JP2024037235A - Mixed gas manufacturing device and mixed gas manufacturing method - Google Patents

Abstract

To provide a mixed gas manufacturing device capable of manufacturing mixed gas controlled so that water concentration included in the mixed gas is controlled to target moisture concentration.SOLUTION: A mixed gas manufacturing device 10 includes: a source gas generation part Y0 which prepares mixed gas in which concentration of a target compound is higher than target concentration; a humidified gas supply part X0 supplying humidified gas; and a mixed gas dilution part W0 which dilutes first mixed gas in higher target compound concentration than the target concentration with the humidified gas. The humidified gas supply part X0 is provided with: humidifying means 120 which is provided with temperature control means CTWB controlling temperatures of a humidifier container HB for humidifying the dilution gas and water housed in the humidifier container HB and first pressure control means BPC controlling pressure in the humidifier container HB; and second flow rate control means MFC2 controlling flow rate of dilution gas to be supplied for the humidifying means 120. The mixed gas dilution part W0 is provided with first flow rate control means MFC1 controlling flow rate of the first mixed gas.SELECTED DRAWING: Figure 1

Description

Application for application of Article 30, Paragraph 2 of the Patent Act has been filed. - Published on September 8, 2021 in the lecture proceedings of the 70th Annual Meeting of the Japanese Society of Analytical Chemistry.・On September 23, 2021, a conference presentation was made at the 70th annual meeting of the Japanese Society of Analytical Chemistry.・Published on November 29, 2021 in the lecture proceedings of Pacifichem 2021.・On December 20, 2021, an academic conference presentation was made at Pacifichem 2021.・Published on May 2, 2020 in the lecture proceedings of the 82nd Analytical Chemistry Symposium.・On May 15, 2020, an academic presentation was made at the 82nd Analytical Chemistry Symposium.

The present invention relates to a mixed gas production device and a mixed gas production method.

Gases emitted from living organisms contain a variety of volatile organic compounds (hereinafter referred to as "VOCs"), and these VOCs can be used in various ways as test substances (biomarkers) for diseases. Research is being conducted. Although the concentration of the test substance contained in the biological gas is often a very small amount of several nmoles/mol or less, the biological gas contains an order of magnitude larger amount of water than the test substance. When measuring the concentration of VOC contained in biological gas using a measurement device such as a GC/MS or a VOC sensor, water is a typical interfering component and affects the detection section of the device by causing interference. In addition, VOCs other than the test substance also have an effect such as interference on the detection section of the device as interfering components. For this reason, it is preferable to calibrate the measuring instrument using a standard gas that contains the same components as the biological gas and whose concentration is close to that of the biological gas.

On the other hand, standard gases that contain components similar to biological gases contain a large amount of water, which condenses when pressurized, so they cannot be supplied by filling them into high-pressure containers, or so-called cylinders. . When supplying standard gas by filling it into a high-pressure container, only dry standard gas containing almost no water can be supplied.

When a standard gas containing water is required, it is prepared at the time of use using a mixed gas generator, but in this conventional mixed gas generator, diluent gas is bubbled through heated water. humidification was performed.

Martin Leidinger et al, Meas. Sci. Tecnol., 29, 015901 (2018) The above non-patent document describes that a gas containing a target compound and a diluent gas are mixed using a mass flow controller to produce a mixed gas. A mixed gas production device is described. The above non-patent document states that a portion of the carrier gas can be humidified by passing the diluent gas through a constant temperature bath (washing bottle) whose temperature is controlled to be slightly lower than room temperature. .

However, in the mixed gas production apparatus of the prior art, it has not been possible to increase the concentration of water contained in the mixed gas to a high water concentration target concentration such as 100 percent relative humidity. In other words, in conventional technology, humidification is performed by bubbling carrier gas into water whose temperature is controlled, but when the target moisture concentration is high, this method It was not possible to control the concentration to the target concentration. Therefore, when the target concentration is high, there is a problem in that it is not possible to obtain a mixed gas in which the concentration of water contained in the mixed gas is increased to the target concentration. Another problem is that when the flow rate of the carrier gas is changed, the concentration of water contained in the humidifying gas changes even if the temperature of the heated water is constant. Further, there was a problem in that the flow rate of the diluent gas after humidification could not be determined accurately. That is, there was a problem in that it was not possible to accurately determine the concentration of VOC and the concentration of water contained in the mixed gas generated by the mixed gas production apparatus of the prior art.

The present invention has been made in view of the above-mentioned circumstances, and is a method for producing a mixed gas that is capable of producing a mixed gas accurately adjusted to a target moisture concentration even when producing a mixed gas with a high moisture concentration. To provide an apparatus, or to provide a method for producing a mixed gas that can produce a mixed gas accurately adjusted to a target moisture concentration even when producing a mixed gas with a high moisture concentration; An object of the present invention is to provide a method for producing a mixed gas that can produce a mixed gas accurately adjusted to a target VOC concentration even when producing a mixed gas with a high moisture concentration.

[1] The mixed gas production device of the present invention includes a source gas generation unit that prepares a mixed gas containing a target compound and in which the concentration of the target compound is higher than the target concentration, and a humidifying gas that humidifies the mixed gas. A mixed gas production device comprising: a humidified gas supply unit; and a mixed gas dilution unit that dilutes a first mixed gas having a first concentration higher than a target concentration with the humidified gas. The humidifying gas supply unit includes a humidifying container for humidifying the diluent gas, a temperature control means for controlling the temperature of water contained in the humidifying container, and a first pressure controlling the pressure inside the humidifying container. and a second flow rate control means for controlling the flow rate of the diluent gas supplied to the humidification means, and the mixed gas diluting section controls the flow rate of the first mixed gas. The present invention is characterized by comprising a first flow rate control means for controlling the flow rate.

[2] In the mixed gas production apparatus of the present invention, it is preferable that the second flow rate control means is arranged upstream of the humidification means.

[3] In the mixed gas production apparatus of the present invention, it is preferable that the humidified gas supply section further includes a moisture content measuring means for measuring the moisture content contained in the humidified gas.

[4] The mixed gas production apparatus of the present invention includes a pre-dilution section that supplies the diluent gas that dilutes the second mixed gas in which the target compound has a second concentration higher than the first concentration. Preferably, the preliminary dilution section includes a third flow rate control means for controlling the flow rate of the dilution gas.

[5] In the mixed gas production apparatus of the present invention, it is preferable that the first flow rate control means and the second flow rate control means are mass flow controllers.

[6] In the mixed gas production apparatus of the present invention, it is preferable that the humidifying container includes a first humidifying container and a second humidifying container.

[7] In the mixed gas production apparatus of the present invention, it is preferable that the source gas generation section includes a diffusion tube containing the target compound in a solid or liquid phase, and a second pressure control means. .

[8] In the mixed gas production apparatus of the present invention, it is preferable that the source gas generation section includes a high-pressure container containing a gas containing the target compound.

[9] In the mixed gas production apparatus of the present invention, it is preferable that the source gas generation section includes a permeation tube containing the target compound in a solid phase, liquid phase, or gas phase.

[10] In the method for producing a mixed gas of the present invention, the first mixed gas in which the concentration of the target compound is the first concentration is supplied by controlling the flow rate per unit time to the first flow rate. a gas supply step; a humidification gas supply step in which a humidified gas obtained by humidifying a dilution gas is supplied while controlling a flow rate per unit time to a second flow rate based on the supply amount of the dilution gas before humidification; a mixing step of mixing the first mixed gas supplied in the first mixed gas supply step and the humidifying gas supplied in the humidifying gas supplying step, the humidifying gas supplying step and a pressure-controlled humidifying container, wherein the diluting gas is humidified by bubbling the diluting gas within the humidifying container containing water.

[11] In the method for producing a mixed gas of the present invention, the humidifying gas supplying step measures the dew point and pressure of the humidifying gas, and calculates the moisture contained in the humidifying gas from the dew point and pressure obtained by the measurement. It is preferable to include a moisture amount calculation step of calculating the amount.

According to the mixed gas production apparatus of the present invention, even when producing a mixed gas with a high moisture concentration, it is possible to produce a mixed gas whose moisture concentration is accurately adjusted to a target moisture concentration. Further, according to the mixed gas production method of the present invention, even when producing a mixed gas with a high moisture concentration, it is possible to produce a mixed gas whose moisture concentration is accurately adjusted to a target moisture concentration. Furthermore, according to the mixed gas production method of the present invention, even when producing a mixed gas with a high moisture concentration, it is possible to produce a mixed gas whose concentration of VOC is accurately adjusted to the target.

1 is a diagram shown to explain the overall configuration of a mixed gas manufacturing apparatus 10 according to a first embodiment. FIG. FIG. 2 is a diagram shown to explain the overall configuration of a mixed gas production apparatus 20 according to a second embodiment. FIG. 3 is a diagram shown to explain the overall configuration of a mixed gas production apparatus 30 according to Embodiment 3. FIG. FIG. 4 is a diagram shown to explain the overall configuration of a mixed gas production apparatus 40 according to a fourth embodiment. It is a figure shown in order to explain the whole composition of mixed gas manufacturing device 50 concerning Embodiment 5. FIG. 7 is a diagram shown to explain a method for producing a mixed gas according to Embodiment 6. FIG. 3 is a diagram showing evaluation results when humidifying gas was produced in Example 1. FIG. 7(a) is a diagram showing changes in the pressure and temperature inside the humidifying container when the flow rate of the diluent gas supplied via the second flow rate control means MFC2 is changed. FIG. 7(b) is a diagram showing a change in the concentration of water in the diluent gas when the flow rate of the diluent gas supplied via the second flow rate control means MFC2 is changed. It is a figure for showing the evaluation result when humidifying gas was manufactured in a comparative example. FIG. 8(a) is a diagram showing changes in the pressure and temperature inside the humidifying container when the flow rate of the diluent gas supplied via the second flow rate control means MFC2 is changed. FIG. 8(b) is a diagram showing changes in the water concentration in the diluent gas when the flow rate of the diluent gas supplied via the second flow rate control means MFC2 is changed. FIG. 2 is a diagram showing an example of a chromatogram obtained by analyzing the acetone mixed gas produced in Example 2 using a gas chromatograph. FIG. 2 is a diagram showing the relationship between the prepared concentration of acetone (target concentration) and the peak area value analyzed by gas chromatography for the acetone mixed gas produced in Example 2 and the acetone mixed gas produced in Reference Example.

Hereinafter, a mode for carrying out the present invention (hereinafter referred to as "embodiment") will be described. The embodiments described below do not limit the claimed invention. Furthermore, not all of the elements and combinations thereof described in the embodiments are essential to the present invention. Furthermore, if the explanations overlap in each embodiment, the explanations may be omitted.

1. Mixed gas production device (Embodiment 1)
FIG. 1 is a diagram shown to explain the overall configuration of a mixed gas production apparatus 10 according to the first embodiment. Hereinafter, a mixed gas production apparatus 10 according to Embodiment 1 will be described using FIG. 1.

1-1. Overall Configuration As shown in FIG. 1, the mixed gas production apparatus 10 according to the first embodiment includes a source gas generation section Y0, a preliminary dilution section Z0, a mixed gas dilution section W0, and a humidified gas supply section X0. .

The source gas generating section Y0 is a section that generates a mixed gas containing the target compound. Here, the term "target compound" refers to a compound contained in the mixed gas that is to be diluted. For example, when the mixed gas is a standard gas for calibrating a measuring instrument, the target compound corresponds to a compound to be analyzed (for example, acetone). Moreover, "humidifying gas" refers to a gas in which water is added to diluted gas to increase the moisture concentration.

The concentration of the target compound contained in the mixed gas prepared in the source gas generating section Y0 is a second concentration higher than the target concentration.

The source gas generation section Y0 includes a flow path 101. The flow path 101 includes a diffusion tube DT as a source gas generation means 110, a second pressure control means APC, and a fifth flow rate control means MFC5. The flow rate of the diluent gas into the container containing the diffusion tube DT is controlled by the fifth flow rate control means MFC5, and a constant amount of the target compound is released from the diffusion tube DT per unit time, so that the mixed gas containing the target compound is controlled. occurs.

The flow path 101 is configured such that a valve 81 is provided between the second pressure control means APC and the diffusion tube DT, and gas flowing through the flow path 101 can be shut off.

The flow path 101 branches at a branch 53 between the fifth flow rate control means MFC5 and the fourth flow rate control means MFC4 of the preliminary dilution section Z0, which will be described later. At the branched end, an analytical instrument sample inlet AS1 for introducing a mixed gas into the analytical instrument and an exhaust valve 91 are provided.

Note that the installation location of the second pressure control means APC and the installation location of the fifth flow rate control means MFC5 may be exchanged. In this case, the second pressure control means APC is one that performs back pressure control.

The mixed gas dilution unit W0 is a part that prepares a mixed gas. Specifically, first, the source gas generation unit Y0 prepares a second mixed gas in which the concentration of the target compound is the second concentration. Next, by diluting the second mixed gas in the pre-dilution section Z0, a first mixed gas in which the concentration of the target compound is the first concentration is prepared. Furthermore, the first mixed gas is diluted with the humidifying gas supplied from the humidifying gas supply section X0 to prepare a humidified mixed gas in which the concentration of the target compound is adjusted to the target concentration.

The preliminary dilution section Z0 is a section that dilutes the second mixed gas in which the concentration of the target compound is the second concentration to prepare a mixed gas in which the concentration of the target compound is the first concentration. The second mixed gas containing the target compound at the second concentration is supplied from the source gas generation section Y0. The second mixed gas is diluted with the diluent gas of the diluent gas introduction section to prepare a mixed gas having the first concentration of the target compound.

The preliminary dilution section Z0 includes two channels 102 and 103. The flow path 102 includes a fourth flow rate control means MFC4, and a merging portion 54 with the flow path 103 is provided on the downstream side of the fourth flow path control means MFC4 with respect to the direction in which the gas flows. In the flow path 103, a diluent gas introduction section 61 and a third flow rate control means MFC3 are arranged in order from the upstream side with respect to the direction in which the gas flows.

A source gas generation section Y0 is installed on the upstream side of the fourth flow rate control means MFC4 in the direction in which the gas flows. Each element from the source gas generation section Y0 to the confluence section 54 is connected by a flow path 102. Each element from the diluent gas introduction part 61 to the confluence part 54 with the flow path 102 is connected by a flow path 103 through which the dilution gas flows. Thereby, the second mixed gas flowing through the flow path 102 and the dilution gas flowing through the flow path 103 can be mixed.

Further, the flow path 102 branches at a branch portion 55 between the confluence portion 54 and the first flow rate control means MFC1 of the mixed gas dilution portion W0. At the branched end, an analytical instrument sample inlet AS2 for introducing a mixed gas into the analytical instrument and an exhaust valve 92 are provided.

The flow path 103 is provided with a valve 82 between the third flow rate control means MFC3 and the merging portion 54, and is configured to be able to shut off gas flowing through the flow path 103.

Although the mixed gas production apparatus 10 according to the first embodiment has been shown as having one line of preliminary dilution section Z0, it may have two or more lines of preliminary dilution section Z0.

Further, it is not essential to have the preliminary dilution section Z0. When the concentration of the target compound contained in the mixed gas prepared by the source gas generation section Y0 is lower than the target concentration, the preliminary dilution section Z0 is It goes without saying that there is no problem even if you are not prepared. In this case, the first concentration, which is the concentration of the target compound in the second mixed gas, and the second concentration, which is the concentration of the target compound in the second mixed gas, are the same.

The mixed gas dilution section W0 includes two flow paths 104 and 106. The flow path 104 is provided with a first flow rate control means MFC1 and a merging portion 56 in this order from the upstream side in the direction in which the gas flows. The flow path 106 is connected to the humidifying gas supply section X0 on the upstream side with respect to the direction in which the gas flows, and is connected to the flow path 104 at the merging section 56. Thereby, the first mixed gas flowing through the channel 104 and the humidifying gas flowing through the channel 106 can be mixed.

The flow path 104 includes an analytical instrument sample introduction port AS3 downstream of the confluence section 56 for introducing the mixed gas into the analytical instrument. Further, the flow path 104 branches at a branching section 57 between the confluence section 56 and the analytical instrument sample inlet AS3, and is provided with an exhaust valve 93 at the branched end.

In the humidifying gas supply section X0, the diluent gas introducing section 71, the second flow rate control means MFC2, and the humidifying means 120 are arranged in order from the upstream side with respect to the direction in which the gas flows. The humidifying means 120 includes a humidifying container HB, a temperature controlling means CTWB, and a first pressure controlling means BPC. Each of the above-mentioned elements is connected by a flow path 105 through which dilution gas or humidification gas flows.

The flow path 105 branches at a branch portion 65 downstream of the first pressure control means BPC. A water content measuring means 130 for measuring the water content contained in the mixed gas is connected to the branched end. Further, a valve 86 is provided between the branch portion 65 of the flow path 105 and the moisture content measuring means 130.

A valve 83 is provided between the second flow rate control means MFC2 and the humidification means 120 in the flow path 105.

The flow path 105 may include a flow path 107 that bypasses the humidification means 120 so that the diluent gas can flow without passing through the humidification means 120. The flow path 105 is provided with valves 84 and 85, and the flow path 107 is provided with valves 87 and 88.

Below, each constituent element which constitutes mixed gas manufacturing device 10 concerning this embodiment is explained in detail.

In the following description, the first flow rate control means MFC1, the second flow rate control means MFC2, the third flow rate control means MFC3, the fourth flow rate control means MFC4, and the fifth flow rate control means MFC5 are collectively referred to as , may be written as "flow rate control means MFC". Further, the valves 81, 82, 83, 84, 85, 86, 87, and 88 may be collectively referred to as "valve 80." Furthermore, the flow paths 101, 102, 103, 104, 105, 106, and 107 may be collectively referred to as "flow path 100."

1-2. Source gas generation means A mixed gas containing the target compound is prepared by a diffusion tube method using a diffusion tube DT. Specifically, a volatile solid or liquid such as an organic solvent that is the target compound is placed in the diffusion tube DT, and the target compound is maintained at a constant temperature to fill the diffusion tube DT with vapor of the target compound. The vapor of the target compound is diffused in the thin tube of the diffusion tube DT, and the target compound is released from the diffusion tube DT at a constant rate. A diluent gas is sent there at a constant flow rate to continuously generate a gas containing the target compound at a constant concentration.

The second pressure control means APC has a function of controlling the gas pressure in the diffusion tube DT to be constant. The second pressure control means APC can be, for example, an automatic pressure controller. By controlling the gas pressure in the diffusion tube DT to be constant using the second pressure control means APC, it becomes possible to release the target compound from the diffusion tube DT at a constant rate.

Without the second pressure control means APC, when the flow rate of gas is changed in the flow rate control means MFC and the external atmospheric pressure fluctuates, the pressure of the gas in the diffusion tube DT will fluctuate. As a result, the gas in the diffusion tube DT expands or contracts, and accordingly, the vapor of the target compound is released from the diffusion tube DT, or the diluent gas flows into the diffusion tube DT, and the concentration of the gas increases or decreases. However, by providing the source gas generation means 110 with the second pressure control means APC, the pressure of the gas in the diffusion tube DT can be kept constant. As a result, it becomes possible to keep the concentration of the target compound constant in the second mixed gas supplied from the diffusion tube DT.

Regarding the diffusion tube DT according to the first embodiment, the reproducibility accuracy of the concentration of the target compound contained in the mixed gas was verified through experiments. Table 1 shows the production conditions of the mixed gas, and Table 2 shows the measurement results of the concentration of the target compound contained in the produced mixed gas.

As shown in Table 2, the average value was 1.745 μmol/mol and the standard deviation was 0.014 μmol/mol in the 10 concentration measurements performed on different days. Note that the values obtained on different measurement days have standard uncertainties of 0.01 μmol/mol to 0.02 μmol/mol.

1-3. Flow Control Means The flow control means MFC controls the flow rate of gas flowing through the flow path 100.

The flow rate control means MFC can be used without particular restriction as long as it can control the flow rate of gas flowing through the flow path 100, but is preferably a mass flow controller. The mass flow controller measures the mass flow rate of gas flowing through the flow path 100 and controls the flow rate by automatically increasing or decreasing the flow rate of the gas flowing through the flow path 100.

The first flow rate control means MFC1 is disposed in the mixed gas dilution section W0, and controls the flow rate _F1 of the first mixed gas in which the concentration of the target compound flowing through the flow path 104 is the first concentration. By controlling the flow rate _F1 of the first mixed gas flowing through the flow path 104 using the first flow rate control means MFC1, it is possible to control the concentration of the target compound in the finally obtained humidified mixed gas. can.

The second flow rate control means MFC2 controls the flow rate _F2 of the diluent gas supplied to the flow path 105 in the humidifying gas supply section X0. By controlling the flow rate _F2 of the diluent gas flowing through the flow path 105 controlled by the second flow rate control means MFC2, the concentration of the target compound in the humidified mixed gas can be controlled.

Note that the second flow rate control means MFC2 is preferably disposed downstream of the dilution gas introduction section 71 and upstream of the humidification means 120 with respect to the direction in which the gas flows.

If the flow rate control means MFC is placed downstream of the humidification means 120, the flow rate of the gas controlled by the flow rate control means will be equal to the sum of the dilution gas and the water (steam) added by the humidification means 120. Become. At this time, the flow rate control means MFC cannot accurately measure the flow rate due to the influence of water (steam) added by humidification, so it is not easy to correctly control the gas flow rate by the flow rate control means MFC. On the other hand, when the flow rate control means MFC is arranged upstream of the humidification means 120, there is no need to consider the influence of water added by the humidification means 120, and it is possible to supply diluent gas at the correct flow rate to the flow path 105. becomes possible.

The third flow rate control means MFC3 controls the flow rate _F3 of the dilution gas flowing through the flow path 103 in the preliminary dilution section Z0.

The fourth flow rate control means MFC4 is arranged in the preliminary dilution section Z0. The fourth flow rate control means MFC4 controls the flow rate _F4 of the second mixed gas in which the concentration of the target compound flowing through the flow path 102 is the second concentration. By appropriately controlling the flow rate _F4 of the second mixed gas flowing through the flow path 102 and the flow rate _F2 of the diluent gas flowing through the flow path 103, the concentration _C1 of the target compound in the first mixed gas is controlled. Can be done.

The fifth flow rate control means MFC5 is arranged downstream of the diffusion tube DT of the source gas generation means 110, and controls the flow rate _FDT of the gas passing through the diffusion tube DT. By controlling the flow rate F _DT of the gas passing through the diffusion tube DT to a constant amount, the concentration C _DT of the target compound contained in the second mixed gas flowing out from the diffusion tube DT can be kept constant.

1-4. Humidifying Means The humidifying means 120 humidifies the diluent gas supplied through the channel 105 to prepare humidified gas. The humidifying means 120 includes at least a humidifying container HB, a temperature controlling means CTWB, and a first pressure controlling means BPC. Note that the humidifying means 120 includes a container for storing water, and has a configuration capable of controlling the temperature of the water stored in the container to a constant temperature and further maintaining the pressure inside the container at a constant pressure. The present invention is not limited to the configuration described below as long as it includes the following.

The humidifying container HB stores water therein, and prepares a humidifying gas by bubbling diluent gas supplied through a pipe (not shown) in the water. The humidifying container HB includes a container section capable of containing water, and piping configured to bubble diluent gas into the water accommodated in the container section.

The piping includes piping on the upstream side and piping on the downstream side with respect to the gas flow. The upstream piping is open to the inside of the humidifying container HB in order to bubble the flowing diluent gas in the water, and the tip of the piping is at least at a position lower than the water surface, preferably the tip of the piping is at the bottom of the container. is located close to. Further, the downstream piping is arranged at a high position far from the water surface in the humidifying container HB so that the piping will not take in liquid water even if the water surface is violently undulated due to bubbling.

Further, the humidifying container HB has an airtight structure so as to block gas flow between the internal space and the outside. As a result, the inside of the humidifying container HB is isolated from the outside environment as a part of the flow path 105, and the pressure inside the humidifying container HB can be kept constant by the first pressure control means BPC, which will be explained later. It becomes possible. Further, in order to manage the internal pressure, the humidifying container HB preferably includes a pressure gauge (pressure transmitter) P1 that can measure the internal pressure.

The humidifying container preferably includes two humidifying containers (a first humidifying container HB1 and a second humidifying container HB2). The first humidifying container HB1 and the second humidifying container HB2 may have the same configuration or may have different configurations. By providing two humidifying containers HB1 and HB2, the ability to humidify the diluent gas can be increased.

Note that it is not essential to have two or more humidifying containers HB. It goes without saying that even if there is only one humidifying container HB, there is no problem even if only one humidifying container HB is provided as long as the humidifying capacity is sufficient.

The temperature control means CTWB controls the temperature of the water contained in the humidifying container HB so that the temperature of the water is constant. As the temperature control means CTWB, a constant temperature bath, a constant temperature water bath, an oven, etc. that house the humidifying container HB can be exemplified. Furthermore, a humidifying container HB wrapped around a heater and further covered with a heat insulating material can also be used as the temperature control means CTWB. The temperature control means CTWB can keep the saturated vapor pressure of the water contained in the humidifying container HB constant.

The first pressure control means BPC is arranged downstream of the humidifying container HB (in the case where the humidifying means 120 includes two humidifying containers, the second humidifying container HB2 arranged on the downstream side), and The pressure inside the HB is controlled to a constant pressure. As the first pressure control means BPC, for example, an automatic back pressure controller can be mentioned. By keeping the pressure inside the humidifying container HB constant, the concentration of water contained in the humidifying gas can be kept constant.

Here, when a humidified gas having a dew point of 35° C. (approximately 0.056 mol/mol in substance amount fraction) is prepared under atmospheric pressure using the humidified gas supply section X0 of the mixed gas production device 10 according to Embodiment 1. The temperature conditions and pressure conditions of the humidifying container HB are shown below.

When the saturated vapor pressure of water at temperature T during humidification is p _s,T and the pressure during humidification is p, the water concentration contained in the prepared humidifying gas is p _s,T /p according to equation (1). You can ask for it. That is, the saturated vapor pressure of water at 35°C is 5629.2 Pa and the atmospheric pressure is 101.325 kPa, so
p _{s, T} /p=5629.2/101325≒0.056...(1)
becomes. A temperature and a pressure that satisfy this relationship are determined and used as the set temperature of the temperature control means CTWB and the set pressure of the first pressure control means BPC, respectively.

The water content measuring means 130 measures the amount of water added to the diluent gas in the humidifying means 120. The moisture content measuring means 130 may use any measuring method as long as it can measure the amount of water contained in the humidifying gas. For example, moisture meters using various measurement methods such as a capacitance type, a crystal oscillation type, a mirror cooling type, and a laser absorption spectroscopy type can be exemplified. Among these, in the mixed gas production apparatus 10 of Embodiment 1, it is preferable to measure the moisture concentration of the humidified gas using a mirror cooling type moisture meter.

In the mixed gas production device 10 of the first embodiment, a valve 86 is disposed between the flow path 105 and the moisture content measuring means 130, and the humidification is performed only when measuring the moisture content of the humidified gas flowing through the flow path 105. Gas can be sampled. Further, a pressure gauge P2 is arranged between the moisture content measuring means 130 and the valve 86.

1-5. Flow path As the piping constituting the flow path 100, for example, a pipe made of stainless steel, glass, perfluoroalkoxyalkane (PFA), fluororesin, etc. with an inner diameter of 1/10 inch to 1/2 inch can be used. can. Among the above tubes, it is preferable to use a stainless steel tube with an inner diameter of 1/4 inch and whose inner wall is coated with quartz glass.

When the pipe is made of a polar material and the target compound also has polarity, the target compound tends to be easily adsorbed on the inner wall of the pipe. Further, even if the material of the piping does not have polarity, the unevenness existing on the inner wall surface tends to attract adsorption, and the target compound may be adsorbed to the unevenness.

If the target compound is adsorbed on the inner wall of the pipe, it may cause tailing in the gas concentration when switching the gas flowing through the flow path 100, and the concentration of the target compound contained in the mixed gas may become inaccurate. When the target concentration of the mixed gas is on the order of nmole/mol, the influence becomes significant.

In the mixed gas production apparatus 10 according to the first embodiment, it is preferable to shorten the overall length of the piping constituting the flow path 100 as much as possible to reduce the area where the gas contacts the piping. Furthermore, as described above, it is preferable to coat the inner wall of the pipe with quartz glass or to make the inner wall smooth so that the target compound is difficult to adsorb.

Furthermore, it is considered that setting the flow rate of the gas flowing through the flow path 100 to be relatively large promotes adsorption and desorption of the target compound to the inner wall of the pipe, and establishes an equilibrium relationship between the adsorption and desorption of the target compound. This is thought to stabilize the concentration of the target compound in the mixed gas, which is preferable.

1-6. Concentration of target compound in mixed gas 1-6-1. Dilution by preliminary dilution section The mixed gas production apparatus 10 according to the first embodiment performs the first stage dilution by diluting the second mixed gas (concentration C _DT ) supplied via the fifth flow rate control means MFC5. I do. The concentration _C1 of the target compound contained in the first mixed gas obtained by the first stage dilution is determined using the flow rate F4 of the fourth flow rate control means _MFC4 and the flow rate F3 of the third flow rate control means _MFC3. , can be calculated using the following equation (2).
C ₁ =C _DT ×F ₄ /(F ₄ +F ₃ )...(2)

1-6-2. Dilution by Mixed Gas Preparation Unit In the mixed gas production device 10, as a second stage of dilution, the mixed gas in which the concentration of the target compound is _C1 is further diluted. The concentration C of the target compound contained in the mixed gas obtained by the second stage dilution is determined using the flow rate F1 in the first flow rate control means _MFC1 and the flow rate _FDIL of the humidifying gas supplied from the humidifying gas supply section X0. It can be calculated using the following equation (3).
C=C ₁ ×F ₁ /(F ₁ +F _DIL )…(3)

Here, the flow rate F _DIL of the humidifying gas supplied from the humidifying gas supply unit X0 is the sum of the flow rate F ₂ of the second flow rate control means MFC2 and the amount F _W of water added by humidification. Therefore, the following equation (4) holds true.
_FDIL = _F2 + _FW ...(4)

The amount of water _FW added by humidification can be derived from the result of measuring the mixed gas after humidification with the moisture content measuring means 130. Specifically, the moisture content measuring means 130 is used to measure the dew point T _DIL of the humidified mixed gas. Next, using the table described in JIS Z 8806, the saturated water vapor pressure P _W at the dew point T _DIL is determined.

At the same time, the pressure gauge P2 disposed in the flow path 105 measures the pressure P _DIL at the position where the dew point T _DIL was measured by the moisture content measuring means 130. The amount of water contained in the humidified mixed gas is synonymous with the partial pressure of water in the humidified mixed gas, and the following formula (5) holds true. The amount of water contained in the humidified mixed gas is calculated using equation (4).
F _W /F _DIL =F _W /(F ₂ +F _W )=P _W /P _DIL …(5)
_FW is determined by equation (5), and the flow rate F _DIL of the humidified diluent gas can be determined. As a result, the concentration C of the target component can be determined using equation (3).

Note that it is also possible to use a diluent gas that does not pass through the humidifying means 120 as the gas for diluting the mixed gas containing the target compound. Specifically, by closing the valves 84 and 85 and opening the valves 87 and 88, the diluent gas is caused to flow through the flow path 107, thereby converting the mixed gas containing the target compound into the non-humidified diluent gas. It can be diluted with

In this case, as shown in equation (6) below,
_FDIL = _F2 ...(6)
becomes.

2. Mixed gas production device (Embodiment 2)
FIG. 2 is a diagram shown to explain the overall configuration of a mixed gas production apparatus 20 according to the second embodiment. Hereinafter, a mixed gas production apparatus 20 according to a second embodiment will be described using FIG. 2.

In the description of the mixed gas manufacturing device 20 according to the second embodiment, points different from the mixed gas manufacturing device 10 according to the first embodiment will be described. Further, the same elements as those in the mixed gas production apparatus 10 according to Embodiment 1 are given the same reference numerals, and explanations thereof will be omitted.

The mixed gas manufacturing device 20 of the second embodiment differs from the mixed gas manufacturing device 10 of the first embodiment in that it does not include the preliminary dilution section Z0. In other respects, it is the same as the mixed gas production apparatus 10 according to the first embodiment.

A source gas containing the target compound at a second concentration is generated in the source gas generation section Y0, and is supplied to the mixed gas dilution section W0.

Similarly to the mixed gas manufacturing device 20 according to Embodiment 1, the mixed gas manufacturing device 20 according to Embodiment 2 also provides a mixed gas manufacturing device capable of manufacturing a mixed gas in which the concentration of water is controlled to a target concentration. can do.

3. Mixed gas production device (Embodiment 3)
FIG. 3 is a diagram shown to explain the overall configuration of a mixed gas production apparatus 30 according to the third embodiment. Hereinafter, a mixed gas production apparatus 30 according to Embodiment 2 will be described using FIG. 3.

In the description of the mixed gas production device 30 according to the third embodiment, points different from the mixed gas production device 10 according to the first embodiment will be explained. Further, the same elements as those in the mixed gas production apparatus 10 according to Embodiment 1 are given the same reference numerals, and explanations thereof will be omitted.

The mixed gas manufacturing device 30 of the third embodiment differs from the mixed gas manufacturing device 10 of the first embodiment in that the moisture content measuring means 130 and the pressure gauge P2 are directly incorporated in the middle of the flow path 105. . In other respects, it is the same as the mixed gas production apparatus 10 according to the first embodiment.

By incorporating the moisture content measuring means 130 directly into the flow path 105, it becomes possible to constantly measure the moisture content of the humidifying gas flowing through the flow path 105. As a result, it becomes possible to feed back the information on the moisture content obtained by the moisture content measurement means 130 to the temperature control means CTWB and the first pressure control means BPC which constitute the humidification means 120.

4. Mixed gas production device (Embodiment 4)
FIG. 4 is a diagram shown to explain the overall configuration of a mixed gas production apparatus 40 according to the fourth embodiment. Hereinafter, a mixed gas production apparatus 40 according to Embodiment 4 will be described using FIG. 4.

In the following description of the mixed gas production apparatus 40 according to the fourth embodiment, the points that are different from the mixed gas production apparatus 10 according to the first embodiment will be mainly explained, and the same points as the mixed gas production apparatus 10 according to the first embodiment will be explained. Elements are given the same reference numerals and their explanations are omitted.

The mixed gas production apparatus 40 of the fourth embodiment differs from the mixed gas production apparatus 10 according to the first embodiment in that the source gas generation means 110 is a high-pressure container PGC filled with a gas containing the target compound. In other respects, it is the same as the mixed gas production apparatus 10 according to the first embodiment.

The high-pressure container PGC is filled with a gas containing the target compound. The gas containing the target compound here corresponds to the source gas generated in the source gas generating means 110 of Embodiment 1, but is not particularly limited as long as it contains the target compound. That is, the gas may be composed only of the target compound, or it may be a mixed gas containing the target compound at a second concentration.

The gas containing the target compound filled in the high-pressure container PGC is reduced in pressure by a pressure reducer (regulator) and is supplied to the flow path 101 . Furthermore, the flow rate is controlled by the fourth flow rate control means MFC4, and in the merging section 54, it is mixed with the diluent gas that has flowed through the channel 103 of the preliminary dilution section Z0.

Similarly to the mixed gas manufacturing apparatus according to Embodiment 1, the mixed gas manufacturing apparatus 40 according to Embodiment 4 also provides a mixed gas manufacturing apparatus capable of manufacturing a mixed gas in which the concentration of water is controlled to a target concentration. can do.

5. Mixed gas production device (Embodiment 5)
FIG. 5 is a diagram shown to explain the overall configuration of a mixed gas production apparatus 50 according to the fifth embodiment. Hereinafter, a mixed gas production apparatus 50 according to Embodiment 5 will be described using FIG. 5.

In the following description of the mixed gas production apparatus 50 according to the fifth embodiment, the points that are different from the mixed gas production apparatus 10 according to the first embodiment will be mainly explained, and the same points as the mixed gas production apparatus 10 according to the first embodiment will be explained. Elements are given the same reference numerals and their explanations are omitted.

The mixed gas production apparatus 50 of Embodiment 5 differs from the mixed gas production apparatus of Embodiment 1 in that the source gas generation means 110 is a permeation tube PT filled with solid, liquid, or gas containing the target compound. Different from 10. In other respects, it is the same as the mixed gas production apparatus 10 according to the first embodiment.

The permeation tube PT prepares a second mixed gas containing the target compound at a second concentration by the permeation tube method. Specifically, the permeation tube PT is a tube made of polymer resin such as polytetrafluoroethylene or polyethylene, in which a solid, liquid, or gas target compound is sealed, and the target compound is maintained at a constant temperature. The target compound permeates and diffuses through the tube at a constant rate. A diluent gas is sent there at a constant flow rate to continuously generate a gas containing the target compound at a constant concentration.

Similarly to the mixed gas manufacturing apparatus 10 according to the first embodiment, the mixed gas manufacturing apparatus 50 according to the fifth embodiment is capable of manufacturing a mixed gas in which the concentration of water is controlled to the target concentration. can be provided.

6. Method for producing mixed gas Next, a method for producing mixed gas according to Embodiment 6 will be described. FIG. 6 is a diagram shown to explain a method for producing a mixed gas according to Embodiment 6. The method for producing a mixed gas according to the sixth embodiment can be suitably carried out by the mixed gas producing apparatus 10 or the like described in the first embodiment or the like.

The mixed gas manufacturing method includes a first mixed gas supplying step ST1, a humidifying gas supplying step ST2, and a mixing step ST3.

The first mixed gas supply step ST1 is a step in which a first mixed gas containing a target compound at a first concentration is supplied at a first flow rate per unit time. The first mixed gas containing the target compound at the first concentration can be prepared using the source gas generation section Y0 of the mixed gas production apparatus 10 or the like. In the method for producing a mixed gas according to Embodiment 6, the first mixed gas containing the target compound at the first concentration is controlled so that the flow rate per unit time is equal to the first flow rate using a flow rate control means such as a mass flow controller. Control and supply so that

The humidifying gas supply step ST2 is a step of supplying humidifying gas obtained by humidifying diluent gas at a second flow rate per unit time based on the supply amount of diluent gas before humidification. In the humidifying gas supply step ST2, the diluting gas is humidified by bubbling the diluting gas in the humidifying container HB whose temperature and pressure are controlled and which contains water. Prepare humidifying gas.

As described above, the humidifying container HB is a container for storing water for humidifying the diluted gas, and has an airtight structure. Further, the humidifying container HB is configured such that the internal pressure can be adjusted by the first pressure control means BPC. During humidification, by controlling the temperature and pressure of the humidifying container HB and bubbling the diluent gas, even when producing a mixed gas with a high moisture concentration, the water concentration can be controlled to the target moisture concentration. Gas can be produced.

The humidifying gas supply step ST2 may include a moisture amount calculation step of calculating the amount of moisture contained in the prepared humidifying gas. Specifically, as described above, the moisture content measuring means 130 included in the mixed gas production apparatus 10 and the like measures the dew point of the humidifying gas and determines the saturated water vapor pressure. At the same time, the pressure of the humidifying gas is measured by the pressure gauge P2 arranged in the flow path 106. Since the amount of moisture contained in the humidifying gas corresponds to the partial pressure of water in the humidifying gas, the amount of moisture can be calculated from the saturated vapor pressure of the humidifying gas and the pressure of the humidifying gas in the flow path 106. .

The mixing step ST3 is a step of mixing the first mixed gas from the first mixed gas supply step ST1 and the humidifying gas from the humidifying gas supplying step ST2. The flow rates of the first mixed gas and humidifying gas per unit time are controlled to a first flow rate and a second flow rate, respectively. Therefore, by mixing the first mixed gas and the humidifying gas, it is possible to obtain a mixed gas in which the concentration of water is controlled to the target water concentration and the concentration of the target compound is accurately controlled.

Note that in the mixed gas manufacturing method according to the fifth embodiment, the flow rate of the humidifying gas is controlled based on the flow rate of the diluent gas before humidification. This makes it possible to accurately control the flow rate of humidifying gas without being affected by water added by humidification.

5. Example [Example 1]
Using the mixed gas production apparatus 10 shown in FIG. 1, a humidifying gas having a dew point of 35° C. (substance fraction: about 0.056 mol/mol) was prepared under atmospheric pressure. In preparing the humidifying gas, the humidifying gas supply section X0 was used, the diluent gas was passed through the source gas generating section Y0 and the preliminary dilution section Z0, and the entire amount was discarded via the exhaust valve 91 or the exhaust valve 92.

Further, the first pressure control means BPC was operated so that the water temperature of the temperature control means CTWB was 48° C. and the pressure inside the humidification container was 201 kPa in absolute pressure as the temperature during humidification. Further, the flow rate _F2 of the diluent gas supplied via the second flow rate control means MFC2 was set in the range of 1 to 10 L/min. The results are shown in FIG.

FIG. 7 is a diagram showing evaluation results when humidifying gas was produced in Example 1. FIG. 7(a) is a diagram showing changes in the pressure and temperature inside the humidifying container when the flow rate of the diluent gas supplied via the second flow rate control means MFC2 is changed. FIG. 7(b) is a diagram showing a change in the concentration of water in the diluent gas when the flow rate of the diluent gas supplied via the second flow rate control means MFC2 is changed.

As shown in FIG. 7(a), even if the flow rate _F2 of the diluent gas supplied via the second flow rate control means MFC2 is changed in the range of 1 to 10 L/min, the flow rate of the second humidifying container HB2 is It can be confirmed that the internal pressure and temperature are controlled to be constant.

As shown in FIG. 7(b), the moisture concentration of the humidifying gas is approximately 0.055 mol/mol, and the fluctuation range during the preparation time is approximately 0.001 mol/mol. .

[Comparative example]
In the mixed gas production apparatus 10 shown in FIG. 1, humidified gas was prepared by keeping the first pressure control means BPC fully open at all times and controlling only the temperature of the temperature control means CTWB. That is, in the comparative example, considering that the conventional device performs humidification by controlling only the temperature during humidification, the water temperature of the temperature control means CTWB is controlled at 35°C, and the dew point is adjusted under atmospheric pressure. An attempt was made to prepare a humidifying gas at 35° C. (approximately 0.056 mol/mol in substance amount fraction).

In the comparative example as well, the humidified gas supply section X0 of the mixed gas production device 10 is used, the dilution gas is passed through the source gas generation section Y0 and the preliminary dilution section Z0, and the gas is passed through the exhaust valve 91 or the exhaust valve 92. The entire amount was discarded. Furthermore, the water temperature of the temperature control means CTWB was set at 35° C. during humidification. The results are shown in FIG.

FIG. 8 is a diagram showing evaluation results when humidifying gas was produced in a comparative example. FIG. 8(a) is a diagram showing changes in the pressure and temperature inside the humidifying container when the flow rate of the diluent gas supplied via the second flow rate control means MFC2 is changed. FIG. 8(b) is a diagram showing changes in the water concentration in the diluent gas when the flow rate of the diluent gas supplied via the second flow rate control means MFC2 is changed.

As shown in FIG. 8(a), even if the flow rate _F2 of the diluent gas supplied via the second flow rate control means MFC2 is changed in the range of 1 to 10 L/min, the flow rate of the second humidifying container HB2 is The internal temperature was kept constant. However, the pressure inside the second humidification container HB2 increased as the flow rate of the diluent gas increased.

Further, as shown in FIG. 8(b), the moisture concentration of the humidifying gas decreased as the flow rate _F2 of the diluent gas to be supplied increased. In addition, the moisture concentration of the humidifying gas was approximately 0.04 mol/mol even under the condition where the flow rate of the diluent gas to be supplied was the smallest, and the result was that humidification could not be achieved to the desired moisture concentration.

[Example 2]
Using the mixed gas production apparatus 10 according to Embodiment 1, an acetone mixed gas of Example 2 and an acetone mixed gas of Reference Example, in which the target compound is acetone, were manufactured. The setting conditions of the first flow rate control means MFC1 to the fourth flow rate control means MFC4 were as shown in Table 3.

The acetone mixed gas of Example 2 uses a humidifying gas as the second-stage diluting gas, and the acetone mixed gas of the reference example uses a non-humidifying diluting gas as the second-stage diluting gas. be.

A highly concentrated acetone mixed gas was generated using a diffusion tube DT. The fifth flow rate control means MFC5 was set at 500 mL/min, and the second pressure control means APC was set at 200 kPa. The concentration of acetone in the high concentration mixed gas at this time was 1.75 μmol/mol.

The humidifying gas in Example 2 was generated in the humidifying means 120 of the humidifying gas supply section X0. The water temperature of the temperature control means CTWB was set to 48° C., and the absolute pressure inside the humidifying container HB was controlled to be 201 kPa by the first pressure control means BPC.

The produced acetone mixed gas of Example 2 and the acetone mixed gas of Reference Example were analyzed using a gas chromatograph equipped with a flame ionization detector and a concentrator. The analytical equipment and analytical conditions used for the analysis are described below.
Gas chromatograph device: Agilent Technologies 7890B
Column: DB-1, 60m x 0.32mm x 1μm
Carrier gas: He, 2.45mL/min
Oven temperature: Initial temperature 35℃ (held for 4 minutes) → Increased temperature by 5℃ per minute → 65℃ → Increased temperature by 20℃ per minute → 225℃ (held for 2 minutes)
Detector: Hydrogen flame ionization detector Concentrator Equipment: Entech Instruments 7200 Preconcentrator
Sample concentration amount: 400mL
Concentration module 1 set temperature: Trap -40℃, Desorb 10℃
Concentration module 2 set temperature: Trap -100℃, Desorb 210℃

Since the concentrator used in the evaluation removes water by concentration before the analysis sample enters the gas chromatograph, the humidified acetone mixed gas of Example 2 becomes a dry gas during analysis. This allows comparison with the acetone mixed gas of the reference example.

The obtained results are shown in Table 4, Table 5, FIG. 9 and FIG. 10.

FIG. 9 is a diagram showing an example of a chromatogram obtained by analyzing the acetone mixed gas produced in Example 2 using a gas chromatograph. The peak with a retention time of 5.677 minutes is acetone.

FIG. 10 is a diagram showing the relationship between the prepared concentration of acetone (target concentration) and the peak area value analyzed by gas chromatography for the acetone mixed gas produced in Example 2 and the acetone mixed gas produced in Reference Example. be.

From FIG. 10, it can be seen that for both the acetone mixed gas produced in Example 2 and the acetone mixed gas produced in Reference Example, the relationship between the prepared concentration of acetone and the peak area value is a good linear relationship. . Further, the slopes of the linear straight lines of the acetone mixed gas produced in Example 2 and the acetone mixed gas produced in Reference Example were almost the same. These results indicate that the production of mixed gas through two-stage dilution is successful, regardless of whether the diluent gas used for the second-stage dilution is a humidifying gas or a non-humidifying diluent gas. It can be said that

The mixed gas production apparatus 10 of the present invention includes a mixed gas dilution section W0 that prepares a mixed gas containing a target compound, and a humidified gas supply section X0 that humidifies the diluted gas that dilutes the mixed gas. The mixed gas dilution unit W0 includes a first flow rate control means MFC1 that controls the flow rate of the first mixed gas in which the concentration of the target compound is a first concentration higher than the target concentration. The humidifying gas supply section X0 includes a humidifying means 120 and a second flow rate control means MFC2 that controls the flow rate of the diluent gas supplied to the humidifying means 120. The humidifying means 120 includes a humidifying container HB for humidifying the diluent gas, a temperature controlling means CTWB for controlling the temperature of the water contained in the humidifying container HB, and a first pressure controlling means BPC for controlling the pressure inside the humidifying container HB. Equipped with.

That is, in the mixed gas production apparatus 10 of the present invention, the humidified gas supply section X0 includes a temperature control means CTWB that controls the temperature of the humidification container HB, and a first pressure control means BPC that controls the pressure of the humidification container HB. Be prepared. This makes it possible to prepare humidifying gas with any moisture concentration without depending on the flow rate of diluent gas.

As a result, even when producing a mixed gas with a high moisture concentration, it is possible to provide a mixed gas production apparatus that can produce a mixed gas with a target moisture concentration.

The mixed gas manufacturing method of the present invention includes a first mixed gas supplying step ST1, a humidifying gas supplying step ST2, and a mixing step ST3.

The first mixed gas supply step ST1 is a step of supplying a first mixed gas containing a target compound at a first concentration while controlling the flow rate per unit time to a first flow rate. The humidifying gas supply step ST2 is a step of supplying humidifying gas obtained by humidifying diluent gas by controlling the flow rate per unit time to a second flow rate based on the supply amount of diluent gas before humidification. The mixing step ST3 is a step of mixing the first mixed gas supplied in the first mixed gas supply step ST1 and the humidifying gas supplied in the humidifying gas supplying step ST2.

Further, in the humidifying gas supply step ST2, the diluent gas is humidified by bubbling the diluent gas in the humidifying container HB whose temperature and pressure are controlled and which contains water.

That is, the mixed gas production method of the present invention humidifies the diluted gas by bubbling the diluted gas inside the humidifying container HB whose temperature and pressure are controlled and which contains water. It has a humidifying gas supply step ST2. This makes it possible to prepare humidifying gas adjusted to any moisture concentration.

As a result, even when producing a mixed gas with a high moisture concentration, it is possible to provide a method for producing a mixed gas with a target moisture concentration.

10, 20, 30, 40, 50... Mixed gas production device, 51, 61, 71... Dilution gas introduction part, 53, 55, 65... Branch part, 54, 56... Merging part, 80, 81, 82, 83, 84, 85, 86, 87, 88... Valve, 91, 92, 93... Exhaust valve, 100, 101, 102, 103, 104, 105, 106, 107... Channel, 110... Source gas generation means, 120... Humidification Means, 130...Moisture content measuring means, APC...Second pressure control means (automatic pressure controller), BPC...First pressure control means (automatic back pressure controller), AS1, AS2, AS3...Analytical instrument sample introduction Port, CTWB...temperature control means (thermal bath), DT...diffusion tube, HB...humidification container, HB1...first humidification container, HB2...second humidification container, MFC...flow rate control means (mass flow controller), MFC1... First flow control means (mass flow controller 1), MFC2...second flow control means (mass flow controller 2), MFC3...third flow control means (mass flow controller 3), MFC4...fourth flow control means (mass flow controller Controller 4), MFC5...Fifth flow rate control means (mass flow controller 5), P1, P2...Pressure gauge, PT...Permeation tube, W0...Mixed gas dilution section, X0...Humidified gas supply section, Y0...Source gas generation Part, Z0...Pre-dilution part

Claims (11)

a source gas generation unit that prepares a mixed gas containing a target compound and in which the concentration of the target compound is higher than the target concentration;
a humidifying gas supply unit that supplies humidifying gas to humidify the mixed gas;
A mixed gas production device comprising: a mixed gas dilution unit that dilutes a first mixed gas having a first concentration higher than a target concentration with the humidifying gas,
The humidifying gas supply section includes a humidifying container for humidifying diluted gas, a temperature control means for controlling the temperature of water contained in the humidifying container, and a first pressure control means for controlling the pressure inside the humidifying container. and a second flow control means for controlling the flow rate of the diluent gas supplied to the humidification means,
A mixed gas manufacturing apparatus, wherein the mixed gas diluting section includes a first flow rate control means for controlling the flow rate of the first mixed gas. The mixed gas production device according to claim 1,
A mixed gas production apparatus characterized in that the second flow rate control means is disposed upstream of the humidification means. The mixed gas production device according to claim 1,
The mixed gas production apparatus characterized in that the humidified gas supply section further includes a moisture content measuring means for measuring the moisture content contained in the humidified gas. The mixed gas production device according to claim 1,
comprising a preliminary dilution unit that supplies the dilution gas that dilutes the second mixed gas in which the target compound has a second concentration higher than the first concentration;
A mixed gas manufacturing apparatus characterized in that the preliminary dilution section has a third flow rate control means for controlling the flow rate of the dilution gas. The mixed gas production device according to claim 1,
A mixed gas production apparatus characterized in that the first flow rate control means and the second flow rate control means are mass flow controllers. The mixed gas production device according to claim 1,
A mixed gas production device characterized in that the humidifying container includes a first humidifying container and a second humidifying container. The mixed gas production device according to claim 1,
A mixed gas production apparatus characterized in that the source gas generation section includes a diffusion tube containing the target compound in a solid phase or a liquid phase, and a second pressure control means. The mixed gas production device according to claim 1,
A mixed gas production apparatus characterized in that the source gas generation section includes a high-pressure container containing a gas containing the target compound. The mixed gas production device according to claim 1,
A mixed gas production apparatus characterized in that the source gas generation section includes a permeation tube containing the target compound in a solid phase, liquid phase, or gas phase. a first mixed gas supply step of supplying a first mixed gas having a first concentration of the target compound while controlling the flow rate per unit time to the first flow rate;
a humidifying gas supply step of supplying a humidified gas obtained by humidifying a diluent gas by controlling the flow rate per unit time to a second flow rate based on the supply amount of the diluent gas before humidification;
a mixing step of mixing the first mixed gas supplied in the first mixed gas supply step and the humidifying gas supplied in the humidifying gas supplying step,
The humidifying gas supply step includes humidifying the diluent gas by bubbling the diluent gas in a humidifying container whose internal temperature and pressure are controlled and which contains water; A mixed gas production method characterized by: The mixed gas production method according to claim 10,
The humidifying gas supply step includes a moisture content calculation step of measuring the dew point and pressure of the humidifying gas, and calculating the moisture content of the humidifying gas from the dew point and pressure obtained by the measurement. A mixed gas production method.

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