JP2009000005A - Method and apparatus for pressure testing - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method and an apparatus for pressure testing, in which size can be increased and gas concentration in a raw material solution can be regulated to measure gas generation. <P>SOLUTION: The apparatus for pressure testing is constituted of a raw material vessel 1 equipped with a movable-type solid piston 3 installed in a hermetically closed cylinder 1c, a reaction vessel 2 for communicating with a stock solution part 1b of the raw material vessel 1 and receiving a stock solution 102, and a pressurizing pump 6 for feeding pressurizing water to a stock solution part 1a of the raw material vessel 1. The method for pressure testing is constituted of: feeding pressurized water from the pressurizing pump 6 to a pressurizing part 1a; increasing the pressure of the stock solution part 1b to a pressure not lower than the atmospheric pressure by movement of the solid piston 3; maintaining even the pressure of the reaction vessel 2, in such a state that the pressure is increased to a pressure not lower than the atmospheric pressure; carrying out a reaction, such as a microbiological reaction in the reaction vessel 2; intermittently removing the solution in the reaction vessel 2; simultaneously feeding the pressurizing water 101 from the pressurizing pump 6 so as to maintain the pressure of the reaction vessel 2 and the stock solution part 1b; and moving the piston 3 and maintaining the pressure of the reaction vessel 2, while extruding the stock solution 102 in the stock solution part 1a into the reaction vessel 2. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention relates to a pressure test method and apparatus for testing chemical reactions and microbial reactions under pressure such as geochemistry and oceanography.

  In the field of investigating phenomena such as microorganisms in the deep sea and deep layers, and testing the layers of final disposal sites where radioactive waste is stored, tests that examine chemical reactions and microbial reactions under pressure are important.

  In this test, microorganisms collected in the deep sea and deep layers need to be cultured in the same environment as in the deep sea. It was difficult and it was inevitably a batch test.

  However, in a batch test, if the test period is long, the raw material of the reaction (substrate in the case of microbial reaction) is depleted and the reaction cannot be continued for a long time. On the other hand, if the concentration is increased from the beginning so that the raw material is not depleted, It becomes a condition.

  In order to solve this problem, an apparatus for continuously supplying raw materials has been developed. A typical example is the apparatus of Non-Patent Document 1. In this method, the raw material is sent to a pressurized microbial reaction tank with a pump having a titanium pump head, but the pump is very expensive.

  In order to solve this problem, Patent Document 1 communicates a raw material container with a culture vessel for performing a microbial reaction, and provides a diaphragm in the raw material container, and pushes a pressure medium on the opposite side of the diaphragm with a syringe pump, thereby content of the raw material solution. By changing the product, the raw material solution is fed into the culture tank without using an expensive pump, while the liquid is extracted from the culture tank, enabling continuous testing.

  Note that Patent Document 2 is similar to Patent Document 1, and Patent Document 3 is similar to Non-Patent Document 1.

JP 2001-258545 A US Pat. No. 5,248,300 Japanese Patent Publication No. 7-8227 Jannasch et a1. (1996) Appl. Env Microbio1., Vol.62, N0.5: 1593-1596, American Society of Microbiology.

  By the way, in Patent Document 1, a diaphragm is used as means for making the internal volume of the raw material solution variable. However, there is a problem of strength and it is difficult to increase the size structurally. Moreover, in patent document 1, after enclosing a raw material solution, adjustment of the gas concentration in a raw material solution and measurement of gas generation cannot be performed, but there exists a problem which cannot take the gas material balance.

  Accordingly, an object of the present invention is to provide a pressure test method and apparatus that can solve the above-mentioned problems, can be enlarged, and can adjust the gas concentration in the raw material solution and measure the gas generation.

  In order to achieve the above object, according to the first aspect of the present invention, a movable solid piston is provided in a sealed cylinder of a raw material container, and the sealed cylinder is divided into a pressurizing section and a stock section for storing a stock solution for reaction. Divide and communicate with the reaction tank that receives the stock solution from the stock solution part of the raw material container, send the pressurization water from the pressurization pump to the pressurization part of the raw material container, and move the solid piston to the pressure of the stock solution part to atmospheric pressure In addition to increasing the pressure in the reaction tank, the reaction tank is maintained at a pressure higher than atmospheric pressure to cause a reaction such as a microbial reaction in the reaction tank, and the liquid in the reaction tank is withdrawn intermittently. A pressurization test method characterized by maintaining the pressure in the reaction tank while sending the pressure water from the pressure pump to maintain the pressure in the stock solution and moving the piston to push the stock solution in the stock solution into the reaction tank. is there.

  The invention of claim 2 starts the pressurization of the stock solution part after injecting a gas into a part of the stock solution part, dissolves the gas in the stock solution, and then supplies the stock solution having an increased dissolved gas concentration to the reaction tank It is a pressurization test method of Claim 1 made to do.

  Invention of Claim 3 is a pressurization test method of Claim 1 or 2 with which a raw material container is accommodated in refrigeration equipment and the temperature of a stock solution part is controlled.

  According to a fourth aspect of the present invention, a liquid containing microorganisms is injected into the reaction tank, and a nutrient salt for growing microorganisms is added to the raw liquid in the raw liquid part, and the microbial reaction is performed in the reaction tank. 3. The pressure test method according to any one of 3 above.

  In the invention of claim 5, a discharge line is connected to the reaction tank, and two valves are connected to the discharge line, and the valve is opened and closed to sample the liquid while maintaining the pressure in the reaction tank. It is a pressurization test method in any one of Claims 1-4.

  According to a sixth aspect of the present invention, there is provided a raw material container in which a movable solid piston is provided in a sealed cylinder, and the sealed cylinder is divided into a pressurizing unit and a stock solution part for containing a stock solution for reaction, A pressurizing pump that sends pressurized water to the stock solution part to increase the pressure of the stock solution part to atmospheric pressure, a transfer line that transports the stock solution part of the raw material container, and a transfer line connected to the stock solution part of the raw material container. It is a pressure test apparatus characterized by comprising a reaction vessel that accepts microorganisms in a high-pressure state and reacts with microorganisms, and a discharge line that intermittently extracts a liquid that has undergone microbial reaction in the reaction vessel.

  A seventh aspect of the present invention is the pressure test apparatus according to the sixth aspect, wherein the raw material container is accommodated in the refrigeration facility.

  The invention according to claim 8 is the pressure test apparatus according to claim 6 or 7, wherein a filter or a check valve is connected to the transfer line.

  In the invention of claim 9, an injection line for injecting a liquid containing microorganisms is connected to the reaction tank, and a raw material injection line for injecting nutrient salts for growing microorganisms into the stock solution is connected to the stock solution part. The pressure test apparatus according to any one of Items 6 to 8.

  According to a tenth aspect of the present invention, a discharge line is connected to the reaction tank, and two valves for sampling the liquid while maintaining the pressure in the reaction tank are connected to the discharge line. The pressure test apparatus according to any one of the above.

  The present invention pressurizes the stock solution part of the raw material container using a movable piston made of solid such as metal, plastic, etc., so that the piston can move almost from end to end in the cylindrical raw material container. A large-capacity raw material solution is held on one side, and the raw material solution can be sent to the reaction vessel by movement of the piston in the cylinder. That is, the overall apparatus can be increased in size. Moreover, since the raw material container can be enlarged, a predetermined amount of gas can be filled and pressurized in a part thereof, and the gas concentration of the raw material solution can be adjusted. Furthermore, not only liquid but also gas can be collected from the discharge line of the reaction tank.

  Thus, the present invention enables the following tests that cannot be performed with the prior art.

  For example, when a sample amount of a certain amount or more is required for water quality analysis accompanying the reaction, the raw material container and the reaction vessel can be enlarged to increase the sample amount at one time. In groundwater tests, the concentration of dissolved gas is often high and the gas concentration cannot often be obtained at atmospheric pressure. However, if the present invention is used, the gas concentration can be matched with the actual state. Furthermore, by analyzing the amount and composition of the gas taken in the plastic sample container at the time of sampling, the gas material balance can be taken, for example, the methane generation rate can be known.

  A preferred embodiment of the present invention will be described below in detail with reference to the accompanying drawings.

  FIG. 1 shows a first embodiment of the present invention, and the basic configuration is composed of two sealed pressure-resistant containers, that is, a raw material container 1 and a reaction tank 2.

  The raw material container 1 is composed of a sealed cylinder 1c whose upper and lower cylinders are closed, and is provided with a slidable solid piston 3 that is divided into a pressurizing part 1a and a raw liquid part 1b.

  The piston 3 is in contact with the inner wall of the sealed cylinder 1c, and can move within the range of the lower stopper 4a and the upper stopper 4b.

  Connected to the pressurizing section 1a are a pressurized water inflow line 8 for feeding the pressurizing water 101 in the pressurizing water tank 5 and a pressurized water circulation line 11 for returning the pressurizing 101 water in the pressurizing section 1a to the pressurizing water tank 5. .

  A pressurizing pump 6 that pressurizes the pressurizing water 101 from the pressurizing water tank 5 is connected to the pressurizing water inflow line 8, and a pressurized water inflow valve 7 is connected to the downstream side thereof.

A pressurized water circulation valve 9 and a pressure adjustment valve 10 are connected to the pressurized water circulation line 11. A pressurized water pressure gauge 12 is connected by a branch pipe between the pressurized water circulation valve 9 and the pressure adjusting valve 10 on the pressurized water circulation line 11. The raw solution 102 is injected into the raw solution part 1 b of the raw material container 1. The raw material injection line 14 to be transferred and the transfer line 16 for transferring the raw solution 102 of the raw material container 1 to the reaction tank 2 are connected.

  A raw material injection valve 13 is connected to the raw material injection line 14, and the raw material 102 can be supplied to the raw material injection line 14 through the raw material injection valve 13. In the case of performing a microbial reaction test, the raw material 102 contains a nutrient salt for growing the microorganism.

  A transfer valve 15 is connected to the transfer line 16, and a filter (filter) or a check valve 17 is connected to the downstream side as necessary.

  The raw material container 1 is housed in the refrigeration facility 18 and controlled so that the temperature of the raw material container 1 becomes an appropriate temperature as required.

  A discharge line 21 for discharging the liquid 110 in the reaction tank 2 is connected to the upper part of the reaction tank 2, and an injection line 27 for the test material 103 is connected to the discharge line 21.

  A discharge valve 19 and a sampling valve 20 are connected to the discharge line 21. The discharge valve 19 and the sampling valve 20 may be manual valves or automatic valves such as electromagnetic valves.

  A pressure gauge 22 is connected to a discharge line 21 between the discharge valve 19 and the sampling valve 20 via a branch pipe, and a sampling container 30 for sampling a predetermined amount of the liquid 110 in the reaction tank 2 is connected appropriately. .

  The injection line 27 is provided with an injection part 24 for injecting the test material 103 into the injection line 27 and connected to the injection valve 23.

  The reaction tank 2 is provided with a stirring facility 25 such as a magnetic stirrer as necessary. Moreover, the reaction tank 2 is accommodated in the thermostat 26 as needed.

  Next, the operation of the present invention will be described.

  First, in a state where the piston 3 of the raw material container 1 is located at the lowest position, which is located on the lower stopper 4a, the pressurizing water 101 is put into the pressurizing part 1a of the raw material container 1 from the pressurizing water tank 5 by the pressurizing pump 6. Then, the pressurized water inflow valve 7 and the pressurized water circulation valve 9 are closed. The pressurizing water 101 may be tap water, or pure water, a reducing agent, or sterilization according to the test application.

  Next, the test stock solution 102 is introduced from the raw material injection line 14 into the stock solution portion 1 b of the raw material container 1. At this time, the transfer valve 15 and the injection valve 23 of the reaction tank 2 are opened, and the stock solution 102 enters the reaction tank 2 as it is, and it is confirmed that the injection port 24 of the reaction tank 2 is full. (First method).

  Alternatively, after dividing the transfer line 16 on the reaction tank 2 side of the transfer valve 15, etc., the test stock solution 102 is put into the stock solution part 1 b from the raw material injection line 14, and the transfer valve 15 overflows from the transfer valve 15. 15 and the material injection valve 13 are closed. Next, the stock solution 102 is introduced from the reaction vessel inlet 24 with the discharge valve 19 and the sampling valve 20 opened. When the stock solution becomes full, the discharge valve 19, the sampling valve 20 and the injection valve 23 are closed, and the raw material container 1 and the reaction vessel 2 are closed. Are combined again in the transfer line 16 (second method).

  After the stock solution 102 is put into the stock solution part 1b, the raw material container 1 and the reaction tank 2 can be sterilized as they are or in the middle of the transfer line. The stock solution 102 is a culture solution if the test deals with microbial reactions.

  Next, the test material 103 is introduced from the reaction vessel inlet 24. The test material 103 is a microorganism if the test deals with a microbial reaction.

  The preparation is completed and the test is started. At the start of the test, the pressurized water inflow valve 7, the pressurized water circulation valve 9, the pressure regulating valve 10 and the transfer valve 15 are opened, and the other valves 13, 19, 20, 23 are opened. Is closed.

  In this state, the pressure pump 6 is operated, and the pressure adjustment valve 10 is squeezed to a predetermined pressure while looking at the pressure water pressure gauge 12. In this process, the piston 3 is pushed upward by the pressure increase of the pressurizing unit 1a. However, since there is no escape place for the stock solution 102, the pressures of the stock solution unit 1b and the reaction tank 2 are substantially equal to the pressure of the pressurizing unit 1a.

  In the test, the liquid in the reaction tank 2 is appropriately sampled. As a sampling operation, first, the sampling valve 20 is opened, and the space between the discharge valve 19 and the sampling valve 20 in the discharge line 21 is filled with air or other gas. Next, when the sampling valve 20 is closed and the discharge valve 19 is opened, the liquid in the reaction tank 2 enters the space between the discharge valve 19 and the sampling valve 20. Next, the discharge valve 19 is closed, the sampling valve 20 is opened, and this liquid is extracted.

  At that time, the amount of gas generated can also be measured by collecting the liquid with a plastic sealed bag 30 such as a tetra bag and analyzing the amount and composition of the mixed gas.

  Since the pressure in the reaction tank 2 and the stock solution part 1b is reduced by sampling, the piston 3 is pushed up, the stock solution 102 flows into the reaction tank 2 from the stock solution part 1b, and the pressure in the reaction tank 2 and the stock solution part 1b is increased. It returns to almost the same as the pressure of the pressure part 1a.

  If the discharge valve 19 is opened separately from the sampling operation, the pressure in the reaction tank 2 can be measured.

  In this way, the reaction tank 2 can proceed with the reaction while receiving the supply of the stock solution 102 while maintaining a constant pressure, and the sampled solution can be sampled and analyzed.

  A second embodiment of the present invention will be described with reference to FIG. 2 (however, FIG. 2 shows a test preparation stage).

  The difference between the second embodiment shown in FIG. 2 and the first embodiment shown in FIG. 1 is the operation at the test preparation stage.

  The stock solution 102 is added separately from the stock solution portion 1b of the raw material container 1 and the reaction tank 2 (the second method described above).

  However, in the first embodiment, the test stock solution 102 is put into the stock solution part 1b of the material container 1 from the material injection line 14, and when the transfer valve 15 overflows, the transfer valve 15 and the material injection valve 13 are closed. However, in the second embodiment, a predetermined amount of the test stock solution 102 is measured from the raw material inlet 14 into the stock solution portion 1b of the raw material container 1 to form a space 1d in the stock solution portion 1b. After that, in a state where the transfer valve 15 is opened, the gas 104 having a known composition is sent from the raw material inlet 14 into the space 1d, and is discharged as the discharge gas 105 through the transfer valve 15, and the space of the stock solution 1b is discharged. After the 1d gas is replaced with the gas 104 having a known composition, the transfer valve 15 and the raw material injection valve 13 are closed.

  When the pressurization pump 6 is operated in this state and pressurization is started, the pressure of the stock solution portion 1b increases and the gas 104 starts to dissolve. After the gas is dissolved for a certain period of time, the transfer line 16 connecting the raw material container 1 and the reaction vessel 2 is assembled and operated in the same manner as in the first embodiment.

  At the time of the first sampling, if the liquid 110 is collected with a plastic sealed bag 30 such as a tetra bag and the amount and composition of the mixed gas is analyzed, how much of the gas 104 initially added to the space 1d will be analyzed. It can be calculated whether or not is dissolved in the liquid.

  Thereby, it becomes possible to test by adjusting the amount of dissolved gas in the liquid in accordance with the test purpose.

It is a figure which shows one embodiment of this invention. It is a figure which shows other embodiment of this invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Raw material container 2 Reaction tank 1a Pressurization part 1b Raw liquid part 3 Piston 14 Raw material injection line 16 Transfer line 19 Discharge valve 20 Sampling valve 24 Reaction tank inlet

Claims (10)

  A movable solid piston is provided in the closed cylinder of the raw material container, and the closed cylinder is divided into a pressurizing part and a raw liquid part for containing a raw liquid for reaction, and the raw liquid from the raw liquid part of the raw material container is received. Communicating the reaction tank, sending pressurized water from the pressure pump to the pressurizing part of the raw material container, and increasing the pressure of the stock solution part above atmospheric pressure by moving the solid piston, and the pressure of the reaction tank above atmospheric pressure The reaction tank is kept in an elevated state to perform a reaction such as a microbial reaction, and the liquid in the reaction tank is intermittently withdrawn and pressurized from the pressure pump to maintain the pressure in the reaction tank and the stock solution. A pressure test method characterized in that the pressure in the reaction tank is maintained while feeding the water and moving the piston to push the stock solution in the stock solution portion into the reaction tank.   The gas solution is injected into a part of the stock solution portion, and then pressurization of the stock solution portion is started. After the gas is dissolved in the stock solution, the stock solution having an increased dissolved gas concentration is supplied to the reaction tank. The pressure test method as described.   The pressurization test method according to claim 1 or 2, wherein the raw material container is accommodated in a refrigeration facility and the temperature of the stock solution part is controlled.   A liquid containing microorganisms is injected into the reaction tank, and a nutrient salt for growing microorganisms is placed in the stock solution of the stock solution part, and a microbial reaction is performed in the reaction tank. Pressure test method.   A discharge line is connected to the reaction tank, and two valves are connected to the discharge line, and the valve is opened and closed to sample the liquid while maintaining the pressure in the reaction tank. A pressure test method according to claim 1.   A movable solid piston is provided in the hermetic cylinder, and the hermetic cylinder is divided into a pressurizing part and a raw liquid part into which a stock solution for reaction is divided, and water for pressurization is supplied to the raw liquid part of the raw material container. A pressure pump that increases the pressure of the stock solution to atmospheric pressure, a transfer line that transfers the stock solution of the raw material container, and a transfer line that is connected to the transfer line and accepts the stock solution of the stock solution of the raw material container in a high-pressure state for microbial reaction And a discharge line for intermittently extracting a liquid that has undergone microbial reaction in the reaction tank.   The pressure test apparatus according to claim 6, wherein the raw material container is accommodated in a refrigeration facility.   The pressure test apparatus according to claim 6 or 7, wherein a filter or a check valve is connected to the transfer line.   9. An injection line for injecting a liquid containing microorganisms is connected to the reaction tank, and a raw material injection line for injecting a nutrient salt for growing microorganisms into the stock solution is connected to the stock solution part. The pressure test apparatus according to 1.   10. A discharge line according to claim 6, wherein a discharge line is connected to the reaction tank, and two valves for sampling the liquid are connected to the discharge line while maintaining the pressure in the reaction tank. Pressure test device.

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