Sample collection device and sample collection method

Abstract

To provide a sample collection device and a sample collection method capable of easily and safely collecting a hydrogen gas.SOLUTION: A sample collection device comprises a first pipeline, a pressure reduction valve installed on the first pipeline, a second pipeline, a third pipeline, a discharge part, a fourth pipeline, a first valve and a second valve. The first pipeline has: a first end which can be connected to a hydrogen supply device; and a second end. The second pipeline has: a third end which is connected to the first pipeline in the second end; and a fourth end. The third pipeline has: a fifth end which is connected to the first pipeline on the second end; and a sixth end. The discharge part has a discharge hole which may be connected to an external part of the sample collection device and the discharge part is connected to the fourth end and the sixth end. The fourth pipeline has: a seventh end which is connected to the second pipeline; and an eighth end which can be connected to a sample container. The first valve is installed on the second pipeline on a side closer to the second end side than the seventh end, and switches a state of the second pipeline between a closed state and an open state. The second valve is installed on the third pipeline, and serves as a flow rate adjusting valve of a hydrogen gas which circulates in the third pipeline.SELECTED DRAWING: Figure 1

Description

[Technical field]

[0001] The present disclosure relates to sample collection devices and methods. [Background technology]

[0002] Hydrogen stations are being developed to realize a hydrogen society. One aspect of quality control in the operation of hydrogen stations is the analysis of impurities in hydrogen gas. To perform impurity analysis, hydrogen gas needs to be collected from a hydrogen gas storage container installed at the hydrogen station into a sample container. Collection devices for extracting hydrogen gas as a sample from a hydrogen gas storage container are known. For example, Patent Document 1 describes a sample collection device for extracting high-pressure hydrogen gas of 70 MPa from a hydrogen gas storage container installed at a hydrogen station or the like, reducing the pressure to 14 MPa, and collecting the gas in a high-pressure gas cylinder.

[0003] Patent Document 2 describes a system for collecting samples of hydrogen gas stored in a hydrogen station or the like. A pressure reducing valve and a flow control valve are provided in series from the input side of the pipeline of the sample collecting device disclosed in Patent Document 2. The pressure reducing valve is capable of reducing the pressure of hydrogen gas at a temperature of -40°C and a pressure of 82 MPa to less than 1 MPa (e.g., 0.85 MPa). A flow control valve is provided downstream of the pressure reducing valve. The flow control valve controls the flow rate of the hydrogen gas reduced to less than 1 MPa by the pressure reducing valve to about 15 L / min. [Prior art documents] [Patent documents]

[0004] [Patent Document 1] JP 2016-114463 A [Patent Document 2] JP 2018-132428 A Summary of the Invention [Problem to be solved by the invention]

[0005] As described above, it is necessary to collect hydrogen gas from a high-pressure hydrogen gas storage container at a hydrogen station, etc. At this time, it is desirable that the collection of hydrogen gas from a hydrogen supply device can be easily and safely performed, and that accurate sampling can be performed without causing a difference in the components contained in the stored hydrogen gas and the collected hydrogen gas.

[0006] In light of this current situation, one of the objects of the present disclosure is to provide a sample collection device that can easily and safely collect hydrogen gas from a hydrogen gas supply device, and that can perform accurate sampling without causing differences in the components contained in the stored hydrogen gas and the collected hydrogen gas, as well as a sample collection method for collecting such hydrogen gas. [Means for solving the problem]

[0007] The sample collection device according to the present disclosure is a sample collection device for filling a sample container with hydrogen gas from a hydrogen supply device that supplies hydrogen gas. The sample collection device includes a first pipe, a pressure reducing valve installed in the first pipe, a second pipe, a third pipe, an exhaust unit, a fourth pipe, a first valve, and a second valve. The first pipe includes a first end connectable to the hydrogen supply device and a second end opposite the first end. The second pipe includes a third end connected to the first pipe at the second end and a fourth end opposite the third end. The third pipe includes a fifth end connected to the first pipe at the second end and a sixth end opposite the fifth end. The exhaust unit includes an exhaust port connectable to the outside of the sample collection device and is connected to the fourth end and the sixth end. The fourth pipe includes a seventh end connected to the second pipe and an eighth end opposite the seventh end and connectable to the sample container. The first valve is installed on the second pipe closer to the second end than the seventh end and switches the second pipe between a closed state in which the second pipe is blocked and an open state in which the second pipe is opened. The second valve is a flow rate control valve installed on the third pipe and controls the amount of hydrogen gas flowing through the third pipe.

[0008] The sample collection method according to the present disclosure is a sample collection method for collecting hydrogen gas in a sample container in a sample collection device for filling a sample container with hydrogen gas from a hydrogen supply device that supplies hydrogen gas. The sample collection device includes a first pipe, a second pipe, and a third pipe. The first pipe includes a first end connectable to the hydrogen supply device and a second end opposite the first end. The second pipe includes a third end connected to the first pipe at the second end and a fourth end opposite the third end, and is connected to an exhaust unit including an exhaust port connectable to the outside of the sample collection device at the fourth end. The third pipe includes a fifth end connected to the first pipe at the second end and a sixth end opposite the fifth end, and is connected to the exhaust unit at the sixth end. The second pipe is branched into a pipe connected to the sample container midway. The third pipe is provided with a second valve that is a flow rate adjustment valve that adjusts the amount of hydrogen gas flowing through the third pipe. The sample collection method includes a sampling step of flowing hydrogen gas into the sample container to collect hydrogen gas in the sample container, in which hydrogen gas is collected in the sample container through the second piping while a portion of the hydrogen gas flowing into the first piping from the first end is circulated through the third piping and a portion of the hydrogen gas is discharged from the discharge portion. Effect of the Invention

[0009] According to the sample collection device of the present disclosure, when sampling hydrogen gas supplied from a high-pressure storage container via a hydrogen supply device, the hydrogen gas can be collected easily and safely, and no difference in the components occurs between the stored hydrogen gas and the collected hydrogen gas, allowing for accurate sampling. Also, according to the sample collection method of the present disclosure, when sampling hydrogen gas supplied from a high-pressure storage container via a hydrogen supply device, the hydrogen gas can be collected easily and safely, and no difference in the components occurs between the stored hydrogen gas and the collected hydrogen gas, allowing for accurate sampling. [Brief description of the drawings]

[0010] [Figure 1] FIG. 1 is an explanatory diagram showing the configuration of a sample collecting device according to an embodiment of the present disclosure. [Diagram 2] FIG. 2 is a flowchart showing an outline of a sample collection method according to an embodiment of the present disclosure. [Diagram 3] FIG. 3 is an explanatory diagram showing an overview of sample analysis using the sampling device according to the embodiment of the present disclosure. [Figure 4] FIG. 4 is a diagram showing a sample collection device according to an embodiment of the present disclosure. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0011] [Outline of the embodiment] First, an overview of the sample collection device and sample collection method according to the present disclosure will be listed and described. The sample collection device according to the present disclosure is a sample collection device for filling a sample container with hydrogen gas from a hydrogen supply device that supplies hydrogen gas. The sample collection device includes a first pipe, a pressure reducing valve installed in the first pipe, a second pipe, a third pipe, an exhaust unit, a fourth pipe, a first valve, and a second valve. The first pipe includes a first end connectable to the hydrogen supply device and a second end opposite the first end. The second pipe includes a third end connected to the first pipe at the second end and a fourth end opposite the third end. The third pipe includes a fifth end connected to the first pipe at the second end and a sixth end opposite the fifth end. The exhaust unit includes an exhaust port connectable to the outside of the sample collection device and is connected to the fourth end and the sixth end. The fourth pipe includes a seventh end connected to the second pipe and an eighth end opposite the seventh end and connectable to the sample container. The first valve is installed on the second pipe closer to the second end than the seventh end and switches the second pipe between a closed state in which the second pipe is blocked and an open state in which the second pipe is opened. The second valve is a flow rate control valve installed on the third pipe and controls the amount of hydrogen gas flowing through the third pipe.

[0012] Devices for sampling hydrogen gas at hydrogen stations and the like are known. For example, Patent Document 1 discloses a portable sample collection device that maintains safety with a rupture disk and a safety valve and prevents unnecessary hydrogen gas exhaust in order to safely collect high-pressure hydrogen gas. However, the device of Patent Document 1 collects 14 MPa hydrogen gas in a high-pressure gas cylinder, which corresponds to a manufacturing act under the High Pressure Gas Safety Act and requires a qualified worker to perform the work. For this reason, the ease of collection work is not necessarily sufficient. In this regard, the sample collection device of Patent Document 2 reduces the pressure of high-pressure hydrogen gas to less than 1 MPa before sampling. In the sample collection device of Patent Document 2, sampling is performed with the flow rate of hydrogen gas flowing through the piping set to about 1 L to 10 L / min.

[0013] For hydrogen gas, 14 analysis items have been officially established for impurity analysis. Of these, there was concern that highly adsorbent components (e.g., H2O, NH3, HCHO, etc.) would be adsorbed onto the piping, and it was thought that the possibility of adsorption would increase if the flow rate of hydrogen gas flowing through the piping was slow. In addition, when a resin hose is used as part of the piping, there was concern that trace amounts of components would be desorbed from the hose and mixed into the hydrogen gas. Under these circumstances, a device was considered that could sample hydrogen gas at low pressure while suppressing concerns about the loss or mixing of impurity components and allowing for more accurate collection of hydrogen gas. As a result of repeated consideration, a device was found that has a pressure reducing valve on a first pipe having an end that can be connected to a hydrogen supply device, a pipe connected to a sample container downstream of the pressure reducing valve, and a pipe bypassing the pipe and connected to an exhaust part and equipped with a flow control valve.

[0014] This device allows sampling at low pressure, making it easy to handle and safe to collect hydrogen gas. At the same time, hydrogen gas can be collected in the sample container while a portion of the hydrogen gas flowing from the hydrogen storage container to the sample collection device is discharged. This allows sampling at low pressure while maintaining a high hydrogen gas flow rate, making it possible to sample hydrogen gas more accurately.

[0015] The sample collection device may further include a fifth pipe including a ninth end connected to the first pipe and a tenth end connected to a moisture measuring unit that measures the moisture content of the hydrogen gas. With this device, when sampling hydrogen gas, the moisture content in the hydrogen gas can be confirmed at the sampling location.

[0016] In the sample collection device, the capacity of the sample container may be 30 L or less. When the capacity of the sample container is in this range, a sample collection system can be configured that can collect an amount of hydrogen gas that allows analysis of official items, is easy to transport, and is more convenient.

[0017] In the sample collection device, the pressure of the hydrogen gas contained in the sample container may be less than 1 MPaG. When the hydrogen gas pressure is less than 1 MPaG, safety is high and the pressure falls outside the range of high-pressure gases regulated by the High Pressure Gas Safety Act, making the sample collection operation easier and also making it easier to transport the sample container after sample collection.

[0018] The sample collection method according to the present disclosure is a method for collecting hydrogen gas in a sample container in a sample collection device for filling a sample container with hydrogen gas from a hydrogen supply device that supplies hydrogen gas. The sample collection device includes a first pipe, a second pipe, and a third pipe. The first pipe includes a first end connectable to the hydrogen supply device and a second end opposite the first end, and a pressure reducing valve is installed. The second pipe includes a third end connected to the first pipe at the second end and a fourth end opposite the third end, and the fourth end is connected to an exhaust unit including an exhaust port connectable to the outside of the sample collection device. The third pipe includes a fifth end connected to the first pipe at the second end and a sixth end opposite the fifth end, and the sixth end is connected to the exhaust unit. The second pipe is branched into a pipe connected to the sample container midway. The third pipe is provided with a second valve that is a flow rate adjustment valve that adjusts the amount of hydrogen gas flowing through the third pipe. The sample collection method includes a sampling step of flowing hydrogen gas into the sample container to collect hydrogen gas in the sample container. In the sampling step, hydrogen gas is collected in the sample container through the second pipe while a portion of the hydrogen gas flowing into the first pipe from the first end is circulated through the third pipe and a portion of the hydrogen gas is discharged from the discharge portion. According to this method, hydrogen gas can be collected easily, safely, and accurately, as in the above-mentioned device. The sample collection method according to the present disclosure may be implemented in the above-mentioned sample collection device.

[0019] In the sample collection method, the flow rate of the hydrogen gas circulated through the third pipe in the sampling step may be 10 L / min to 500 L / min. By collecting the hydrogen gas while circulating the hydrogen gas through the third pipe in this range, the effects of the present disclosure can be more reliably obtained.

[0020] [Specific example of embodiment] Next, an example of a specific embodiment of the sample collection device and sample collection method according to the present disclosure will be described with reference to the drawings. In the following drawings, the same or corresponding parts are given the same reference numerals, and the description thereof will not be repeated. In this specification, the side of the sample collection device close to the hydrogen gas supply source is referred to as the "upstream side", and the side close to the exhaust port is referred to as the "downstream side". However, in actual operation, the flow direction of the gas flowing through the piping is not limited to this.

[0021] (Sampling device) FIG. 1 is an explanatory diagram showing the configuration of a sample collection system 1 including a sample collection device 10 according to an embodiment of the present disclosure. The sample collection system 1 is a system for filling a canister 52 as a sample container with hydrogen gas supplied from a hydrogen supply device. Specifically, the hydrogen supply device may be, for example, a dispenser at a hydrogen station or a filling machine at a hydrogen shipping facility. Typically, the hydrogen supply device is a device for supplying hydrogen gas as fuel to a mobile object that uses hydrogen gas, such as a fuel cell vehicle. The sample collection device 10 is used to collect hydrogen gas as an analysis sample from the hydrogen supply device in order to check the quality of hydrogen gas stored in the hydrogen supply device or for the purpose of inspecting the hydrogen supply device.

[0022] Referring to FIG. 1, the sample collection system 1 includes a sample collection device 10 and an external component 50. The sample collection device 10 is a device in which a plurality of pipes, valves, pressure gauges, flow meters, and other components are combined. The external component 50 includes a canister 52 as a sample container and a moisture meter 51. The canister 52 and the moisture meter 51 included in the external component 50 are detachably connected to the sample collection device 10 via pipes. Note that the external component 50 is not limited to the canister 52 and the moisture meter 51 shown in FIG. 1, and may include various analytical instruments and measuring instruments such as an oxygen concentration meter.

[0023] The sample collection device 10 will be described with reference to FIG. 1. The sample collection device 10 has a connection part 20 at a first end p1 that can be connected to a hydrogen supply device. Specifically, the connection part 20 is, for example, a receptacle that can be connected to a nozzle of the hydrogen supply device. A first pressure reducing valve 31 and a second pressure reducing valve 32 are provided in series on a first pipe 11 that extends from the connection part 20. The first pipe 11 is a pipe between the first end p1 and the second end p2.

[0024] The pressure of the hydrogen gas supplied from the hydrogen supply device is not particularly limited, but may be, for example, about 50 MPaG to 82 MPaG, and is typically, for example, 82 MPaG. The first pressure reducing valve 31 reduces the pressure of the hydrogen gas of 82 MPaG to 0.8 MPaG. The second pressure reducing valve 32 is a pressure gauge-equipped pressure reducing valve having two pressure gauges 21 and 22. The second pressure reducing valve 32 reduces the pressure of the hydrogen gas of 0.8 MPaG to a maximum of 0.6 MPaG, specifically, for example, 0.27 MPaG. The outlet side pressure of the second pressure reducing valve 32, that is, the pressure measured by the pressure gauge 22, may be 0 MPaG or more and 0.6 MPaG or less. In the sample collecting device 10, the pressure of the hydrogen gas is reduced to 0.6 MPaG or less by the two pressure reducing valves, that is, the first pressure reducing valve 31 and the second pressure reducing valve 32. The sample collecting device 10 is a device that collects hydrogen gas under conditions that do not fall under the requirements for high-pressure gas production in the High Pressure Gas Safety Act.

[0025] A third end p3, which is one of both ends of the second pipe 12, is connected to the second end p2 of the first pipe 11. A fourth pipe 14, which is a pipe connected to a canister 52, branches off from the second pipe 12. Although the sample collection device 10 shown in FIG. 1 is configured to be connectable to two canisters, the number of canisters that can be connected to the sample collection device according to the present disclosure may be one, or three or more. A fourth end p4, which is the end opposite the third end p3, of both ends of the second pipe 12, is connected to a discharge section 19.

[0026] Further, a fifth end p5, which is one of both ends of the third pipe 13, is connected to the second end p2 of the first pipe 11. A sixth end p6, which is the end of the third pipe 13 opposite to the fifth end p5, is connected to the discharge section 19. That is, the second pipe 12 and the third pipe 13 are pipes provided in parallel with each other. Being in parallel with each other means that a pipeline is formed between the first pipe 11 and the discharge section 19 that passes through the second pipe 12 without passing through the third pipe 13, and that a pipeline is formed that passes through the third pipe 13 without passing through the second pipe 12. That is, the third pipe 13 functions as a bypass pipe for the second pipe 12.

[0027] The sample collecting device 10 includes an outlet 29 that discharges the hydrogen gas supplied to the sample collecting device 10 to the outside of the sample collecting device 10. The outlet 29 is a part that can be connected to the outside of the sample collecting device 10. The outlet 29 is provided with a connection part such as a quick connector, and a discharge line can be connected to the outlet 29.

[0028] The fourth pipe 14 is connected to the second pipe 12 at a seventh end p7, which is one of the two ends. An eighth end p8, which is the end opposite to the seventh end p7, preferably has a connector that can be connected to the canister 52 with one touch. A part of the fourth pipe 14 may be composed of a flexible hose. The sample collection device 10 includes two fourth pipes 14. Both of the two fourth pipes 14 branch off from the second pipe 12 and are installed in parallel with each other.

[0029] The second pipe 12 is provided with a valve 33 as a first valve that switches the second pipe 12 between a closed state where the second pipe 12 is blocked and an open state where the second pipe 12 is opened. The valve 33 is provided on the second end p2 side of the seventh end p7, in other words, upstream of the branching portion of the fourth pipe 14 in the second pipe 12. The valve 33 is, for example, a manual gate valve that can be manually opened and closed. In addition, a valve 37 and a check valve 38 are provided on the second pipe 12 on the fourth end p4 side of the seventh end p7, that is, downstream of the branching portion of the fourth pipe 14 in the second pipe 12. In addition, a flow meter (not shown) is provided between the valve 37 and the check valve 38.

[0030] The third pipe 13 is provided with a valve 34 which is a flow rate control valve serving as a second valve for adjusting the amount of hydrogen gas flowing through the third pipe 13. A flow meter 25 is provided on the third pipe 13. By adjusting the opening of the valve 34 while checking the flow meter 25, a predetermined amount of hydrogen gas can be caused to flow through the third pipe 13 and be discharged from the exhaust port 29.

[0031] In the sample collection device 10, the second pipe 12 and the third pipe 13 are provided in parallel. With this configuration, hydrogen gas can be collected into the canister 52 through the second pipe 12 while a portion of the hydrogen gas supplied from the hydrogen supply device through the first pipe 11 is discharged from the third pipe 13. For example, the amount of gas flowing through the third pipe 13 can be 10 L / min or more and 500 L / min or less, and in order to ensure the bypass purge effect, it is preferably 50 L / min or more and 500 L / min or less. This allows sampling to be performed while maintaining a high gas flow rate during sampling of hydrogen gas.

[0032] Generally, when filling a fuel cell vehicle (FCV) with hydrogen gas, it is set so that 5 kg can be filled in 3 minutes, so the flow rate of hydrogen gas during filling is extremely fast. In this regard, according to the sample collection device 10, by performing sampling while discharging a portion of the hydrogen gas from the third pipe 13, which is a bypass route, it is possible to collect hydrogen gas at a high gas flow rate. In other words, it is possible to collect hydrogen gas as a sample under conditions similar to those when hydrogen gas is filled into a vehicle. This reduces the possibility that the impurity concentration will differ between the hydrogen gas filled into the vehicle and the sampled hydrogen gas.

[0033] The sample collecting device 10 includes a fifth pipe 15 that can be connected to a moisture meter 51 that is a moisture measuring unit. The fifth pipe 15 is connected to the first pipe 11 at a ninth end p9, which is one of both ends. The tenth end p10, which is the end opposite to the ninth end p9, preferably has a connector that can be connected to the moisture meter 51 with one touch. The outlet side of the moisture meter 51 is connected to the discharge unit 19 via the sixth pipe 16. The moisture meter 51 may be, for example, a capacitance moisture meter. The moisture meter is not limited to the capacitance type, and may be a CRDS (cavity ring down spectroscopy) moisture meter, a quartz crystal oscillation moisture meter, a mirror dew point meter, or the like. A valve 41 that opens and closes the pipe as necessary is provided midway through the fifth pipe 15. A valve 42 that opens and closes the pipe as necessary is provided midway through the sixth pipe 16. The valves 41 and 42 may be, for example, gate valves that can be opened and closed manually. Further, a check valve 43 is provided midway along the sixth pipe 16 .

[0034] 1, the moisture meter 51 is connected to the sample collection device 10, but the moisture meter 51 is not an essential component, and there are cases where the moisture meter 51 is not attached. Also, instead of the moisture meter 51, another component analysis device, specifically, for example, an oxygen meter, may be connected to measure the oxygen concentration in the hydrogen gas.

[0035] The sample collection device 10 is provided with pressure release valves 39, 40 as safety devices. The set pressure of the pressure release valve 39 is 0.99 MPaG. The pressure release valve 39 is subjected to the pressure in the piping between the first pressure reducing valve 31 and the second pressure reducing valve 32 in the first piping 11. The set pressure of the pressure release valve 40 is 0.6 MPaG. The pressure release valve 40 is connected to the second piping 12 and is subjected to the pressure in the second piping 12. In addition, the pressure release valve 39 and the pressure release valve 40 are connected. By providing the pressure release valves 39, 40, it is possible to prevent the pressure in the piping from unintentionally rising to or exceeding the set pressure.

[0036] A seventh pipe 17 branches off from the first pipe 11 between the first pressure reducing valve 31 and the second pressure reducing valve 32. A sampling device or the like can be connected to the seventh pipe 17 as required. A valve 44, which is a gate valve that opens and closes the pipe as required, is provided midway along the seventh pipe 17.

[0037] The capacity of the canister 52 connected to the sample collection device 10 is not particularly limited, but is, for example, 30 liters or less, preferably 15 liters or less, and more preferably 6 liters or less. A container with a capacity of 30 liters or less is excellent in portability. In particular, a container with a capacity of 6 liters or less is easy to carry in a hand carry and is particularly easy to handle.

[0038] The canister 52 does not need to be a high-pressure gas container. The pressure of the hydrogen gas stored in the canister 52 is less than 1 MPaG. The canister 52 may be, for example, a container with a pressure resistance of 0.6 MPaG or less, and is preferably a container with a pressure resistance of 0.27 MPaG or less.

[0039] The material of the canister may be, for example, stainless steel, and a stainless steel container with polished inner surface is preferable. It is known that when there are points on the surface of stainless steel that have localized positive and negative charges, called active sites, polar components are adsorbed, which makes the concentration more likely to decrease. For this reason, by using a container that has been subjected to an inert treatment (SiO2 coating, etc.), the concentration decrease of sulfur-based components (COS, H2S, etc.) and volatile organic compounds (VOCs) in particular can be suppressed. For example, a commercially available product developed for measuring VOC components in the air can be used as the canister.

[0040] A demonstration experiment was carried out using the sampling device according to the present disclosure to collect hydrogen gas in a canister that had been deactivated. Hydrogen gas containing polar components NH3, HCOOH, HCHO, HCL, and sulfur compounds (COS, etc.) at concentrations close to the standard values ​​stipulated in ISO14687 Grade-D was created and filled into a canister. The attenuation of the concentration of each component after filling was investigated. When a canister that had not been deactivated was used, the concentration of sulfur compounds (COS being the representative) was almost zero immediately after filling, whereas in the canister that had been deactivated, there was almost no attenuation even after one week had passed. Although the concentrations of NH3, HCOOH, HCHO, and HCL could not be completely maintained, when a canister that had been deactivated was used, the concentrations were maintained at about 30 to 70% of the concentrations at the time of filling even after one week had passed. In addition, within three days, the concentrations of all components NH3, HCOOH, HCHO, HCL, and COS were maintained at 50% or more of the concentrations at the time of filling.

[0041] (Sample collection method) The sample collection method according to the present disclosure is a method for collecting hydrogen gas in a sample container in a sample collection device that collects hydrogen gas from a hydrogen supply device into a sample container. The method according to the present disclosure includes a sampling step of flowing hydrogen gas into the sample container to collect hydrogen gas in the sample container. In this sampling step, hydrogen gas is collected in the sample container while a portion of the hydrogen gas flowing into the sample collection device is discharged from a bypass piping.

[0042] Although the device in which the sample collection method according to the present disclosure is carried out is not limited, it is typically preferably carried out in the above-mentioned sample collection device. Fig. 2 is a flow chart showing an outline of the sample collection method according to the present disclosure. In the following, the collection method shown in Fig. 2 will be explained with partial reference to the device shown in Fig. 1. In addition, in the following explanation, the characteristic configuration of the sample collection method according to the present disclosure will be mainly explained, and the operation on the hydrogen supply device (hydrogen station) side and the procedures performed for safety will be omitted as appropriate.

[0043] Referring to FIG. 2, sample collection is started (S0). In the start step, the work contents and procedures are confirmed. Next, the apparatus is prepared (S10). Specifically, as the preparation step, the sample collection apparatus is installed next to the hydrogen supply apparatus, and the sample collection apparatus (sample collection apparatus 10) and two canisters (canister 52) are connected to each other via flexible hoses (fourth pipe 14). In addition, a moisture meter (moisture meter 51) is connected to the sample collection apparatus. A purge line (sixth pipe 16) is also connected to the moisture meter. In addition, a vent line is connected to the exhaust port (exhaust port 29) of the sample collection apparatus. The two pressure reducing valves (first pressure reducing valve 31, second pressure reducing valve 32) are closed. All six valves of the sample collection apparatus (corresponding to valves 41, 33, 34, 44, 37, 42) are fully closed. After that, the nozzle of the hydrogen supply apparatus is connected to the receptacle (connection part 20) of the sample collection apparatus. The pressure is slowly increased from the pressure accumulator at the hydrogen station to the nozzle of the hydrogen supply device until the pressure is the same.

[0044] Next, a leak check is performed (S20). Specifically, the pressure reducing valve (first pressure reducing valve 31) is adjusted so that the pressure on the primary side pressure gauge (pressure gauge 21) is set to 0.8 MPaG. In addition, the pressure reducing valve (second pressure reducing valve 32) is adjusted so that the pressure on the secondary side pressure gauge (pressure gauge 22) is set to 0.27 MPa. Next, the valve 33 of the second pipe 12 is opened, and all of the joints are checked for leaks. If a leak is detected (NG in S20), leak countermeasures are taken (S21), and a leak check is performed again (S20).

[0045] If it is confirmed that there is no leak (OK in S20), piping purging is performed (S30). In piping purging, the inside of the collection device is purged with hydrogen gas using the first pressure reducing valve 31 and the valve 37 in the second piping 12. For example, purging is repeated 10 times to replace the inside of the piping of the collection device with hydrogen gas. In addition, the flow rate control valve (valve 34) of the third piping 13, which is the bypass piping, is adjusted to set the bypass flow rate to 200 L / min. A leak check is performed on the joints downstream of the valve 34 and the vent line. The hydrogen gas flow rate in the third piping 13 is maintained at 200 L / min for a predetermined time (for example, about 5 minutes), and the inside of the third piping 13 is purged with hydrogen gas. The following steps are performed while maintaining a state in which hydrogen gas is circulated at 200 L / min through the third piping 13, which is the bypass piping, and discharged from the vent line.

[0046] Next, moisture measurement is performed (S40). Specifically, valve 42 is fully opened, and valve 41 is adjusted to a predetermined hydrogen gas flow rate (e.g., 1 L / min). Next, moisture meter 51 is powered ON and measurement is performed. After measurement under the predetermined conditions, moisture meter 51 is powered OFF, valve 41 is fully closed, and then valve 42 is also fully closed. Moisture meter 51 is removed.

[0047] Next, the sample container (canister 52) is purged (S50). Specifically, first, it is confirmed that the outlet side of the first pressure reducing valve 31 is 0.8 MPaG, and the outlet side of the second pressure reducing valve 32 is 0.27 MPa. It is also confirmed that the valves 41, 33, 44, and 37 are closed, and the valve 34, which is a flow rate control valve, is adjusted open (hydrogen gas flow rate 200 L / min). Next, the valve 35 of the canister 52 is fully opened, and the valve 37 is opened to release the gas in the canister. After the gas in the canister is released, the valve 37 is closed. Next, the inside of the canister 52 is purged with hydrogen gas by opening and closing the valves 33 and 37. The purging conditions are, for example, a state in which the pressure in the canister 52 is 0.27 MPaG (upper limit of the canister's withstand pressure) and a state in which it is 0 MPaG (atmospheric pressure) are repeated a predetermined number of times (for example, 15 times).

[0048] Next, hydrogen gas is collected (S60). Specifically, after the above-mentioned purging is completed, valve 37 is closed, valve 33 is opened, and 0.27 MPaG of hydrogen gas is collected in canister 52. During collection, the collected pressure is confirmed with pressure gauge 23. Note that even during collection, hydrogen gas is circulated at 200 L / min through bypass piping (third piping 13) to maintain a state in which it is discharged from the vent line. After collection, valve 35 of canister 52 is closed. First pressure reducing valve 31 is closed, and valve 37 is opened to release hydrogen from the device. Thereafter, second pressure reducing valve 32 is closed, and all valves are fully closed. The hydrogen supply device is depressurized.

[0049] Next, the removal work is carried out (S70). Specifically, the nozzle and vent line connected to the sampling device are removed. Also, the canister is removed from the sampling device. After recording the necessary items and carrying out maintenance, the work is completed (S80).

[0050] FIG. 3 is an explanatory diagram showing an overview of sample analysis using a sample collection device according to the present disclosure. With reference to FIG. 3, samples are collected at a hydrogen station 100. Hydrogen gas is collected into a canister 152 from a filling nozzle 201 of a hydrogen supply device 200 at the hydrogen station 100. The moisture content of the hydrogen gas is measured using a moisture meter 151. The collected hydrogen gas is transported and taken to an analysis institution 90. Note that the hydrogen gas filled in the sample container 152 does not fall under the category of high-pressure gas, and can also be transported by route bus.

[0051] The analysis system in the analysis facility 90 includes a sample / standard gas dilution unit 91, a pretreatment unit 92, and a detector unit 93. In the sample / standard gas dilution unit 91, hydrogen gas, which is the sample, is taken out from a canister 152 and diluted as necessary. Also, a standard gas 155 is supplied and diluted as necessary. The sample processed in the sample / standard gas dilution unit 91 is transferred to the pretreatment unit 92. At this time, the sample is passed through a methanizer 95 depending on the analysis item.

[0052] The pretreatment section 92 includes a separation treatment section 96 including a gas chromatography device and a cooling section (cold trap). The sample pretreated in the separation treatment section 96 is transferred to the detector section 93. The detector section 93 is analyzed by an analyzer 97 including a TOF-MS (time-of-flight mass spectrometer). It is preferable that the combination of the sample and standard gas dilution unit 91, the pretreatment section 92, and the detector section 93 collectively analyzes 13 components, excluding water, out of 14 components to be analyzed in hydrogen gas.

[0053] FIG. 4 is a diagram showing a sample collection device according to an embodiment of the present disclosure. Referring to FIG. 4, the sample collection device 210 is a device for collecting hydrogen gas in two canisters 252. The sample collection device 210 has the same piping configuration as the above-mentioned sample collection device 10, so a description of the piping will be omitted. The sample collection device 210 accommodates piping, valves, pressure gauges, and flow meters in a space surrounded by an aluminum frame 250. The frame 250 is 280 mm wide, 450 mm deep, and 260 mm high. The diameter of the piping is 1 / 4 inch (outer diameter 13.8 mm) or 3 / 8 inch (outer diameter 17.3 mm). Specifically, for example, EP (electrolytic polishing) piping made of SUS316L is used as the piping. The material of the piping is not limited as long as it is a material resistant to hydrogen, and may be, for example, a BA (bright annealing) pipe or EP pipe made of SUS304 or SUS316. The sample collecting device 210 and the canister 252 are connected via a flexible pipe 214 .

[0054] The sample collection device according to the present disclosure is a small device configured with the above-mentioned dimensions, and can be easily carried, for example, in a carry case, etc. Of course, the specific configuration and dimensions of the sample collection device according to the present disclosure are not limited to those described above, and the example in Figure 4 is merely one example.

[0055] The embodiments disclosed herein are illustrative in all respects and should not be construed as limiting. The scope of the present invention is defined by the claims, not the above description, and is intended to include all modifications within the scope and meaning equivalent to the claims. [Explanation of symbols]

[0056] 1 Sampling system, 10, 210 Sampling device, 11 First pipe, 12 Second pipe, 13 Third pipe, 14 Fourth pipe, 15 Fifth pipe, 16 Sixth pipe, 17 Seventh pipe, 19 Discharge section, 20 Connection section, 21, 22, 23 Pressure gauge, 25 Flow meter, 29 Discharge port, 31 First pressure reducing valve, 32 Second pressure reducing valve, 33, 34, 37, 41, 42, 44 Valve, 35 Valve, 38, 43 Check valve, 39, 40 Pressure release valve, 50 External component, 51, 151 Moisture meter, 52, 152, 252 Canister, 90 Analysis engine, 91 Sample and standard gas dilution unit, 92 Pretreatment section, 93 Detector section, 95 Methanizer, 96 Separation treatment section, 97 Analyzer, 100 Hydrogen station, 200 Hydrogen supply device, 201 filling nozzle, 214 flexible piping, 250 frame.

Claims

1. A sample collection device for filling a sample container with hydrogen gas from a hydrogen supply device that supplies hydrogen gas, comprising: a first pipe including a first end connectable to the hydrogen supply device and a second end opposite to the first end; A pressure reducing valve installed in the first pipe; a second pipe including a third end connected to the first pipe at the second end and a fourth end opposite the third end; a third pipe including a fifth end connected to the first pipe at the second end and a sixth end opposite the fifth end; a discharge section including a discharge port connectable to the outside of the sample collecting device and connected to the fourth end and the sixth end; a fourth pipe including a seventh end connected to the second pipe and an eighth end opposite the seventh end and connectable to the sample container; a first valve that is installed on the second pipe on the second end side relative to the seventh end and switches the second pipe between a closed state in which the second pipe is blocked and an open state in which the second pipe is opened; a second valve that is installed in the third piping and is a flow rate regulating valve that regulates the amount of hydrogen gas flowing through the third piping.

2. 2. The sample collecting device of claim 1, further comprising a fifth pipe including a ninth end connected to the first pipe and a tenth end connected to a moisture measuring unit that measures a moisture content of hydrogen gas.

3. 2. The sample collection device of claim 1, wherein the volume of the sample container is 30 liters or less.

4. 2. The sample collecting device according to claim 1, wherein the pressure of the hydrogen gas contained in the sample vessel is less than 1 MPaG.

5. 1. A method for collecting hydrogen gas in a sample container in a sample collection device for filling a sample container with hydrogen gas from a hydrogen supply device that supplies hydrogen gas, comprising: The sample collection device includes: a first pipe including a first end connectable to the hydrogen supply device and a second end opposite to the first end, the first pipe including a pressure reducing valve; a second pipe including a third end connected to the first pipe at the second end and a fourth end opposite to the third end, the second pipe being connected at the fourth end to a discharge section including a discharge port connectable to the outside of the sampling device; a third pipe including a fifth end connected to the first pipe at the second end and a sixth end opposite to the fifth end, the third pipe being connected to the discharge port at the sixth end; Including, The second pipe is branched into a pipe connected to the sample container midway, the third pipe is provided with a second valve which is a flow rate control valve that adjusts the amount of hydrogen gas flowing through the third pipe; The method for collecting samples comprises: A sampling step of sampling hydrogen gas into the sample container by flowing hydrogen gas into the sample container, In the sampling step, a portion of the hydrogen gas flowing into the first piping from the first end is caused to flow through the third piping, and a portion of the hydrogen gas is discharged from the discharge portion, while the hydrogen gas is collected in the sample container through the second piping. Sampling methods.

6. In the sampling step, the flow rate of the hydrogen gas flowing through the third pipe is 10 L / min or more and 500 L / min or less.

6. The method of claim 5.

7. 1. A method for collecting hydrogen gas in a sample container in a sample collection device for filling a sample container with hydrogen gas from a hydrogen supply device that supplies hydrogen gas, comprising: The sample collection device is a sample collection device according to any one of claims 1 to 4, The method for collecting samples comprises: A sampling step of sampling hydrogen gas into the sample container by flowing hydrogen gas into the sample container, In the sampling step, a portion of the hydrogen gas flowing into the first piping from the first end is caused to flow through the third piping, and a portion of the hydrogen gas is discharged from the discharge portion, while the hydrogen gas is collected in the sample container through the second piping. Sampling methods.

Images