas flow rate.
As a result, there was a drawback that buoyancy was imparted to the balance section of the thermogravimetric measuring device, making it impossible to perform accurate weight measurements. It's ox.
In addition, there is a method in which a filler is placed inside the cell, the volatile gas is passed through it, and the vaporized gas is condensed and collected by the filler. This method has the disadvantage that the agent must be heated again to volatilize it, which is cumbersome.

(Object of the Invention) The present invention solves the drawbacks of the prior art described above, and includes a trap container connected to the lower part of the reaction container of a thermogravimetric measuring device, and a trap center protruding from the center of the bottom of the trap container. This is a thermogravimetric measuring device in which a heat pipe, which is lower in temperature than the wall surface of the trap container, is inserted into the trap center, and the volatile products are collected on the outer wall of the trap center to increase the trapping efficiency. The purpose of this product is to provide a complete vaporization gas trap device.

(Structure of the Invention) The present invention heats a reaction vessel using a heating device while changing the temperature at a constant rate, and connects the reaction vessel in such a way that the vaporized gas evaporated from the sample in the reaction vessel is passed all the way through the lower opening of the reaction vessel. The trap center, which protrudes from the center of the bottom of the trap container and is inserted into the reaction container through the opening of the reaction container, is connected to a heat pipe connected to a cooling device that can be set to an arbitrary cooling temperature. The high boiling point volatile product gas, which becomes liquid or solid again at this temperature, is condensed in the trap center.
In short, it is possible to efficiently collect and emit 1 J of the low-boiling point volatilized gas that is a gas at that temperature from the trachea.

(Example) (Figures 1 to 8) Figure 1 is a side sectional view of a vaporized gas trap device for a thermogravimetric measuring device of the present invention, and Figure 2 is a side sectional view of the main parts of a trap container. FIG. 3 shows another embodiment of the trap vessel.

In Figure 1, ■ is a tube that houses the support part of the hanging type weight measuring device, and 7 is a carrier gas injection hole into which a carrier gas such as helium or nitrogen is injected into the tube.
is connected to. Reference numeral 3 denotes a support portion of a hanging type thermogravimetric measuring device, which is supported by a support device (not shown) with respect to the tube body 1. 2 is an arm, 4 is a support for each sample sample suspended from the tip of arm 2, and 1'i! 5 to 1lS
l: The container 11 holding the sample is suspended. Reference numeral 6 is an opening provided on the side of the body 1, and 5 is a gasket filled between the opening 6 and the side wall of the connecting pipe 8.

Reference numeral 10 denotes a reaction vessel, and its upper part is provided with a concave part that tapers gently in two directions, and is fitted against the widening part that gently widens downward in the connecting tube 8 (&
I'm playing ft5t. 9 is a carrier gas guide section. The lower part of the reaction vessel] 0 is provided with a gently tapering part, extends into a straight tube shape, and is provided with an opening 10' at the bottom thereof. 12 is a heating element made of, for example, a nichrome wire, 25 is a thermocouple, z6 and 28
is a lead wire, and 27 is a temperature control device. thermocouple 25
is placed near the sample container 11, and applies its detected temperature to the temperature control device z7. While monitoring the input detected temperature, the temperature control device 27 applies electric power to the heating body 12 to heat the sample placed in the sample container 11 so that the temperature increases at a constant rate of, for example, 10° C./minute. 15 is a transparent trap container, 15' is a trap center projecting upward from the bottom center of the trap container, and 14 is a vaporized gas exhaust pipe. The trap center 15' is a bottom opening 1 of a straight pipe section connected to the bottom 1 section of the reaction vessel 10.
0', and the widening part that gradually expands upwards at the top of the trap container 15 and the rounded corner part that gradually narrows toward the F direction of the reaction container 10 are fitted and connected. . The exhaust pipe 14 is attached to the trap container 15 at a position higher than the bottom opening 10' of the straight pipe portion of the reaction container 10. Because exhaust pipe 1
4 is provided below the bottom opening 10' of the straight pipe portion of the reaction vessel 10, the volatilized gas discharged from the - port 10' may be introduced into the exhaust fiW 14 without being trapped. . 16 is a heat pipe, 17 is a heat insulator, and 18 is a cooling member, and the lower part of the heat pipe 16 is embedded in the cooling member 18. The cooling member 18 stores, for example, a liquid bottle and the like. Reference numeral 19 denotes a heating furnace for heating the cooling member 18. The heating furnace 19 heats the cooling member 18, vaporizes the liquid nitrogen inside it, and uses the heat of vaporization to cool the cooling member], 8. .

21 is a casing, and the casing 21 is the cooling member 1
8 and the heating furnace 19. 20 is a thermocouple, 2z and 2
4 is a lead wire, and 23 is a temperature regulator that controls the heating power to the heating furnace 19, and controls the heating temperature of the cooling member 18 of the heating furnace 19 while supervising the temperature output from the thermocouple 20. do. Note that the temperature regulator 28 is
A temperature setting means is provided which can arbitrarily vary the cooling temperature of the cooling member 18 by controlling the heating power. The cooling member 8 is heated by the heating furnace 19, and the liquid nitrogen stored therein is vaporized and cooled. This cools the heat pipe 16, and the trap center 15 of the trap container 15 is cooled. Maintain temperature below wall temperature.

FIG. 2 shows the state in which the gas is collected in the trap center, and the vaporized gas from the sample discharged from the reaction vessel IO becomes liquid or solid again at the ambient temperature of the trap center 15' of the trap vessel 15. The high-boiling point volatilized gas is collected as a volatilized product 29, and the low-boiling point volatilized gas that forms a cluster at the temperature i is discharged from the bottom opening 10' of the straight pipe section of the reaction vessel 10. The sample is introduced through an exhaust pipe 14 into a sample introduction section of a gas analyzer (not shown) such as a gas chromatograph or a mass spectrometer through an introduction pipe such as a vinyl tube.

The operation of the device shown in FIG. 1 will be explained.

In the figure, a carrier gas such as helium or ions is injected at a predetermined flow rate from a carrier gas injection hole 7 of a tube 1. The carrier gas flows through the connecting pipe 8 and the carrier gas guide section 9 into the periphery of the sample container 11 located in the reaction container 10 . Heating is performed while changing the temperature at a constant rate controlled by a temperature control device. The volatilized gas that evaporates from the sample in response to the rising heating temperature, together with the carrier gas, fills the gap between the constriction that gradually narrows downward in the reaction vessel 10 and the trap center 15' of the trap vessel 15. flowing down. Since the heat pipe 16 inserted into the trap center 15' is maintained at a lower temperature than the wall surface temperature of the trap container 15 by the cooling member 18, high boiling point volatilization which becomes liquid or solid again at this low temperature is generated. As shown in FIG. 2, the gas is collected around the trap center 15' and becomes a trapped material 29, so that the volatilized product gas with a high d set point is collected on the wall surface of the trap container 15. do not have. Furthermore, the formation of the collected matter 29 that is collected around the trap center 15' can be visually observed through the trap container 15. Only the low-boiling point volatilized gas that forms a gas trap at the low temperature described above is exhausted from the exhaust pipe 14 of the trap container 15. The sample is evacuated from the exhaust pipe 14 and introduced into a sample injection section of a gas analyzer such as a low-boiling point device or a mass spectrometer via a gas introduction pipe such as a vinyl tube, and analyzed. The collected material z9 collected in the trap center 15' of the trap container 15 is collected by removing the trap container 15 from the reaction container 10 and sampling it.
Component analysis is performed using an analysis device such as an I-body chromatography device.

Note that by controlling the cooling temperature of the cooling member 18 with the temperature controller 23, the temperature of the trap center 15' of the trap container 15 is changed to ol', and the high boiling point volatilization to be collected in the trap center 15' is The component substances can be arbitrarily selected, and the low boiling point volatile product gas introduced into the analyzer connected to the exhaust pipe 14 can also be arbitrarily selected.

Furthermore, the temperature of the heat pipe 16 is maintained at a low temperature to condense and collect the vaporized gas in the trap center 15', and then the heat pipe 16 is gradually heated and the gas is captured in the trap center 15'. The collected volatile products are volatilized and introduced into a gas chromatograph device (not shown), and the components of the volatile products can also be analyzed at each heating temperature.

In addition, in this actual example, the configuration is described in which the F blade including the opening of the reaction vessel is suspended perpendicularly to the trap vessel, and the trap center protruding from below is inserted into the opening. The lower part of the container, including the opening, is suspended vertically into the trap container, bent 90 degrees in the middle, and the trap center is horizontally protruded from the side of the i-wrap container, and is deeply inserted into the opening of the reaction container. A product gas trap device may also be configured.

FIG. 3 shows a side sectional view of the main parts of the reactor tube and trap container, which are different from those in the embodiment shown in FIG.

In the figure, the lower part of the reaction vessel 10 has a very gentle 1
It has a beveled portion and an opening 10' at its end. The neck 18 of the trap container 15 similarly has a very gentle slope upward, and the two are connected by rubbing together. 11 is a sample container suspended within the reaction container;
14 is an exhaust pipe, and 15' is a trap center of the trap container 15. 16ha heat pipe, trap center 1
It is inserted within 5'. In the above configuration,
The lower slope of the reaction vessel 10 is neither too narrow nor too wide, and is formed very gently.
There is no leakage in the gas flow path due to the collected material 29 collected in the trap center 15', the collection efficiency does not decrease, and the volatilized gas can be caused to flow down with reduced resistance.

(Effects of the Invention) As explained above, according to the present invention, a trap container having a trap center is connected to a reaction container of a thermogravimetric measuring device, a heat pipe is inserted into the trap center, and the cooling temperature of the heat pipe is By controlling arbitrarily, it is possible to select and collect a high-boiling point volatile product gas in the trap center, and also to select a low-boiling point volatile product gas. Precise thermogravimetry can be performed without causing condensation of volatile gases in the gas passage that connects the exhaust pipe and the gas analyzer, thereby not interfering with the passage. Volatile gas can be easily trapped without using it.

[Brief explanation of drawings]

Fig. 1 is a side cross-sectional view of an embodiment of the vaporized product gas trap device for a thermogravimetric measuring device of the present invention, and Fig. 2 is a causal diagram when the collected material is collected in the trap center of the trap container. and FIG. 8 shows a side sectional view of an embodiment of the piece shown in FIG. In the figure, 1 is a tube body, 2 is an arm, 3 is a support part of a hanging type thermogravimetric measuring device, 4 is a sample container support, 5 is a packing, and 6
is the opening of the tube body ■, 7 is the carrier gas injection hole, 8 is the connecting pipe, 9 is the carrier gas guide part, 10 is the reaction vessel, lO'
is the opening of the reaction vessel 10, 15 is the trap vessel, 15' is the opening of the trap vessel, 16 is the heat pipe, 17 is the heat insulating material, 1 is the cooling part shrine, 9 is the heating furnace, 20 and 25 are the thermocouples, 23 is a temperature controller for the heating furnace 19, 27 is a reaction vessel (Fig. 1, Fig. 2).

Claims (4)

[Claims] (1) A trap container that surrounds the opening of the reaction container of a thermogravimetric measuring device and can be connected to the reaction container, and has an exhaust pipe on its side wall and a trap container that protrudes upward from the center of its bottom surface and extends below the reaction container. a trap center inserted through an opening provided in the trap center, a heat pipe inserted into the trap center, and a cooling device connected to the heat pipe and capable of arbitrarily adjusting the cooling temperature. ,
The cooling temperature of the trap center is such that the wall temperature of the trap container is also low, and the exhaust pipe of the trap container is installed at a higher position than the location of the opening provided below the reaction container. A vaporization gas trap device for a thermoelectric precision foot measuring device, characterized by: (2) A trap container having a part that has a slight inclination angle from the lower part of the reaction container to the opening provided at the lower end thereof, and a part that is connected to the part having the above-mentioned small inclination angle. A volatilization product gas trap device for a thermogravimetry measuring device according to claim 1, characterized in that the device comprises: (3) The lower part of the reaction container including the opening is bent by 90 degrees, the trap center protrudes horizontally from the side of the trap container, and the trap center is deeply inserted into the opening. A volatilization product gas trap device for a thermogravimetric measuring device according to claim 1. (4) The volatilization product gas trap device for a thermogravimetric measuring device according to claim 1, wherein the trap container is transparent.