JP2013205298A - Device and method for filling raw material for standard gas - Google Patents

Abstract

PROBLEM TO BE SOLVED: To efficiently fill a container with a raw material of component gas contained in standard gas.SOLUTION: A filling device 1 for filling a container 10 with a raw material of component gas contained in standard gas includes a filling flow passage 2 and temperature alternation means 3. The filling flow passage 2 includes: a connection unit 23 to be connected to a container vale 12 arranged in an inflow outlet 11 of the container 10; and an injection unit 24 to which a raw material is injected. A raw material vaporized by heating is introduced into the container 10 through the connection unit 23. The temperature alternation means 3 lowers temperature of the filling flow passage 2 from the injection unit 24 to the connection unit 23.

Description

  The present invention relates to a filling device for filling a container with a raw material for standard gas, and a filling method thereof.

  In recent years, various harmful substances have been detected in the atmosphere, and there are concerns about the effects on health caused by the long-term exposure of the human body to the atmosphere containing the harmful substances. Therefore, it is necessary to periodically measure the concentration of harmful substances in the atmosphere and monitor the concentration so as not to exceed a predetermined level.

  Such harmful substances are measured by an analytical instrument that measures the concentration of each component, and high analysis accuracy (reliability) is required. In order to ensure high analytical accuracy, it is necessary to calibrate the analytical equipment periodically. For this calibration, a standard gas prepared to contain harmful components at a "predetermined concentration" is used. . In other words, the concentration of the harmful component contained in the prepared standard gas is measured by an analytical instrument, and the measured value of the analytical instrument is adjusted so that the measured value matches the “predetermined concentration” of the harmful component contained in the standard gas. Calibration is performed.

Therefore, the standard gas used in this way needs to be prepared with the concentration of harmful components as set values.
As a standard gas preparation method, when the target component is gaseous at room temperature, it is possible to adjust the set value with high accuracy by using a simple apparatus and flowing a dilution gas.

  For example, a gas regulator equipped with a mass flow controller consisting of a mass flow meter and a valve is proposed as a device that generates a gas with a predetermined concentration by diluting a component gas with a diluent gas when the target component is gaseous at room temperature. (For example, refer to Patent Document 1).

JP 61-116638 A

  Some standard gases contain high-boiling volatile organic compounds that are liquid or solid at room temperature, and in the case of such high-boiling components, they are injected into the filling pipe. A method of vaporizing by using a diluent gas as a carrier gas is conceivable, but it is liquefied or adsorbed by staying at the middle part of the pipe to the container or the container valve provided at the inlet / outlet of the container, May not reach inside of container. In this case, with respect to the concentration of the component gas, an error of several tens of percent may occur with respect to the set value (the “predetermined concentration”).

Therefore, in order to obtain a highly accurate standard gas, it is important to reduce as much as possible the raw materials that cannot reach the container when filling the container with the standard gas.
Then, an object of this invention is to provide the filling apparatus which can be filled with the raw material of the component gas contained in standard gas efficiently, and its filling method.

  (1) The present invention is a filling device for filling a container with a raw material of component gas contained in a standard gas, the connecting portion connected to a container valve provided at the inlet / outlet of the container, and the raw material A filling flow path for introducing the raw material injected from the injection part and heated and vaporized into the container through the connection part, and toward the connection part from the injection part. A temperature change means for lowering the temperature of the filling flow path, and the filling flow path is provided with a flow path main body from the connecting portion to the injection portion, and further extended from the flow passage main body. And a carrier gas flow path section for flowing the gas toward the injection section.

  According to the present invention, by reducing the temperature of the filling channel from the injection part toward the connection part, the raw material injected into the injection part can naturally flow toward the connection part. It is possible to suppress liquefaction or adsorption in the container, and efficiently guide the raw material into the container through the connection portion and the container valve to fill the container.

  Furthermore, since the filling flow path of the present invention has a carrier gas flow path section for allowing the carrier gas to flow toward the injection section, the vaporized raw material is injected with the carrier gas and injected. It is possible to flow from the portion toward the connecting portion, and it becomes possible to fill the container with the raw material more reliably.

(2) Moreover, it is preferable that the said temperature change means has a heater which heats the said filling flow path, and makes the heating amount with respect to the said injection | pouring part side larger than the heating amount with respect to the said connection part side.
In this case, the temperature of the filling channel can be lowered from the injection part toward the connecting part by heating the filling channel with the heater.

(3) Further, the container valve is provided with a safety valve that is opened when the temperature is raised to the first temperature, and is capable of discharging the gas in the container. Is preferably a second temperature lower than the first temperature.
For example, even if the container and the gas in the container become too hot due to a fire and the container internal pressure becomes excessively high, if the container valve is provided with a safety valve that discharges the gas before the container breaks, the function of the safety valve It is possible to fill the container with the raw material without impairing.

(4) Further, in the filling device, the temperature changing means is configured such that the temperature of the region on the injection portion side in the carrier gas flow path portion is the same as the temperature of the injection portion or the temperature of the injection portion. It is preferable to increase the height.
In this case, even if the carrier gas is not flowing, it is possible to prevent the raw material injected into the injection part from flowing in the direction opposite to the container side (the direction toward the carrier gas flow path side). .

(5) Moreover, it is preferable that the temperature of the said injection | pouring part is set to 50-105 degreeC by the said temperature change means, and the temperature difference of the said injection | pouring part and the said connection part shall be 10-35 degreeC.
When the temperature of the injection part is less than 50 ° C., the raw material may be difficult to vaporize. When the temperature exceeds 105 ° C., the temperature of the connection part becomes high, and the safety valve is provided in the container valve. In addition, the safety valve may be open.
Further, if the temperature difference between the injection part and the connection part is less than 10 ° C., the action of the raw material naturally flowing toward the connection part may be weakened, and if this temperature difference exceeds 35 ° C., There is a possibility that the temperature of the connecting portion is lowered and the raw material is liquefied or adsorbed in the pipe.

(6) In addition, the present invention is directed to the injection portion of the filling flow path connected to the container valve provided at the inlet / outlet of the container in order to fill the container with the raw material of the component gas contained in the standard gas. A filling method of injecting the raw material and guiding the injected raw material into the container through the container valve in a vaporized state, wherein the temperature of the filling channel is changed from the injection portion toward the container valve. The raw material is injected into the filling flow path after being lowered.
According to the present invention, since the raw material is injected into the filling flow path after the temperature of the filling flow path is lowered from the injection portion toward the container valve, the injected raw material naturally moves toward the container valve. The raw material can be efficiently led into the container through the container valve and filled into the container.

  According to the present invention, it is possible to efficiently guide the component gas material contained in the standard gas into the container and fill the container.

It is a schematic block diagram which shows one Embodiment of the filling apparatus of the raw material for standard gas. It is a table | surface which shows the result of having measured the density | concentration of the gas with which the container was filled.

Hereinafter, embodiments of the present invention will be described with reference to the drawings.
FIG. 1 is a schematic configuration diagram illustrating one embodiment of a standard gas raw material filling apparatus. The standard gas raw material filling device 1 (hereinafter referred to as a filling device 1) is equipment for filling a container 10 with a component gas raw material (mixed raw material M described below) contained in a standard gas.

The standard gas is a gas that is adjusted to have the same components as the atmosphere containing harmful substances, and is used for analytical instruments (not shown) that measure the concentration of harmful substances contained in the actual atmosphere. . In other words, the standard gas contains multiple types of component gases that have the same components as harmful substances contained in the atmosphere, and each component gas is prepared by a mass ratio mixing method so that it has a predetermined concentration. Has been.
In order to enclose such a standard gas in the container 10, the mixed material M containing a plurality of types of component gas raw materials (reagents that become component gases) contained in the standard gas is filled into the container by the filling device 1 of the present invention. 10 is filled.

In the present embodiment, a raw material having a high boiling point is included as a raw material for the component gas contained in the standard gas. For example, a volatile organic compound having a boiling point of 150 to 220 ° C. at normal pressure is included.
Such a high-boiling-point raw material has a low vapor pressure, and the amount that can be filled in the container 10 generally used for filling a standard gas is several hundred μg to several tens of grams with respect to the container 10 having a capacity of 10 liters. It is about mg.

  The container 10 will be described. A container valve 12 is provided at an inflow / outlet port 11 that is an opening of the container 10. The container valve 12 is attached to the inlet / outlet port 11 in order to prevent gas flow between the container 10 (the container internal space) and the outside (atmosphere). The container valve 12 is provided with a safety valve 13 in addition to the connection port 14 for taking out the standard gas stored in the container 10 and filling the raw material of the component gas.

  The safety valve 13 can be opened when the temperature is raised to a predetermined temperature (first temperature T1), and the gas in the container 10 can be discharged. Specifically, the safety valve 13 is made of a member (alloy) that melts when the temperature is raised to a first temperature (for example, 105 ° C.). The container valve 12 is provided with a through hole (not shown) that allows the inside of the container 10 to communicate with the outside. The through hole is covered with the member to be dissolved. That is, the safety valve 13 is composed of a fusible stopper that melts at a predetermined temperature. Thus, since the safety valve 13 is provided in the container valve 12, even if the gas in the container 10 and the container 10 becomes high temperature due to a fire and the internal pressure of the container 10 becomes excessively high, the container 10 is damaged. The gas can be discharged to the outside before it is done.

  The filling device 1 includes a filling pipe 22 connected to the container 10 (container valve 12). A filling flow path 2 is formed in the filling pipe 22. The filling pipe 22 according to the present embodiment has a first pipe 25 and a second pipe 26 made of straight pipes, and a first valve 27 is interposed between the first pipe 25 and the second pipe 26. doing. A connecting portion 23 connected to the container valve 12 is provided at one end of the first piping 25, and an injection portion 24 for injecting the mixed raw material M is provided in the middle of the first piping 25. A microsyringe 9 containing the mixed raw material M is connected to the injection part 24.

A second valve 28 is connected to the second pipe 26, and a carrier gas C supply pipe 29 is connected to the second valve 28 as a dilution gas. The carrier gas C can be nitrogen gas or helium gas. The carrier gas C supplied to the supply pipe 29 flows from the second pipe 26 to the first pipe 25 and accompanies the mixed raw material M supplied from the injection part 24 to the filling flow path 2 to store the mixed raw material M in a container. 10 to the inside.
Accordingly, in FIG. 1, the supply pipe 29 on the side to which the carrier gas C is supplied is the upstream side in the flow direction of the gas (vaporized mixed raw material M), and the connection portion 23 is the downstream side in the flow direction. The second pipe 26 has a branch portion, and a pump (suction pump) 35 for discharging the air in the filling pipe 22 is connected to the branch pipe 26a.

  In the filling flow path 2 (filling pipe 22) according to the present embodiment, the flow path main body 4 is provided from the connection portion 23 to the injection portion 24, and the flow passage main body 4 is further extended upstream. This portion is used as a carrier gas flow path section 5. That is, the carrier gas flow path section 5 is closer to the supply pipe 29 than the injection section 24. Further, as will be described later, when the mixed raw material M is filled in the container 10, the air in the container 10 and the filling flow path 2 is discharged to the outside by the pump 35, and the container 10 and the filling flow path 2 are decompressed. It is in a state (almost vacuum state).

  The filling device 1 further includes a temperature changing means 3 that lowers the temperature of the filling channel 2 from the injection part 24 toward the connection part 23. The temperature changing means 3 according to the present embodiment has a heater for heating the filling pipe 22 (filling flow path 2). Although various types of heaters can be employed as the heater, in the present embodiment, the heater includes a mantle heater 30 (hereinafter simply referred to as the heater 30). The heater 30 has a coiled heating wire (nichrome wire) and a heat insulating material (heat insulating material) that covers the heating wire. In FIG. 1, the outer contour line of the heater 30 (heat insulating material) is indicated by a two-dot chain line.

  The density of the heating wire (coil) that the heater 30 has is not uniform along the longitudinal direction of the filling flow path 2, and the heating amount on the injection portion 24 side is larger than the heating amount on the connection portion 23 side. As described above, the heating wires are arranged as an unequal distribution. Specifically, the number of heating wire turns of the heater 30 is gradually reduced from the injection part 24 toward the connection part 23. Thereby, the temperature of the injection part 24 can be made higher than the temperature of the connection part 23, and the temperature can be gradually lowered (in a straight line) from the injection part 24 toward the connection part 23. .

The temperature changing means 3 further includes a controller 31 that controls the output of the heater 30 and a sensor (thermocouple) 32 that detects the temperature (surface temperature) of the filling pipe 22. When the detection signal of the sensor 32 is input to the controller 31, the controller 31 adjusts the output of the heater 30 so that the temperature at the temperature detection point by the sensor 32 becomes the set temperature.
In the present embodiment, as shown in FIG. 1, the heater 30 only covers the flow path main body 4 between the connection portion 23 and the injection portion 24 and heats the flow path main body 4. The container valve 12 is also covered, and the container valve 12 is also heated. Furthermore, the heater 30 covers a part of the carrier gas flow path part 5 on the injection part 24 side, that is, a region from the injection part 24 to the first valve 27, and this part is also heated. Yes.

  According to the filling pipe 22 having the above configuration, the mixed raw material M injected into the injection section 24 with the connection section 23 of the filling pipe 22 connected to the connection port 14 of the container valve 12 has a low internal pressure. When heated by the heater 30 in the (substantially vacuum) filling pipe 22, it becomes vaporized and can be moved into the container 10. That is, according to the filling flow path 2 and the temperature changing means 3 according to this embodiment, the mixed raw material M injected and vaporized from the injection part 24 can be guided into the container 10 through the connection part 23 and the container valve 12. .

A filling method for filling the container 10 with the mixed raw material M by the filling apparatus 1 having the above configuration will be described.
The container 10 is sealed by a container valve 12, and the inside of the container 10 is previously depressurized to a predetermined internal pressure. And the filling piping 22 is connected to the container valve 12 (connection port 14) of the container 10 like the structure shown in FIG. In the state where the filling pipe 22 is connected to the container valve 12, air is present inside the first pipe 25 and the second pipe 26, so this air is supplied by the pump 35 connected to the second pipe 26. Drain and make the inside vacuum (substantially vacuum). At this time, the second valve 28 is closed. Then, the connection port 14 of the container valve 12 is opened.

Further, the filling pipe 22 is heated by the heater 30, and the temperature of the filling pipe 22 (filling flow path 2) is gradually (linearly) lowered from the injection section 24 toward the connection section 23. To do. The temperature difference between the injection part 24 and the connection part 23 is preferably 10 to 35 ° C., more preferably 15 to 30 ° C. And it is preferable to set the temperature of the injection | pouring part 24 to 50-105 degreeC, and it is more preferable to set to 60-95 degreeC.
For example, when the temperature of the injection part 24 is 60 ° C., the temperature of the connection part 23 is 30 to 45 ° C., and when the temperature of the injection part 24 is 95 ° C., the temperature of the connection part 23 is 65 to 80 ° C. . The temperature of each part is kept constant by the controller 31.
If the temperature of the injection part 24 is less than 50 ° C., the mixed raw material M may be difficult to vaporize, and if it exceeds 105 ° C., the temperature of the connection part 23 becomes high and the safety valve 13 may be opened. There is.
In addition, when the temperature difference between the injection part 24 and the connection part 23 is less than 10 ° C., the action of the mixed raw material M naturally flowing toward the connection part 23 may be weakened. If it exceeds ° C., the temperature of the connecting portion 23 is lowered, and the mixed raw material M may be liquefied or adsorbed in the pipe.

  In this state, the syringe 9 from which a certain amount of the mixed raw material M has been collected is connected to the injection portion 24 of the filling pipe 22, and this syringe 9 is operated to fill the mixed raw material M in the syringe 9 through the injection portion 24. Inject into the channel 1. Then, the filling pipe 22 guides the mixed raw material M into the container 10 through the container valve 12 in a vaporized (gasified) state, and fills the container 10 with the mixed raw material M. Since the injection of the mixed raw material M into the filling flow path 2 is performed in a state where the temperature of the filling pipe 22 is lowered from the injection portion 24 toward the connection portion 23, the injected mixed raw material M is a container valve. It can flow naturally toward 12 and can reach into the container 10.

  In the present embodiment, after the mixed raw material M in the syringe 9 is injected into the filling pipe 22 through the injection portion 24, the second valve 28 is opened after a predetermined time has elapsed (several minutes later), and the carrier gas C is supplied from the supply pipe 29, and the vaporized mixed raw material M is filled in the container 10 along with the gas flow of the carrier gas C. Note that when the flow rate of the carrier gas C is increased, the carrier gas C may take heat from the vaporized mixed raw material M and the filling pipe 22 to promote reliquefaction of the mixed raw material M in some cases. For this reason, the supply flow rate of the carrier gas C is preferably about 20 to 100 milliliters per minute.

  Moreover, in this embodiment, the temperature of the connection part 23 is lower than the 1st temperature T1 (for example, 105 degreeC) by which the safety valve 13 provided in the container valve 12 will be in the open state by the temperature changing means 3. The temperature is adjusted to be the temperature T2. In particular, in this embodiment, the heater 30 is heating not only the connection part 23 but the container valve 12, and makes the temperature of the container valve 12 the same as the temperature of the connection part 23 (second temperature T2). As described above, the temperature of the connecting portion 23 is in the range of 30 to 45 ° C. or 65 to 80 ° C. Since this temperature is lower than the first temperature T1 (105 ° C.), the safety valve 13 is opened. There is no.

  Furthermore, in the present embodiment, the temperature changing means 3 causes at least the region on the injection portion 24 side of the carrier gas flow path portion 5, that is, the first piping 25 to the first valve 27 from the injection portion 24 to the first valve 27. The temperature is adjusted so that the temperature of the portion is the same as the temperature of the injection portion 24 or slightly higher than the temperature of the injection portion 24. This prevents the mixed raw material M injected into the injection section 24 from flowing in the direction opposite to the container 10 side, that is, the carrier gas flow path section 5 side, even in a time zone when the carrier gas C is not flowing. It becomes possible.

  Then, after a predetermined time has elapsed from the start of the injection of the mixed raw material M (for example, one hour later), the connection port 14 of the container valve 12 is closed, and the filling of the mixed raw material M into the container 10 is finished.

〔Example〕
An embodiment of a method of filling the mixed raw material M into the container 10 by the filling apparatus 1 having the above configuration will be described. In the following, Comparative Examples 1 and 2 will be described in addition to Examples 1 and 2. In each of Examples 1 and 2 and Comparative Examples 1 and 2, a heater heating wire is wound around the filling pipe 22, the temperature of a predetermined portion of the filling pipe 22 is measured by a sensor (thermocouple), and the controller 31 fills Although the temperature control of the pipe 22 is performed, the comparative examples 1 and 2 are compared with the first and second embodiments in the configuration of the heating wire of the heater 30 and the heating condition (heating temperature) of the filling pipe 22 by the heater 30. ) Is different.

  Here, the mixed raw material M used in Examples 1 and 2 and Comparative Examples 1 and 2 will be described. As volatile hydrocarbon substances having a relatively high boiling point (150 to 220 ° C), decane (boiling point 174 ° C), 1,2,3-trimethylbenzene (boiling point 175 ° C), m-diethylbenzene (boiling point 182 ° C), p- Diethylbenzene (boiling point 184 ° C.), undecane (boiling point 195 ° C.), dodecane (boiling point 216 ° C.) are each collected in 0.003 mol, and these are mixed in a glass bottle (vial bottle) having a volume of 10 ml. Yes. Further, for the concentration analysis of each component, 0.003 mol of hexane having a low boiling point (boiling point 63.8 ° C.) is added to the mixed raw material M as an index material for comparison. And this mixed raw material M is extract | collected to the micro syringe 9 about a fixed quantity.

  As shown in FIG. 1, the filling pipe 22 is connected to the container valve 12 of the container 10. The capacity | capacitance of the container 10 is 10 liters, it is sealed by the container valve 12, and is pressure-reduced to 13 Pa or less beforehand. In addition, after the connection to the container valve 12, the air present in the filling pipe 22 is exhausted by the pump 35 to make a vacuum (substantially vacuum). Then, the connection port 14 of the container valve 12 is opened.

  The filling pipe 22 is heated with the configuration of the heating wire of the heater 30 and the heating condition (heating temperature) of the filling pipe 22 by the heater 30 as the following Examples 1 and 2 and Comparative Examples 1 and 2, respectively. One hour after the temperature of each part of the filling pipe 22 reaches the set temperature, filling of the mixed raw material M in the microsyringe 9 is started.

  Further, 5 minutes after the start of filling, nitrogen gas is introduced as the carrier gas C from the supply pipe 29, and the mixed raw material M vaporized is filled in the container 10 along with the nitrogen stream. The supply flow rate of the carrier gas C is 100 milliliters per minute.

  One hour after the start of injection, the connection port 14 of the container valve 12 is closed, and the filling of the mixed stock solution M is completed. After this filling, the container 10 was filled with nitrogen gas for dilution, and the total amount of standard gas in the container was 20 mol (the internal pressure of the container 10 was 5 MPa). The injection amount of the mixed stock solution M is set so that the concentration of each component in the gas is about 500 ppb.

And about each of Examples 1, 2 and Comparative Examples 1, 2, the density | concentration of each component gas contained in the gas (standard gas) with which the container 10 was filled is measured.
The concentration is measured using gas chromatography (manufactured by Shimadzu Corporation, model number: GC14B-FID, column: NB-1 (manufactured by GL Sciences, inner diameter 0.25 mm × length 60 m), carrier gas: helium). I went. The analysis is evaluated by comparing the response value of hexane and the response value of each component gas.

[Example 1]
The number of turns of the heating wire of the heater 30 is gradually reduced in the direction from the injection part 24 to the connection part 23 of the filling pipe 22, and the temperature of the filling pipe 22 is gradually lowered toward the container valve 12. . When the temperature of the injection part 24 was set to 80 ° C., the temperature of the container valve 12 became 65 ° C.
Under this condition, with the filling pipe 22 heated, the mixed raw material M was filled in the container 10 and the concentration analysis of the gas (standard gas) filled in the container 10 was performed. The result is shown in FIG. The analysis result of dodecane having the highest boiling point is within ± 3%, and according to the temperature setting of the filling pipe 22 according to Example 1, a satisfactory filling result was obtained. Further, the concentrations of components other than dodecane are also shown in FIG. 2, and good filling results were obtained.

In addition, the numerical value of the concentration in FIG. 2 is a relative sensitivity with respect to hexane. That is, the component gas filled in the container 10 is analyzed, the relative sensitivity of each component gas to hexane is obtained, and evaluation is performed using a deviation generated between them. The deviation is defined by the following equation.

[Example 2]
As in the first embodiment, the number of turns of the heating wire of the heater 30 is gradually reduced in the direction from the injection part 24 to the connection part 23 of the filling pipe 22, and the temperature of the filling pipe 22 gradually increases toward the container valve 12. It was configured to decrease. When the temperature of the injection part 24 was set to 70 ° C., the temperature of the container valve 12 became 50 ° C.
Under this condition, with the filling pipe 22 heated, the mixed raw material M was filled in the container 10 and the concentration analysis of the gas (standard gas) filled in the container 10 was performed. As a result of the analysis (see FIG. 2), the concentration of dodecane was within ± 3%, and according to the temperature setting of the filling pipe 22 according to Example 2, a good filling result was obtained.

[Comparative Example 1]
Unlike the first and second embodiments, the number of turns of the heating wire of the heater 30 is gradually increased in the direction from the injection part 24 to the connection part 23 of the filling pipe 22, and the temperature of the filling pipe 22 is increased toward the container valve 12. Was configured to gradually increase. When the temperature of the container valve 12 was set to 80 ° C., the temperature of the injection part 24 became 52 ° C.
Under this condition, with the filling pipe 22 heated, the mixed raw material M was filled in the container 10 and the concentration analysis of the gas (standard gas) filled in the container 10 was performed. As a result of the analysis (see FIG. 2), the concentration of dodecane was -13% as compared with the case of normal filling, and the filling result was not preferable.

[Comparative Example 2]
The number of turns of the heating wire of the heater 30 was made uniform from the injection part 24 to the connection part 23 of the filling pipe 22 so that the temperature gradient in the filling pipe 22 disappeared. The temperature of the injection part 24 was set to 80 ° C.
Under this condition, with the filling pipe 22 heated, the mixed raw material M was filled in the container 10 and the concentration analysis of the gas (standard gas) filled in the container 10 was performed.
As a result of the analysis (see FIG. 2), the concentration of dodecane was −8% compared to the case of normal filling, and the filling result was not preferable.

  According to the above-described filling apparatus 1 according to the present embodiment, the vaporized mixed raw material M is injected into the filling pipe 22 in a state where the temperature of the filling pipe 22 is lowered from the injection section 24 toward the connection section 23. Therefore, the injected mixed raw material M can naturally flow toward the connecting portion 23. For this reason, it becomes possible to efficiently guide the mixed raw material M into the container 10 through the connection portion 23 and the container valve 12 to fill the container.

Further, in the filling pipe 22 according to the present embodiment, a carrier gas channel portion 5 is provided so as to extend further from the channel main body portion 4 from the connection portion 23 to the injection portion 24. According to the carrier gas flow path section 5, the carrier gas C can be flowed toward the injection section 24, and the mixed raw material M in a vaporized state is entrained with the carrier gas C from the injection section 24. It can be made to flow toward the connection part 23, and it becomes possible to fill the container 10 with the mixed raw material M more reliably.
In particular, when the mixed raw material M contains a high-boiling-point raw material that is difficult to move into the container 10 only by the vapor pressure of the component gas itself, the mixed raw material M is vaporized, and the gas flow of the carrier gas C By being accompanied and moved into the container 10, reliable filling becomes possible.

  In addition, the filling device 1 of the present invention is not limited to the illustrated form, and may be of another form within the scope of the present invention. For example, according to the temperature changing means 3 of the above-described embodiment, the temperature of the filling pipe 22 gradually decreases (in a straight line) from the injection part 24 toward the connection part 23. It may be changed. In this case, what is necessary is just to change the winding number of the heating wire of the heater 30 in steps.

  1: Standard gas raw material filling device 2: Filling flow path 3: Temperature change means 4: Flow path body part 5: Flow path part for carrier gas 10: Container 11: Inlet / outlet 12: Container valve 13: Safety valve 23: Connection Part 24: Injection part 30: Heater (heater) M: Mixed raw material (raw material)

Claims (6)

A filling apparatus for filling a container with a raw material of component gas contained in a standard gas,
A connecting portion connected to a container valve provided at an inlet / outlet of the container and an injecting portion into which the raw material is injected; the raw material injected from the injecting portion and heated and vaporized through the connecting portion; A filling channel leading into the container;
Temperature changing means for lowering the temperature of the filling channel from the injection part toward the connection part;
With
The filling channel includes a channel main body from the connection unit to the injection unit, and a carrier gas channel that extends further from the channel main unit and allows a carrier gas to flow toward the injection unit. And a standard gas raw material filling apparatus.   2. The filling of the standard gas raw material according to claim 1, wherein the temperature changing unit includes a heater for heating the filling flow path, and the heating amount for the injection portion side is larger than the heating amount for the connection portion side. apparatus. The container valve is provided with a safety valve that is opened when the temperature is raised to the first temperature and can discharge the gas in the container.
3. The standard gas raw material filling apparatus according to claim 1, wherein the temperature changing means sets the temperature of the connecting portion to a second temperature lower than the first temperature.   The temperature changing means makes the temperature of the region on the injection portion side of the carrier gas channel portion the same as or higher than the temperature of the injection portion. The standard gas raw material filling apparatus according to claim 1.   The temperature of the said injection | pouring part is set to 50-105 degreeC by the said temperature change means, and the temperature difference of the said injection | pouring part and the said connection part is 10-35 degreeC, It is any one of Claims 1-4. Standard gas raw material filling equipment. In order to fill the container with the raw material of the component gas contained in the standard gas,
Injecting the raw material to the injection part of the filling flow path connected to the container valve provided at the inlet / outlet of the container,
A filling method for introducing the injected raw material into the container through the container valve in a vaporized state,
A standard gas raw material filling method, wherein the raw material is injected into the filling flow path after the temperature of the filling flow path is lowered from the injection portion toward the container valve.

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