JP2016061648A - Gas sampling device and gas analysis method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a gas sampling device and a gas analysis method capable of simply and highly accurately analyzing each component contained in a sampling gas, and capable of sampling a sampling gas for which a balance of a composition of a whole of the gas can be analyzed.SOLUTION: The gas sampling device is provided with: a thermostatic tank 13 that has a thermostatic part 13a heatable to a gas temperature of an off gas G or higher; a gas sampling line 12 that has a part thereof being disposed in the thermostatic part 13a and samples the off gas G; a flow meter 18 that is disposed in the gas sampling line 12 in the thermostatic part 13a and measures a flow rate of the off gas G flowing through the gas sampling line 12; a flow rate control part 21 that controls the gas flow rate of the off gas G flowing through the gas sampling line 12 on the basis of the gas flow rate of the off gas G measured by the flow meter 18; a gas component absorption part 14 that absorbs the components contained in the off gas G supplied from the gas sampling line 12; and a gas sampling part 16 that samples the off gas G, the components of which have been absorbed by the gas component absorption part 14.SELECTED DRAWING: Figure 1

Description

  The present invention relates to a gas sampling device and a gas analysis method, and for example, relates to a gas sampling device and a gas analysis method that are preferably used for analyzing off-gas such as coal gasification gas.

Conventionally, carbon dioxide (CO ₂ ), nitrogen (N ₂ ), moisture (H ₂ O), ammonia (NH ₃ ), hydrogen sulfide (H ₂ S) discharged from plants such as gas facilities of IGCC (Integrated Gasification Combined Cycle) For example, a technique for analyzing off-gas such as coal gasification gas whose main component is gas) has been proposed (see, for example, Patent Document 1). In this analysis technique, a predetermined amount of off-gas is collected with a syringe, and an absorption liquid that absorbs a specific component into the collected off-gas is injected into the syringe so that the carbon dioxide and ammonia contained in the off-gas react with each other. The product is absorbed by the absorbent and analyzed. In this analysis technique, by analyzing the concentration of other components in the residual gas that has absorbed the precipitates by gas chromatography, it is possible to grasp the balance of the composition of the entire off-gas gas, which was difficult by official analysis such as JIS. It becomes possible.

Japanese Patent No. 5123833

  However, in the analysis technique described in Patent Document 1, since the exhaust gas is collected with a syringe, the amount of gas that can be analyzed is limited. For this reason, it has been difficult to grasp the balance of the composition of the whole gas by grasping the average value of the gas composition taking into account the variation of the gas composition of the exhaust gas every predetermined period and the variation range of the gas composition.

  The present invention has been made in view of such circumstances, and a sampled gas that can analyze each component contained in the sampled gas simply and with high accuracy and can analyze the balance of the composition of the entire gas. An object is to provide a gas sampling device and a gas analysis method that can be collected.

  The gas sampling device of the present invention includes a thermostatic chamber having a thermostatic section that can be heated to a temperature higher than the gas temperature of the gas to be collected, a gas sampling line that is partially disposed in the thermostatic section, and collects the gas to be sampled. A gas flow meter provided in the gas sampling line in the constant temperature section and measuring the flow rate of the sampled gas flowing through the gas sampling line; and the gas based on the gas flow rate of the sampled gas measured by the flow meter. A flow rate control unit for controlling the gas flow rate of the sampled gas flowing through the sampling line, and a component included in the sampled gas supplied from the gas sampling line, provided at a subsequent stage of the thermostatic chamber in the gas sampling line. Gas component absorption unit for absorbing, and gas collection unit for collecting the sampled gas, which is provided at the subsequent stage of the gas component absorption unit in the gas sampling line and the component is absorbed by the gas component absorption unit Characterized by comprising a.

  According to this configuration, the sampled gas is continuously controlled by controlling the flow rate of the sampled gas while preventing condensation and precipitation of the gas components in the sampled gas in a state where the sampled gas is heated above the gas temperature of the sampled gas in the constant temperature part. Therefore, it is possible to analyze the average value and the fluctuation value in consideration of the composition fluctuation of various gas components in the sampled gas every predetermined period. Thereby, each component contained in the sampled gas can be analyzed easily and with high accuracy, and a gas sampling device capable of analyzing the balance of the composition of the entire sampled gas can be realized.

  In the gas sampling device of the present invention, it is preferable that the gas sampling apparatus includes a suction nozzle that is connected to the gas sampling line and has a distal end portion disposed along the gas flow direction of the sampled gas. With this configuration, the sampled gas containing the mist-like component contained in the sampled gas can be collected, so that the composition of the entire sampled gas including the mist-like component can be analyzed.

  In the gas sampling apparatus of the present invention, it is preferable that the flow rate control unit slows the gas flow rate of the sampled gas flowing through the gas sampling line with respect to the flow rate of the sampled gas. With this configuration, it is possible to prevent the excessive mist-like component from being sucked from the tip of the suction nozzle, so that the composition of the entire gas including the mist-like component of the sampled gas can be analyzed with high accuracy.

  In the gas sampling apparatus of the present invention, it is preferable that the gas sampling apparatus includes a suction nozzle that is connected to the gas sampling line and has a tip portion disposed in a direction facing the gas flow direction of the sampled gas. With this configuration, it is possible to collect the sampled gas excluding the mist-like component contained in the sampled gas, and thus it is possible to analyze the gas composition of the gaseous component of the sampled gas.

  In the gas sampling apparatus of the present invention, it is preferable that the flow rate control unit makes the gas flow rate of the sampled gas flowing through the gas sampling line substantially equal to the flow rate of the sampled gas. With this configuration, the suction of the mist-like component from the tip of the suction nozzle can be prevented, so that the gas composition of the gaseous component of the sampled gas can be analyzed with high accuracy.

  In the gas sampling device of the present invention, a nozzle drive unit that switches the tip of the suction nozzle between a direction along the gas flow direction of the sampled gas and a direction facing the gas flow direction of the sampled gas. It is preferable to provide. With this configuration, it is possible to analyze the composition of the entire gas in the sampled gas containing the mist-like component, analyze the gaseous component in the sampled gas, and analyze the mist-like component in the sampled gas. Therefore, it is possible to accurately analyze the balance of the composition of the gas to be collected.

  In the gas sampling device of the present invention, the first gas sampling line and the second gas sampling line, which are formed by branching the gas sampling line in the subsequent stage of the thermostat, and the subsequent stage of the thermostat in the first gas sampling line. A first gas component absorber that absorbs a component contained in the sampled gas supplied from the first gas sampling line, and a stage subsequent to the first gas component absorber in the first gas sampling line. A first gas sampling unit that collects the sampled gas whose components have been absorbed by the first gas component absorption unit, and a second stage of the thermostat bath in the second gas sampling line. A second gas component absorber that absorbs a component contained in the sampled gas supplied from the second gas component absorber, and a second gas component absorber that is provided in a stage subsequent to the second gas component absorber in the second gas sampling line. A second gas sampling unit that collects the sampled gas in which the component is absorbed by the gas component absorption unit; and a direction of the tip of the suction nozzle that is switched by the nozzle driving unit; and the first gas sampling line; It is preferable that a control unit that controls switching of the flow path of the sampled gas with the second gas sampling line is provided. With this configuration, the composition of the entire gas in the sampled gas including the mist component can be changed by simply switching the gas flow path of the sampled gas between the first gas sampling line and the second gas sampling line by the control unit. Analysis, analysis of the gaseous component in the sampled gas, and analysis of the mist-like component in the sampled gas are possible, so that the balance of the composition of the entire sampled gas can be analyzed easily and accurately.

  In the gas sampling apparatus of this invention, it is preferable that a heat insulating material is provided in the front | former part of the said thermostat in the said gas sampling line. With this configuration, it is possible to prevent cooling of the sampled gas flowing through the gas sampling line, and thus it is possible to prevent condensation and precipitation of gas components in the sampled gas introduced into the constant temperature bath.

  In the gas sampling device of the present invention, it is preferable that a heating unit for heating the gas sampling line is provided in a previous stage of the thermostatic chamber in the gas sampling line. With this configuration, it is possible to prevent cooling of the sampled gas flowing through the gas sampling line, and thus it is possible to prevent condensation and precipitation of gas components in the sampled gas introduced into the constant temperature bath.

  The gas analysis method of the present invention is a gas analysis method using the gas sampling device, wherein the gas component absorption unit analyzes the sulfuric acid having absorbed ammonia and moisture in the sampled gas by ion chromatography. Determining the concentration of ammonia and moisture in the sampled gas, and analyzing the sampled gas collected in the gas collecting unit by gas chromatography to analyze at least one of hydrogen sulfide, carbon dioxide, nitrogen, hydrogen and methane. And a step of determining the concentration of the seed.

  According to this method, in the sampled gas continuously collected by controlling the flow rate of the sampled gas while preventing the deposition and condensation of gas components in the sampled gas in the gas sampling line. Ammonia, moisture, hydrogen sulfide, carbon dioxide, nitrogen, hydrogen and methane can be analyzed. As a result, it is possible to analyze the average value and fluctuation value considering the composition fluctuation of ammonia, moisture, hydrogen sulfide, carbon dioxide, nitrogen, hydrogen and methane in the sampled gas every predetermined period. It is possible to realize a gas analysis method that can analyze each component contained in the gas easily and with high accuracy and can analyze the balance of the composition of the entire gas to be collected.

  In the gas analysis method of the present invention, the water in the sampled gas is analyzed by the Karl Fischer titration method by analyzing the ethanol in which the moisture, the polar component and the organic component in the sampled gas are absorbed by the gas component absorption unit, It is preferable to include the process of calculating | requiring the density | concentration of a polar component and an organic component. By this method, moisture in the sampled gas obtained by continuously collecting the sampled gas by controlling the flow rate of the sampled gas while preventing precipitation and condensation of gas components in the sampled gas in the gas sampling line, Since the polar component and the organic component can be analyzed, it is possible to analyze the average value and the variation value in consideration of the composition variation of the water, the polar component, and the organic component in the sampled gas every predetermined period.

  According to the present invention, there is provided a gas sampling apparatus and a gas analysis method capable of collecting a sampled gas that can analyze each component contained in the sampled gas easily and with high accuracy and can analyze the balance of the composition of the entire gas. realizable.

FIG. 1 is a schematic diagram of a gas sampling apparatus according to the first embodiment. FIG. 2 is a schematic diagram of a gas sampling device according to the second embodiment. FIG. 3 is a schematic diagram of a gas sampling device according to the second embodiment. FIG. 4A is a schematic diagram of the suction nozzle of the gas sampling device according to the second embodiment. FIG. 4B is a schematic diagram of the suction nozzle of the gas sampling device according to the second embodiment. FIG. 5 is a schematic diagram of a gas sampling apparatus according to the third embodiment. FIG. 6A is a schematic diagram of a gas sampling apparatus according to the third embodiment. FIG. 6B is a schematic diagram of the gas sampling device according to the third embodiment. FIG. 7 is a schematic diagram of a gas sampling apparatus according to the fourth embodiment.

  Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. In addition, it is not limited to each following embodiment, It can implement by changing suitably. Also, the following embodiments can be implemented in combination as appropriate.

(First embodiment)
FIG. 1 is a schematic diagram of a gas sampling device 1 according to a first embodiment of the present invention. The gas sampling apparatus 1 according to the present embodiment can collect off-gas (collected gas) G such as coal gasification gas to be collected and analyze each component contained in the off-gas G to grasp the gas composition. This is a gas sampling device. Here, the off-gas is a concentration of components removed from the coal gasification gas in the process of the coal gasification gas, and ammonia (NH ₃ ), hydrogen sulfide (H ₂ S), and carbon dioxide (CO ₂ ). ₂ ) A by-product gas having a main composition.

  The gas sampling device 1 according to the present embodiment includes a gas sampling line 12 having one end connected to a hole 11b provided in the flange portion 11a of the gas mother pipe 11 through which the off gas G flows. The gas sampling line 12 includes a thermostatic chamber 13 in which a part of the gas sampling line 12 is disposed from one end side to the other end side of the gas sampling line 12, and a gas component contained in the offgas G. A gas component absorption unit 14 that absorbs part of the gas, a dehydration unit 15 that dehydrates moisture contained in the off gas G in which part of the gas component is absorbed, and a gas sampling unit 16 that collects the off gas G are provided in this order. ing. The connecting portion between the gas mother pipe 11 and the thermostatic chamber 13 at the front stage of the thermostatic chamber 13 of the gas sampling line 12 is kept warm by a heat insulating material 12a that prevents the gas temperature of the off-gas G flowing through the gas sampling line 12 from decreasing. Has been. In this way, by keeping the connecting portion between the gas mother pipe 11 and the thermostatic chamber 13 with a heat insulating material, the carbon dioxide in which the gas components in the offgas G have reacted due to the decrease in the gas temperature of the offgas G flowing through the gas sampling line 12. It becomes possible to prevent precipitation and condensation of ammonium and the like.

  The constant temperature bath 13 includes a constant temperature portion 13a capable of heating the interior to a temperature higher than the off-gas temperature and a normal temperature portion 13b set to a normal temperature. A part of the gas sampling line 12 is disposed in the constant temperature portion 13 a of the constant temperature bath 13. A flow rate control valve 17 that adjusts the flow rate of the off-gas G flowing in the gas sampling line 12 from one end side to the other end side of the gas sampling line 12 is provided in the gas sampling line 12 in the thermostatic part 13a of the thermostatic chamber 13; A flow meter 18 for measuring the flow rate of the off gas G flowing in the gas sampling line 12 and a suction pump 19 for sucking the off gas G in the gas sampling line 12 are provided in this order. In addition, the constant temperature part 13a is provided with a heating part 20 that heats the constant temperature part 13a to a predetermined temperature (for example, 120 ° C.) that is equal to or higher than the temperature of the offgas G. In the example shown in FIG. 1, the example in which the heating unit 20 is provided inside the constant temperature unit 13a has been described. However, the heating unit 20 is not provided inside the constant temperature unit 13a, and the constant temperature unit 13a is covered. A heating unit may be provided to heat the constant temperature unit 13a.

  In addition, a flow rate control unit 21 that displays the flow rate of the off gas G flowing through the gas sampling line 12 and controls the flow rate of the off gas G is disposed in the normal temperature unit 13 b of the thermostatic chamber 13. The flow rate control unit 21 sets in advance the flow rate of the off gas G flowing through the gas sampling line 12 via the flow rate control valve 17 based on the flow rate of the off gas G flowing through the gas sampling line 12 measured by the flow meter 18. Control to flow rate. When the flow rate of the off gas G is high, the flow rate control unit 21 reduces the flow rate of the off gas G by reducing the opening degree of the flow rate control valve 17. Further, when the flow rate of the off gas G is small, the flow rate control unit 21 increases the flow rate of the off gas G by increasing the opening degree of the flow rate control valve 17. The flow rate control unit 21 may control the flow rate of the off gas G by changing the suction amount of the suction pump 19. Thus, in this embodiment, since the flow rate of the off gas G can be controlled in the constant temperature portion 13a under a constant temperature condition, it is possible to prevent precipitation and condensation of the gas components in the off gas G, and the flow rate of the off gas G Can be accurately controlled to improve the collection accuracy of the off-gas G.

The gas component absorption part 14 is provided with the 1st absorption part 14a provided in the back | latter stage of the thermostat 13 in the gas sampling line 12, and the 2nd absorption part 14b provided in the back | latter stage of the 1st absorption part 14a. The first absorption part 14a is, for example, comprises an absorbent bottle first absorbing liquid _{L 1} to absorb ammonia in the off-gas G such as an internal in a 20% by weight sulfuric acid _(H 2 SO ₄₎ is sealed. The second absorption part 14b is, for example, the absorption bottle water in the off-gas G such as an internal in absolute ethanol (C 2 _{H 6 O),} the second absorption liquid L ₂ to absorb polar components and organic components are sealed Is provided. The gas component absorption unit 14 absorbs ammonia in the off-gas G such as 20% by mass sulfuric acid (H ₂ SO ₄ ) inside each of the first absorption unit 14a and the second absorption unit 14b. ₁ may be enclosed, and a second absorption liquid L ₂ that absorbs moisture in the off-gas G such as absolute ethanol (C ₂ H ₆ O) is contained in each of the first absorption section 14a and the second absorption section 14b. It may be enclosed. In addition, methanol and isopropyl alcohol can also be used as an absorbing solution that absorbs moisture, polar components, and organic components.

  The dehydrating unit 15 is configured by, for example, a glass column in which a dehydrating agent 15a such as calcium chloride that absorbs moisture of the gas component absorbing unit 14 off-gas G is enclosed. The dehydrating unit 15 is not particularly limited as long as it can remove moisture in the offgas G, and for example, silica gel or the like may be used. The gas sampling unit 16 includes, for example, a container that can collect gas inside a gas sampling bag or the like.

  Next, the overall operation of the gas sampling device 1 according to this embodiment will be described. First, the gas sampling unit 16 is connected to the other end of the gas sampling line 12, and a predetermined amount (for example, 100 ml) of 20% by mass sulfuric acid is respectively added to the first absorption unit 14a and the second absorption unit 14b of the gas component absorption unit 14. Connect two charged bottles in series. Next, the flow rate control unit 21 causes the heating unit 20 to set the temperature in the constant temperature unit 13a of the constant temperature bath 13 to a predetermined temperature (for example, 120 ° C.) higher than the temperature (for example, 100 ° C.) of the offgas G flowing through the gas mother pipe 11. ) To adjust. Subsequently, the flow rate control unit 21 sets the flow rate of the gas flowing through the gas sampling line 12 at a predetermined flow rate (for example, 5 m / sec or more and 20 m / sec) to a predetermined flow rate (for example, 1 L / min), and the suction pump 19 is turned on. At the same time, the flow control valve 17 is adjusted to a predetermined opening, and the off-gas G flowing through the gas mother pipe 11 is drawn into the gas sampling line 12. As a result, the off-gas G flowing through the gas mother pipe 11 is drawn into the thermostatic part 13 a of the thermostatic bath 13 through the gas sampling line 12. Here, in this embodiment, since the heat insulating material 12a is wound between the gas mother pipe 11 and the thermostatic chamber 13 in the gas sampling line 12, the gas sampling from the gas sampling line 12 to the inside of the thermostatic chamber 13 is performed. It becomes possible to prevent the cooling of the off-gas G in the line 12 and to prevent the gas components of the off-gas G from aggregating and precipitating.

The off-gas G drawn into the gas sampling line 12 is introduced into a gas component absorption unit 14 provided at the subsequent stage of the thermostatic chamber 13 after the flow rate is measured by the flow meter 18. The off-gas G introduced into the gas component absorption unit 14 absorbs ammonia (NH ₃ ) and moisture (H ₂ O) in the gas by the first absorption unit 14a and the second absorption unit 14b. Thereafter, the off-gas G in which ammonia and moisture are absorbed is collected by the gas collection unit 16 after the moisture and sulfuric acid mist are absorbed by the dehydrating agent 15 a disposed in the dehydration unit 15.

Next, two absorption bottles each containing a predetermined amount (for example, 100 ml) of absolute ethanol are connected in series to the first absorption unit 14a and the second absorption unit 14b of the gas component absorption unit 14, respectively. Then, the flow rate control unit 21 sets the flow rate of the gas flowing through the gas sampling line 12 at a predetermined flow rate (for example, 5 m / sec or more and 20 m / sec) to a predetermined flow rate (for example, 1 L / min), and starts the suction pump 19. At the same time, the flow control valve 17 is adjusted to a predetermined opening, and the off-gas G flowing through the gas mother pipe 11 is drawn into the gas sampling line 12. The off-gas G drawn into the gas sampling line 12 is introduced into a gas component absorption unit 14 provided at the subsequent stage of the thermostatic chamber 13 after the flow rate is measured by the flow meter 18. In the off-gas G introduced into the gas component absorption unit 14, moisture, polar components, and organic components are absorbed by the first absorption unit 14a and the second absorption unit 14b. Thereafter, the off-gas G in which moisture, polar components, and organic components are absorbed is collected by the gas collection unit 16 after the moisture and ethanol are absorbed by the dehydrating agent 15 a disposed in the dehydration unit 15. In the off-gas G recovered by the gas sampling unit 16 in this way, hydrogen sulfide (H ₂ S), carbon dioxide gas (CO ₂ ), nitrogen (N ₂ ), hydrogen (H ₂ ), methane (CH ₄ ) and the like are recovered.

Next, the off-gas G collected in the gas sampling unit 16 is analyzed by a gas chromatography (GC) / thermal conductivity detector (TCD), so that hydrogen sulfide (H ₂ S), carbon dioxide gas (CO ₂ ), The concentration of nitrogen (N ₂ ), hydrogen (H ₂ ), methane (CH ₄ ), etc. is required. Further, by analyzing the absorption liquid using 20% by mass sulfuric acid recovered from the gas component absorption unit 14 by ion chromatography (IC), the ammonium ion (NH ₄ ⁺ ) is quantified to determine the amount of ammonia (NH ₃ ). The concentration is required. Further, by analyzing the absorption liquid using anhydrous ethanol collected from the gas component absorption unit 14 by Karl Fischer (KF) titration method, H ₂ O is quantified to determine the moisture concentration in the offgas. As a result, it is possible to accurately analyze each component contained in the offgas G while extracting the offgas G flowing through the gas mother pipe 11 to the gas sampling line 12 at a predetermined flow rate. It becomes possible to grasp the balance.

  As described above, according to the gas sampling device 1 according to the present embodiment, the off-gas G can be sampled while being heated to a temperature higher than the gas temperature of the off-gas G in the constant temperature portion 13a. The off-gas G can be continuously collected by controlling the flow rate of the off-gas G while preventing the precipitation and condensation of the gas components in the off-gas G. As a result, it becomes possible to analyze the average value and the fluctuation value in consideration of the composition fluctuation of various gas components in the off-gas G every predetermined period, so that each component contained in the off-gas G can be easily and accurately analyzed. Further, it is possible to realize a gas sampling device that can analyze the balance of the composition of the entire off-gas G gas.

  In particular, according to the present embodiment, the analysis can be performed in a short time (for example, 2 hours) from the collection of the offgas G to the calculation of the analysis results of the various components of the offgas G. Can be recorded, so the amount of sampled gas can be accurately grasped. As for data reliability, the analysis accuracy can be greatly improved as compared to the JIS absorption method. Moreover, since the collection flow rate and the collection time of the off gas G can be set arbitrarily, the off gas G can be collected under conditions that take into account the variation in the gas composition of the off gas G.

Furthermore, according to the present embodiment, carbon dioxide (CO ₂ ), nitrogen (N ₂ ), moisture (H ₂ O), ammonia (NH ₃ ) as main components in an off-gas G system such as coal gasification gas. Hydrogen sulfide (H ₂ S) and the like can be analyzed easily and with higher accuracy, and the operation of the plant process can be further optimized and stabilized.

In the above-described embodiment, the case of off-gas generated by coal gasification gas or the like has been described. However, the present invention is not limited to this. For example, IGCC gas equipment, NH ₃ plant, and petroleum plant It can also be used for monitoring and analysis of exhaust gas discharged from the

  Moreover, although embodiment mentioned above demonstrated the example which heat-insulates between the gas mother pipe 11 and the thermostat 13 in the gas sampling line 12 with the heat insulating material 12a, the heat insulating material 12a is the gas sampling line 12. If the aggregation and precipitation of the gas components of the off-gas G flowing through the gas can be prevented, it is not always necessary. Further, the flow rate control valve 17 and the suction pump 19 are not necessarily provided as long as the flow rate of the off gas G measured by the flow meter 18 can be within a predetermined range.

(Second Embodiment)
By the way, when analyzing off-gas G, such as coal gasification gas, in the off-gas G, in addition to a gas component, a mist-like component in which fine droplets are dispersed may exist. Therefore, when the off gas G is simply drawn into the gas sampling line 12 from the gas mother pipe 11, the mist-like component contained in the off gas G is also drawn into the gas sampling line 12 and is therefore included in the off gas G. The analysis is performed in a state in which a mist-like component is added in addition to the gas component, and the gas / liquid abundance ratio of the offgas G cannot be accurately analyzed, and the gas composition may not be accurately analyzed.

  Therefore, the present inventors connect a nozzle having a predetermined tip shape to one end side of the gas sampling line 12 and collect the off-gas G flowing through the gas mother pipe 11 in the gas sampling line 12, thereby misting the off-gas G. It has been found that the analysis result of the total gas composition including the gaseous component, the analysis result of the gas composition of the gas component excluding the mist component, and the analytical result of the gas composition of the mist component excluding the gas component can be analyzed.

  Hereinafter, a second embodiment of the present invention will be described. In the following, differences from the gas sampling device 1 according to the first embodiment described above will be mainly described, and overlapping description will be avoided.

  2 and 3 are schematic views showing an example of a gas sampling device according to the second embodiment of the present invention. As shown in FIGS. 2 and 3, the gas sampling device 2 according to the present embodiment is connected to one end side of the gas sampling line 12 in addition to the configuration of the gas sampling device 1 according to the first embodiment described above. The distal end portion 22 a includes a suction nozzle 22 disposed in the gas mother pipe 11. The suction nozzle 22 has an L-shaped tip portion 22 a in a side view, and the tip portion 22 a serving as an off-gas G suction port can be rotated around the axial direction of the suction nozzle 22 to the gas sampling line 12. It is connected. As a result, the suction nozzle 22 rotates around the axial direction, whereby the direction along the gas flow direction of the off gas G flowing in the gas mother pipe 11 (see FIG. 2) and the opposite direction to the gas flow direction of the off gas G It becomes possible to arrange the tip portion 22a facing (see FIG. 3). Since other configurations are the same as those of the gas sampling device 1 according to the first embodiment described above, description thereof is omitted.

  Next, the overall operation of the gas sampling device 2 according to the present embodiment will be described with reference to FIGS. 4A and 4B. First, as in the case of the gas sampling device 1 according to the first embodiment described above, the temperature of the thermostatic chamber of the thermostatic chamber 13 of the gas sampling device 2 was set to be equal to or higher than the temperature of the off-gas G flowing through the gas mother pipe 11. Thereafter, the tip 22 a of the suction nozzle 22 disposed in the gas mother pipe 11 is disposed in a direction opposite to the gas flow direction of the off gas G. Next, the flow rate control unit 21 sets the flow rate of the off-gas G flowing through the gas sampling line 12 to a constant velocity suction speed that substantially matches the flow rate (flow rate) of the off-gas G flowing through the gas mother pipe 11, and the flow rate control valve 17. Is adjusted to a predetermined opening, and the off-gas G flowing through the gas mother pipe 11 is drawn into the gas sampling line 12. As a result, the off-gas G flowing through the gas mother pipe 11 is drawn into the constant temperature portion 13 a of the constant temperature bath 13 through the gas sampling line 12. Here, as shown in FIG. 4A, the tip 22a of the suction nozzle 22 is arranged in a direction opposite to the gas flow direction of the off gas G, so that a mist-like component that flows along with the off gas G (insoluble) Is drawn into the suction nozzle 22 together with the off-gas G. Since the off gas G is sucked into the suction nozzle 22 at a constant suction speed that substantially matches the gas flow rate of the off gas G, an excessive mist-like component is not sucked from the peripheral side of the suction nozzle 22. Thereby, in this Embodiment, it becomes possible to analyze correctly the composition of the whole gas of the offgas G including the mist-like component accompanying the offgas G.

  Next, the suction nozzle 22 disposed in the gas mother tube 11 is rotated by 180 °, and the tip 22a is disposed along the gas flow direction of the off gas G. Next, the flow rate control unit 21 sets the flow rate of the off gas G flowing through the gas sampling line 12 to a speed slower than the constant velocity suction speed that substantially matches the flow rate (flow velocity) of the off gas G flowing through the gas mother pipe 11. The control valve 17 is adjusted to a predetermined opening, and the off gas G flowing through the gas mother pipe 11 is drawn into the gas sampling line 12. As a result, the off-gas G flowing through the gas mother pipe 11 is drawn into the constant temperature portion 13 a of the constant temperature bath 13 through the gas sampling line 12. Here, as shown in FIG. 4B, the tip 22a of the suction nozzle 22 is arranged along the gas flow direction of the offgas G, and the offgas G is sucked into the suction nozzle 22 at a flow rate slower than the gas flow rate of the offgas G. Therefore, a mist-like component (not shown) that flows along with the off-gas G in the vicinity of the tip 22a of the suction nozzle 22 is separated from the off-gas G, and only the gaseous component of the off-gas G is separated. It is sucked into the suction nozzle 22. Thereby, in this Embodiment, it becomes possible to analyze correctly the gas composition of only the gaseous component of the offgas G except the mist-like component accompanying the offgas G. Furthermore, the analysis result of the entire gas composition of the off-gas G including the mist-like component shown in FIG. 4A and the analysis result of the gas composition of only the gaseous component of the off-gas G excluding the mist-like component shown in FIG. By obtaining the difference, it is also possible to obtain an analysis result of the gas composition of only the mist-like component of the off-gas G. The flow rate slower than the gas flow rate of the off gas G is not particularly limited as long as it is a flow rate that can prevent the suction of the mist-like component from the suction nozzle 22.

  As described above, according to the present embodiment, the direction of the distal end portion 22a of the suction nozzle 22 disposed in the gas mother pipe 11 is set to the direction opposite to the gas flow direction of the off gas G and the gas flow direction of the off gas G. Since the gas composition of the off gas G is measured by switching the gas flow rate of the off gas G flowing through the gas sampling line 12, the gas composition of the off gas G including the mist component and the gas state of the off gas G are measured. It becomes possible to accurately analyze the gas composition of only the component and the gas composition of only the mist-like component of the off-gas G, respectively. As a result, it is possible to identify and grasp each component concentration contained in the gaseous component of the off-gas G and each component concentration contained in the mist-like component.

  In the above-described embodiment, the example in which the front end portion 22a of the suction nozzle 22 is directed in a direction substantially matching the direction along the gas flow direction of the off gas G has been described. As long as the composition of the gaseous component excluding the mist-like component of G can be accurately analyzed, it is not always necessary to substantially match the direction along the gas flow direction of the off-gas G. Similarly, in the above-described embodiment, the example in which the tip portion 22a of the suction nozzle 22 is directed in the direction substantially matching the opposite direction to the gas flow direction of the off gas G has been described. As long as the composition of the entire off gas G including the mist-like component of G can be accurately analyzed, it is not always necessary to substantially match the direction opposite to the gas flow direction of the off gas G.

(Third embodiment)
Next, a third embodiment of the present invention will be described. In the following, differences from the gas sampling device 2 according to the above-described second embodiment will be mainly described, and overlapping description will be avoided.

  FIG. 5 is a schematic diagram of the gas sampling device 3 according to the present embodiment. As shown in FIG. 5, the gas sampling device 3 according to the present embodiment includes a suction nozzle 22 disposed in the gas mother pipe 11 in addition to the configuration of the gas sampling device 2 according to the second embodiment described above. The nozzle drive part 31 which rotates is provided. The nozzle drive unit 31 has the tip 22a of the suction nozzle 22 centered on the axial direction of the suction nozzle 22 in the direction along the gas flow direction of the off gas G flowing in the gas mother pipe 11 and the gas flow of the off gas G. It is switched by rotating 180 ° between the opposite direction to the direction.

  In the gas sampling device 3, the gas sampling line 12 is branched into a first gas sampling line 121 and a second gas sampling line 122 after the thermostatic chamber 13. The first gas sampling line 121 includes a first control valve 32 a that controls the gas flow rate of the off-gas G flowing through the first gas sampling line 121 downstream of the thermostatic chamber 13, a first gas component absorber 141 a, and a second water absorption. The first gas component absorption unit 141 including the unit 141b, the first dehydration unit 151 including the dehydrating agent 151a, and the first gas sampling unit 161 are provided in this order. About the structure of the 1st gas component absorption part 141, the 1st dehydration part 151, and the 1st gas sampling part 161, the gas component absorption part 14, the dehydration part 15, and the gas sampling apparatus 1 which concern on 1st Embodiment mentioned above Since it is the same as that of the gas sampling unit 16, its description is omitted.

  The second gas sampling line 122 includes a second control valve 32b that controls the gas flow rate of the off-gas G flowing through the second gas sampling line 122 downstream of the thermostatic chamber 13, a first absorber 142a, and a second gas component absorber. A second gas component absorption unit 142 including 142b, a second dehydration unit 152 including a dehydrating agent 152a, and a second gas sampling unit 162 are provided in this order. About the structure of the 2nd gas component absorption part 142, the 2nd dehydration part 152, and the 2nd gas sampling part 162, the gas component absorption part 14, the dehydration part 15, and the gas sampling apparatus 1 which concern on 1st Embodiment mentioned above Since it is the same as that of the gas sampling unit 16, its description is omitted.

  Further, the gas sampling device 2 includes a control unit 33 that controls the rotation of the suction nozzle 22 by the nozzle driving unit 31 and the opening and closing of the first control valve 32a and the second control valve 32b. The control unit 33 opens the first control valve 32a when the tip 22a of the suction nozzle 22 is directed along the gas flow direction of the off gas G in the gas mother pipe 11 via the nozzle driving unit 31. The second control valve 32b is closed. Further, when the control unit 33 orients the front end portion 22a of the suction nozzle 22 via the nozzle driving unit 31 in a direction opposite to the gas flow direction of the off gas G in the gas mother pipe 11, the second control valve 32b. To close the first control valve 32a.

  That is, in the gas sampling device 2 according to the present embodiment, the gas sampling line 12 is branched at the rear stage of the thermostatic chamber 13 and the control unit 33 supplies the off gas G to the first gas according to the direction of the tip of the suction nozzle 22. The component absorption unit 141, the first dehydration unit 151, and the first gas collection unit 161, or the second gas component absorption unit 142, the second dehydration unit 152, and the second gas collection unit 162 may be separately collected. It becomes possible. Accordingly, as described in the second embodiment, the entire gas composition of the off gas G, the composition of the mist component, and the composition of the gaseous component are changed to the first gas component absorption unit 141 and the first gas sampling unit. 161, or the second gas component absorption unit 142 and the second gas sampling unit 162, respectively, can be analyzed.

  Next, the overall operation of the gas sampling device 2 according to the present embodiment will be described with reference to FIGS. 6A and 6B. As shown in FIG. 6A, first, as in the case of the gas sampling device 1 according to the first embodiment described above, the temperature of the thermostatic chamber 13 of the gas sampling device 3 is higher than the temperature of the off-gas G flowing through the gas mother pipe 11. The temperature of the thermostat is set to a predetermined temperature (for example, 120 ° C.). Next, the control unit 33 directs the distal end portion 22a of the suction nozzle 22 disposed in the gas mother pipe 11 through the nozzle driving unit 31 in a direction facing the gas flow direction of the off gas G, and then The first control valve 32a is opened and the second control valve 32b is closed.

  Subsequently, the flow control unit 21 sets the flow rate of the off gas G flowing through the gas sampling line 12 to a constant speed suction speed that substantially matches the flow rate (flow velocity) of the off gas G flowing through the gas mother pipe 11, and the flow control valve 17. Is adjusted to a predetermined opening, and the off-gas G flowing through the gas mother pipe 11 is drawn into the gas sampling line 12. As a result, after the off-gas G flowing through the gas mother pipe 11 is drawn into the thermostatic part 13a of the thermostatic chamber 13 through the gas sampling line 12, the first gas component is absorbed through the first gas sampling line 121. Collected by the unit 141, the first dehydrating unit 151, and the first gas collecting unit 161. Thereby, in this Embodiment, by analyzing each gas component absorbed and extract | collected by the 1st gas component absorption part 141, the 1st dehydration part 151, and the 1st gas extraction part 161, it is accompanied by the off gas G. It is possible to analyze the gas composition of the entire off-gas G including the mist-like component.

  Next, as shown in FIG. 6B, the control unit 33 rotates the suction nozzle 22 disposed in the gas mother pipe 11 through the nozzle driving unit 31 by 180 ° to cause the distal end portion 22 a to flow in the off-gas G gas flow direction. Then, the second control valve 32b is opened to close the first control valve 32a.

  Subsequently, the flow rate control unit 21 sets the flow rate of the off gas G flowing through the gas sampling line 12 to a speed slower than the constant velocity suction speed that substantially matches the flow rate (flow velocity) of the off gas G flowing through the gas mother pipe 11. The control valve 17 is adjusted to a predetermined opening, and the off gas G flowing through the gas mother pipe 11 is drawn into the gas sampling line 12. As a result, after the off-gas G flowing through the gas mother pipe 11 is drawn into the constant temperature portion 13a of the constant temperature bath 13 via the gas sampling line 12, the second gas component is absorbed via the second gas sampling line 122. Collected by the unit 142, the second dehydration unit 152, and the second gas collection unit 162. Thereby, in the present embodiment, each gas component absorbed and collected by the second gas component absorption unit 142, the second dehydration unit 152, and the second gas collection unit 162 is analyzed, thereby being accompanied by the off gas G. It is possible to analyze the gas composition of the entire off-gas G including the mist-like component. The difference between the analysis results of the first gas component absorption unit 141, the first dehydration unit 151, and the first gas collection unit 161 and the second gas component absorption unit 142, the second dehydration unit 152, and the second gas collection unit 162. It is also possible to obtain an analysis result of the gas composition of only the mist-like component of the off gas G.

  As described above, according to the present embodiment, the control unit 33 determines the direction of the distal end portion 22a of the suction nozzle 22 disposed in the gas mother pipe 11 as the gas flow direction of the off gas G and the gas flow of the off gas G. Since the gas composition of the off gas G is measured via the first gas sampling line 121 and the second gas sampling line 122, respectively, the total gas composition of the off gas G and the off gas G The gas composition containing only the gaseous component and the gas composition containing only the mist-like component of the off-gas G can be more easily analyzed than the second embodiment described above.

(Fourth embodiment)
Next, a fourth embodiment of the present invention will be described. In the following, differences from the gas sampling device 1 according to the first embodiment described above will be mainly described, and overlapping description will be avoided.

  FIG. 7 is a schematic diagram of the gas sampling device 4 according to the present embodiment. The gas sampling device 4 according to the present embodiment includes a heat insulating material 12a provided in the gas sampling line 12 between the gas mother pipe 11 and the thermostatic chamber 13 of the gas sampling device 1 according to the first embodiment described above. Instead, a heating unit 12b for heating the gas sampling line 12 is provided. The heating unit 12b is configured by a ribbon heater or the like, for example, and heats the gas sampling line 12 to a predetermined temperature (for example, 100 ° C.) equal to or higher than the temperature of the off-gas G flowing through the gas mother pipe 11. The heating temperature of the gas sampling line 12 by the heating unit 12 b is controlled by the temperature control unit 41. The heating of the gas sampling line 12 by the heating unit 12b does not necessarily have to be higher than the temperature of the off-gas G, and prevents condensation of gas components contained in the off-gas G and precipitation of ammonium carbonate in the gas sampling line 12. Any temperature above room temperature can be used.

  As described above, according to the present embodiment, the temperature control unit 41 controls the gas sampling line 12 between the gas mother pipe 11 and the thermostatic bath 13 to the normal temperature or higher via the heating unit 12b. It is possible to prevent the condensation and precipitation of gas components in the collection line 12, and to accurately analyze the gas composition of the offgas G.

1, 2, 3, 4 Gas sampling device 11 Gas mother pipe 12 Gas sampling line 12a Heat insulating material 12b Heating part 121 First gas sampling line 122 Second gas sampling line 13 Thermostatic chamber 14 Gas component absorption part 14a First absorption part 14b 2nd absorption part 141 1st gas component absorption part 141a 1st absorption part 141b 2nd absorption part 142 2nd gas component absorption part 142a 1st absorption part 142b 2nd absorption part 15 Dehydration part 15a Dehydrating agent 151 1st dehydration part 152 2nd dehydration part 16 Gas collection part 161 1st gas collection part 162 2nd gas collection part 17 Flow control valve 18 Flow meter 19 Suction pump 20 Heating part 21 Flow control part 22 Suction nozzle 22a Tip part 31 Nozzle drive part 32a 1st control valve 32b 2nd control valve 33 Control part G Off gas L ₁ 1st absorption liquid L ₂ 2nd absorption liquid

Claims (11)

A thermostat having a thermostat capable of heating above the gas temperature of the sampled gas;
A part of the thermostat is disposed, and a gas sampling line for sampling the sampled gas;
A flow meter that is provided in the gas sampling line in the thermostat and measures the flow rate of the sampled gas flowing through the gas sampling line;
A flow rate controller for controlling the gas flow rate of the sampled gas flowing through the gas sampling line based on the gas flow rate of the sampled gas measured by the flow meter;
A gas component absorption unit that is provided in a subsequent stage of the thermostatic chamber in the gas sampling line and absorbs a component contained in the sampled gas supplied from the gas sampling line;
A gas sampling device, comprising: a gas sampling unit that is provided at a subsequent stage of the gas component absorption unit in the gas sampling line and collects the sampled gas in which the component is absorbed by the gas component absorption unit .   The gas sampling device according to claim 1, further comprising a suction nozzle connected to the gas sampling line and having a tip disposed along a gas flow direction of the sampled gas.   The gas sampling device according to claim 2, wherein the flow rate control unit slows a gas flow rate of the sampled gas flowing through the gas sampling line with respect to a flow rate of the sampled gas.   The gas sampling device according to claim 1, further comprising a suction nozzle connected to the gas sampling line and having a tip portion disposed in a direction opposite to a gas flow direction of the sampled gas.   The gas sampling device according to claim 4, wherein the flow rate control unit makes a gas flow rate of the sampled gas flowing through the gas sampling line substantially equal to a flow rate of the sampled gas.   The nozzle drive part which switches the front-end | tip part of the said suction nozzle between the direction in alignment with the gas flow direction of the said to-be-collected gas, and the direction opposite to the gas flow direction of the to-be-collected gas is provided. The gas sampling device according to any one of 5. A first gas collection line and a second gas collection line formed by branching the gas collection line at a subsequent stage of the thermostat;
A first gas component absorption unit that is provided in a subsequent stage of the thermostatic chamber in the first gas sampling line and absorbs a component contained in the sampled gas supplied from the first gas sampling line;
A first gas sampling unit that is provided at a subsequent stage of the first gas component absorption unit in the first gas sampling line and collects the sampled gas in which the component is absorbed by the first gas component absorption unit;
A second gas component absorption part that is provided in a subsequent stage of the thermostat in the second gas sampling line and absorbs a component contained in the sampled gas supplied from the second gas sampling line;
A second gas sampling unit that is provided at a subsequent stage of the second gas component absorption unit in the second gas sampling line and collects the sampled gas in which the component has been absorbed by the second gas component absorption unit;
A control unit that controls the direction of the tip of the suction nozzle that is switched by the nozzle driving unit and that controls the switching of the flow path of the sampled gas between the first gas sampling line and the second gas sampling line The gas sampling device according to claim 6, comprising:   The gas sampling device according to any one of claims 1 to 7, wherein a heat insulating material is provided in a front stage portion of the thermostatic chamber in the gas sampling line.   The gas sampling device according to any one of claims 1 to 8, wherein a heating unit for heating the gas sampling line is provided at a front stage of the thermostatic chamber in the gas sampling line. A gas analysis method for a sampled gas using the gas sampling device according to any one of claims 1 to 9,
Analyzing the sulfuric acid that has absorbed ammonia and moisture in the sampled gas in the gas component absorption unit by ion chromatography to determine the concentration of ammonia and moisture in the sampled gas; and
The gas sampled by the gas sampling part is analyzed by gas chromatography to determine the concentration of at least one of hydrogen sulfide, carbon dioxide, nitrogen, hydrogen and methane. Analysis method.   Ethanol that has absorbed water, polar components, and organic components in the sampled gas in the gas component absorption unit is analyzed by Karl Fischer titration to determine the concentrations of water, polar components, and organic components in the sampled gas. The gas analysis method according to claim 10, comprising a step.

Images