Sampling device
The sampling device addresses the challenge of O-ring sealing in chemical production by employing a specific O-ring arrangement and FFKM materials within a glass-lined structure, achieving enhanced durability and contamination prevention.
Patent Information
- Application Number
- PCT/JP2024/032964
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2023-09-15
- Filing Date
- 2024-09-13
- Publication Date
- 2025-03-20
AI Technical Summary
Existing sampling devices used in chemical production processes, particularly for semiconductor manufacturing, face challenges with O-ring sealing due to the restriction on using lubricants, which can lead to O-ring coating tears and contamination of chemical substances.
The sampling device incorporates a unique arrangement of O-rings with specific groove dimensions and filling rates, utilizing FFKM O-rings to ensure sealing without lubrication, and features a glass-lined actuating portion to prevent contamination and ensure durability.
This configuration enhances the durability and sealing efficiency of the sampling device, preventing O-ring deterioration and contamination, even after extensive use, thereby ensuring the purity of chemical substances during sampling.
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Figure JP2024032964_20032025_PF_FP_ABST
Abstract
Description
Sampling Device
[0001] This specification discloses a technique relating to a sampling device.
[0002] A technology for producing liquid chemicals by stirring a liquid in a reactor is known. In this production process, a sampling device is sometimes used to extract a portion of the liquid during production to check the reaction status. The sampling device moves an actuator located within a cylindrical body and stores the liquid (sample) in a storage section. An O-ring is used in the actuator as a seal to prevent the liquid from leaking from the storage section. The O-ring is placed in a ring groove (housing) provided in the actuator and contacts the inner wall of the cylindrical body. When the actuator operates, the actuator (actually the O-ring) slides against the inner wall of the cylindrical body. Non-Patent Document 1 specifies the relationship between the size (linearity) of the O-ring and the width of the ring groove for O-rings (dynamic O-rings) used in sliding actuators. Japanese Industrial Standards 2401-2:2012 (hereinafter referred to as Non-Patent Document 1) discloses an example in which an O-ring is placed in a ring groove so that a gap is created between the O-ring and the side wall of the ring groove when the O-ring is in contact with a mating member. In Non-Patent Document 1, a gap is provided between the O-ring and the side wall of the ring groove so that the O-ring can move (change shape) within the ring groove when the operating part operates.
[0003] As mentioned above, Non-Patent Document 1 provides a gap between the O-ring and the side wall of the ring groove to allow the O-ring to move within the ring groove. In this case, a lubricant is typically applied to the O-ring to improve sliding between the O-ring and the mating member. Applying a lubricant to the O-ring can prevent damage to the O-ring even when the O-ring moves within the ring groove. However, when producing chemical substances used in the manufacture of semiconductor devices, etc., applying a lubricant to the O-ring is not recommended to prevent impurities from being mixed into the chemical substances during sampling. In this case, the surface of the O-ring is coated with a material with a low friction coefficient, such as PTFE, to ensure sliding performance with the mating member. However, even if the surface of the O-ring is coated with a material with a low friction coefficient, such as PTFE, the coating may break during operation of the operating part, resulting in reduced sealing performance. Furthermore, the broken coating may become contaminated with the chemical substances. Therefore, new measures are needed to prevent O-ring malfunctions even when the use of lubricants is restricted. The present specification aims to provide a novel sampling device characterized by the arrangement of the O-ring.
[0004] A first technology disclosed in this specification may be a sampling device for sampling a liquid in a reaction vessel. This sampling device may have a first groove in which a first O-ring is placed, formed in an actuation part that is actuated during sampling, and when the linear dimension of the first O-ring is taken as 100%, the width of the first groove may be 93% or more and 108% or less, and the filling rate of the first O-ring in the space within the first groove may be 70% or more and 95% or less.
[0005] A second technology disclosed in this specification is the sampling device of the first technology, wherein the operating unit may include a first part that reciprocates within the cylindrical body in the axial direction of the cylindrical body and contacts the inner surface of the cylindrical body via a first O-ring, and a second part that is connected to the first part and closes the opening of the cylindrical body. The first part and the second part may be provided at positions spaced apart from each other in the axial direction, and a storage part that stores a liquid sample may be formed by the first part, the second part, and the inner wall of the cylindrical body.
[0006] A third technique disclosed in this specification is the sampling device of the second technique, wherein the inner surface of the cylindrical body, the surface of the first portion, and the surface of the second portion may be formed of glass lining.
[0007] A fourth technology disclosed in this specification is the sampling device of the second or third technology, wherein a second groove in which a second O-ring is disposed may be formed on the outer peripheral surface of the second part. The diameter of a side wall of the second groove on the first part side may be larger than the inner diameter of the second O-ring and smaller than the outer diameter of the second O-ring. The diameter of a side wall of the second groove on the opposite side from the first part side may be larger than the outer diameter of the second O-ring. Furthermore, when the second part closes the opening, the second part may contact the opening via the second O-ring.
[0008] A fifth technique disclosed in this specification is a sampling device according to any one of the second to fourth techniques, which may include a drive unit for reciprocating the operating unit in the axial direction of the cylindrical body.
[0009] A sixth technology disclosed in this specification is a sampling device according to any one of the first to fourth technologies, wherein the sampling device may have a function of a baffle body that disturbs the flow of liquid inside the reaction vessel.
[0010] FIG. 1 shows a cross-sectional view of a main part of a reaction vessel; FIG. 2 shows a diagram for explaining an outline of a sampling device; FIG. 3 shows an enlarged view of the area surrounded by dashed line III in FIG. 1; FIG. 4 shows a diagram for explaining the arrangement of O-rings; FIG. 5 shows a diagram for explaining the characteristics of a first O-ring; FIG. 6 shows a diagram for explaining the relationship between the first O-ring and a first groove portion; FIG. 7 shows a diagram for explaining the characteristics of a second O-ring; FIG. 8 shows the results of an experimental example; and FIG. 9 shows a diagram for explaining a modified example of the sealing structure between the cylindrical body and the lid portion.
[0011] The sampling device disclosed herein can be suitably used, for example, to extract a portion of a liquid chemical substance being mixed (produced) in a reaction vessel. The sampling device may be fixed to the reaction vessel and extend from the outside to the inside of the reaction vessel. This eliminates the need to remove the lid of the reaction vessel when sampling the liquid (chemical substance) in the reaction vessel. As a result, impurities can be prevented from being mixed into the reaction vessel (chemical substance). For example, by using the sampling device disclosed herein, impurities such as metal ions can be prevented from being mixed into chemical substances when producing chemical substances such as resist materials used in the manufacture of semiconductor devices. The sampling device disclosed herein is suitable for use in a glass-lined reaction vessel. The portion of the sampling device located inside the reaction vessel may be glass-lined. Specifically, the surfaces of the first and second portions may be glass-lined.
[0012] The sampling device may include a cylindrical body and an actuating part that reciprocates in the axial direction of the cylindrical body within the cylindrical body. The actuating part may include a first part that contacts the inner surface of the cylindrical body via a first O-ring, and a second part that is located away from the first part and closes the opening of the cylindrical body. The first and second parts may be connected by a column part having a smaller diameter than the first part. This allows the first and second parts and the inner wall of the cylindrical body to form a storage part for storing a liquid (chemical substance) sample inside the cylindrical body. The first and second parts and the column part may be integrally molded. The second part and the opening of the cylindrical body may be sealed by a second O-ring.
[0013] The first and second O-rings may be made of FFKM (perfluoroelastomer). FFKM O-rings are characterized by excellent chemical resistance and heat resistance. By using FFKM O-rings, deterioration of the first and second O-rings due to the raw materials used in the reactor is suppressed. Furthermore, by using FFKM O-rings as the first and second O-rings, it is not necessary to coat the surfaces of the first and second O-rings with a material such as PTFE. This prevents tearing of the surfaces of the first and second O-rings (the coating layer when coated with a material such as PTFE). Furthermore, by using a first O-ring made of FFKM, sliding between the first O-ring and the inner surface of the cylindrical body can be ensured.
[0014] The sampling device may be attached to the reactor so that the cylindrical body does not interfere with the stirring blades of the reactor. The cylindrical body extends from the top to the bottom of the reactor and may have a circular cross-sectional shape or an irregular cross-sectional shape such as an ellipse. This allows the cylindrical body to function as a baffle that disturbs the flow of liquid within the reactor. By generating turbulence within the reactor, a uniform reaction product (chemical substance) can be produced. The sampling device may also include a drive unit for reciprocating the operating unit in the axial direction of the cylindrical body. The drive unit may include, for example, a motor for driving the operating unit and a supply device for supplying air or the like to the storage unit.
[0015] A first groove in which a first O-ring is disposed may be formed in a first portion of the actuation part. The first groove may be provided on the outer peripheral surface of the first portion. Furthermore, when the linear dimension of the first O-ring is taken as 100%, the width of the first groove may be 93% or more and 108% or less (Condition 1). Furthermore, when the actuation part is in contact with the inner surface of the cylindrical body via the first O-ring (a state in which the first O-ring seals the gap between the actuation part and the cylindrical body), the filling rate of the first O-ring in the space within the first groove may be 70% or more and 95% or less (Condition 2).
[0016] By satisfying the above conditions (1) and (2), the relationship between the O-ring and the ring groove differs significantly from the relationship between the O-ring and the ring groove specified in the JIS (Japanese Industrial Standards). Specifically, by satisfying the above conditions (1) and (2), movement of the first O-ring within the first groove is limited when the actuation portion is actuated. That is, even when the actuation portion is actuated, deformation of the first O-ring is significantly suppressed. This suppresses deterioration (e.g., tearing) of the first O-ring. Furthermore, by satisfying conditions (1) and (2), sufficient sealing between the actuation portion and the cylindrical body is ensured. Note that the width of the first groove relative to the first O-ring may be 96% or more, 100% or more, 102% or more, or 105% or more. Furthermore, the width of the first groove relative to the first O-ring may be 105% or less, 102% or less, 100% or less, or 96% or less. The filling rate of the first O-ring may be 78% or more, 80% or more, 85% or more, or 90% or more, or may be 90% or less, 85% or less, 80% or less, or 78% or less.
[0017] A second groove in which a second O-ring is disposed may be formed on the outer peripheral surface of the second portion. The relationship between the second O-ring and the second groove may be the same as the relationship between the first O-ring and the first groove described above. Alternatively, the height (length from the bottom of the second groove) of the side walls (walls on both axial sides of the actuation portion) of the second groove may be different between the side wall (first side wall) on the first portion side and the side wall (second side wall) opposite the first portion. Specifically, the diameter of the first side wall (diameter perpendicular to the axial direction of the actuation portion) may be larger than the inner diameter of the second O-ring and smaller than the outer diameter of the second O-ring. Furthermore, the diameter of the second side wall may be larger than the outer diameter of the second O-ring. The second O-ring seals the second portion and the end (opening) of the cylinder. Therefore, when the second portion closes the opening of the cylinder, the second portion contacts the opening of the cylinder via the second O-ring, isolating the interior and exterior of the housing. Since the second groove is provided on the outer peripheral surface of the second part, the second O-ring does not contact the end face (bottom surface) of the cylindrical body. When the second part closes the opening of the cylindrical body, the second O-ring contacts the part between the side face and the end face of the cylindrical body (the curved part connecting the side face and the end face).
[0018] (Reaction Vessel) Referring to FIG. 1 , a reaction vessel 100 in which a sampling device 10 is used will be described. The reaction vessel 100 includes a tank 40, a raw material inlet 60, a raw material outlet 72, a motor 50, and an agitating blade 52. The sampling device 10 is attached to the tank 40. The sampling device 10 includes a sampling unit 14 and a drive unit 12 that drives the sampling unit 14. The sampling unit 14 extends from the outside to the inside of the tank 40 and is attached to the tank 40 so as not to interfere with the agitating blade 52. The tank 40 and the sampling unit 14 are glass-lined. Note that glass linings are a composite of metal and glass, and are characterized by excellent corrosion resistance.
[0019] The reactor 100 is used to mix liquid raw materials and produce liquid chemical substances. The raw materials are supplied to the reactor interior 54 through a raw material inlet 60. The raw materials supplied to the reactor interior 54 are agitated by an agitator blade 52. The agitator blade 52 is connected to a motor 50, and by driving the motor 50, the agitator blade 52 rotates and the raw materials are agitated. Agitating the raw materials causes a reaction to proceed, and the target chemical substance can be produced. The reactor 100 may also be equipped with a heater (not shown) for adjusting the temperature of the raw materials, a thermometer (not shown) for measuring the temperature of the raw materials, and the like.
[0020] When producing chemical substances, a portion of the chemical substance inside the can 54 may be extracted using the sampling device 10 to check the progress of the reaction. The sampling device 10 includes a long, tubular sampling section 14 and a drive section 12 that drives components inside the sampling section 14. The sampling section 14 disrupts the flow of the liquid (raw material) inside the can 54, generating turbulence inside the can 54. This promotes the reaction of the raw material inside the can 54 and makes the distribution of the raw material uniform. The sampling section 14 (sampling device 10) can also be considered a sampling baffle. Details of the sampling section 14 will be described later. The produced chemical substance is discharged from a raw material discharge port 72.
[0021] The sampling unit 14 will be described with reference to FIGS. 2 and 3 . As shown in FIG. 2 , the sampling unit 14 includes a cylindrical body 16 having an open tip, an actuating unit 32 provided within the cylindrical body 16, a shaft 17 for actuating the actuating unit 32 in the axial direction of the cylindrical body 16, and a support unit 19 for supporting the actuating unit 32. The cylindrical body 16 and the actuating unit 32 form a storage unit 30 for storing a liquid sample. The support unit 19 is fixed to the shaft 17. A drive device 38 for driving (causing reciprocating motion of) the shaft 17 is provided on the exterior of the cylindrical body 16. Two pipes (a supply pipe 34 and a discharge pipe 36) extend from the exterior of the cylindrical body 16 toward the storage unit 30. The supply pipe 34 can supply a gas or liquid fluid into the storage unit 30. The discharge pipe 36 can discharge a gas or liquid fluid from the storage unit 30.
[0022] FIG. 3 shows an enlarged cross-sectional view of the tip portion of the sampling unit 14. Note that some components (O-rings) are not shown in FIG. 3 . The O-rings will be described later. As described above, an actuating unit 32 is provided within the cylindrical body 16. The actuating unit 32 includes a first portion 24 that contacts the inner surface of the cylindrical body 16 via the O-ring, a second portion 28 that closes the opening portion 16 a of the cylindrical body 16, and a column portion 26 that connects the first portion 24 and the second portion 28. The first portion 24, the second portion 28, and the column portion 26 are each cylindrical. The first portion 24, the second portion 28, and the column portion 26 are integrally molded. The shaft 17 is fitted inside the first portion 24, the second portion 28, and the column portion 26. The support portion 19 supports the outer surface of the second portion 28. The support portion 19 and the second portion 28 form a lid portion 20 that opens and closes the opening portion 16 a. The actuating part 32 and the shaft 17 are fixed and driven by a drive 38 (see also FIG. 2).
[0023] The first portion 24 is located at a distance from the second portion 28. When the lid 20 closes the opening 16a, the first portion 24, the second portion 28, the column portion 26, and the cylindrical body 16 form a storage section 30 for storing a chemical sample. The inner surface of the cylindrical body 16 and the first portion 24 are sealed by a first O-ring (described below). The opening 16a of the lid 20 and the second portion 28 are sealed by a second O-ring (described below). Therefore, the storage section 30 is sealed from the space outside the storage section 30. The supply pipe 34 penetrates the first portion 24 and extends into the storage section 30. The supply pipe 34 extends slightly into the storage section 30 and opens near the first portion 24 (upper side of the storage section 30). Meanwhile, the discharge pipe 36 extends to near the first portion 24 (lower side of the storage section 30).
[0024] As described above, the sampling device 10 is positioned so that the sampling section 14 is located inside the can 54. Before sampling the can interior 54, the lid 20 (second section 28) closes the opening 16a of the cylindrical body 16 (FIG. 2(a)). At this time, air is sealed inside the storage section 30. As described above, the inner surface of the cylindrical body 16 and the first section 24, and the opening 16a and second section 28 of the lid 20 are sealed with O-rings. Therefore, while the lid 20 closes the opening 16a, it is possible to prevent chemical substances from entering the storage section 30 from outside the sampling device 10. Note that immediately before sampling the can interior 54, the supply pipe 34 and the discharge pipe 36 are closed by valves (not shown).
[0025] When sampling the can interior 54, the piston in the drive unit 38 is extended, moving the shaft 17 downward and opening the opening 16a of the cylindrical body 16 ( FIG. 2( b) ). Moving the shaft 17 downward exposes the storage unit 30 to the can interior 54. At this time, the air sealed in the storage unit 30 is discharged into the can interior 54. Chemical substances in the can interior 54 then enter the storage unit 30. That is, when sampling, the sampling device 10 uses the piston in the drive unit 38 to move the shaft 17 downward, thereby discharging the air from the storage unit 30 and allowing the sampled substance (chemical substance) to enter the storage unit 30. After the chemical substance has entered the storage unit 30, the piston in the drive unit 38 moves the shaft 17 upward, closing the opening 16a of the cylindrical body 16 and sealing the chemical substance in the storage unit 30 ( FIG. 2( a) ).
[0026] When the lid 20 closes the opening 16a of the cylindrical body 16, the opening 16a and the second portion 28 are sealed by an O-ring. This prevents the sampled chemical substance from leaking out of the container 30 (inside the can 54). Furthermore, because the inner surface of the cylindrical body 16 and the first portion 24 are sealed by an O-ring, this also prevents the chemical substance from leaking out of the container 30 (above the first portion 24) during sampling. After the sample material is sealed inside the container 30, the valves of the supply pipe 34 and the discharge pipe 36 are opened to supply gas (e.g., nitrogen gas) into the container 30 from the supply pipe 34. Furthermore, the sample material inside the container 30 is discharged out of the sampling section 14 through the discharge pipe 36, and the sample material is sent to a sample material storage portion (e.g., a bottle container). The inside of the container 30 is then cleaned by supplying and discharging a cleaning solution or gas into and from the container 30 using the supply pipe 34 and the discharge pipe 36. This makes it possible to suppress the influence of the sampled substance from the previous sampling when sampling the chemical substance inside the can 54. Note that the inside of the storage unit 30 can also be made into a vacuum state by suctioning the inside of the storage unit 30 through the discharge pipe 36 with the valve of the supply pipe 34 closed.
[0027] 4 to 8, the O-rings used in the sampling device 10 will be described. As shown in Fig. 4, a first O-ring 70 is disposed between the cylindrical body 16 and the first portion 24, a second O-ring 80 is disposed between the cylindrical body 16 and the second portion 28, and a third O-ring 90 is disposed between the actuating portion 32 (first portion 24, second portion 28) and the shaft 17. Each of the O-rings 70, 80, and 90 is made of FFKM (perfluoroelastomer).
[0028] As shown in Fig. 5, three first O-rings 70 are arranged side by side in the axial direction of the cylindrical body 16. Three first grooves 25 (groove 25a, groove 25b, groove 25c) are formed on the outer peripheral surface of the first portion 24. A first O-ring 70 (O-ring 70a, O-ring 70b, O-ring 70c) is fitted into each of the first grooves 25. Each of the first O-rings 70 is in contact with the inner surface of the cylindrical body 16. The first O-rings 70 provide a seal between the cylindrical body 16 and the first portion 24.
[0029] FIG. 6 shows a schematic diagram of the first O-ring 70 and the first groove 25. The width 25w of the first groove 25 is adjusted to be 93% or more and 108% or less of the linear dimension (diameter) 70R of the first O-ring 70. That is, the linear dimension 70R of the first O-ring 70 and the width 25w of the first groove 25 are adjusted to be approximately equal. Therefore, when the first O-ring 70 is fitted into the first groove 25 and brought into contact with the inner surface of the cylindrical body 16, the filling rate of the space within the first groove 25 is high. Specifically, the first O-ring 70 occupies 70% or more and 95% or less of the cross-sectional area (depth 25h × width 25w) of the first groove 25 (see also FIG. 5). Furthermore, by placing the first O-ring 70 in the first groove portion 25 at such a filling rate, when the first part 24 (actuating portion 32) moves back and forth relative to the cylindrical body 16, the movement of the first O-ring 70 in the first groove portion 25 (deformation of the first O-ring 70) is significantly limited.
[0030] As shown in Figures 7(a) and 7(b), the cylindrical body 16 is in an open state, and the cylindrical body 16 is in a closed state. The second O-ring 80 is disposed in a second groove 29 formed on the outer peripheral surface of the second portion 28. The second groove 29 has a first side wall 29a on the first portion 24 side and a second side wall 29b on the opposite side from the first portion 24, each having a different height. The first side wall 29a is positioned inside the cylindrical body 16 when the cylindrical body 16 is closed. The second side wall 29b, specifically the second portion 28, faces the end face of the cylindrical body 16 when the cylindrical body 16 is closed. Therefore, the height of the first side wall 29a is lower than the height of the second side wall 29b. In other words, the diameter of the first side wall 29a is smaller than the inner diameter of the cylindrical body 16. Furthermore, the diameter of first side wall 29a is larger than the inner diameter of second O-ring 80 and smaller than the outer diameter of second O-ring 80. The diameter of second side wall 29b is larger than the outer diameter of second O-ring 80 and larger than the inner diameter of cylindrical body 16. Because the diameters of side walls 29a, 29b are larger than the inner diameter of second O-ring 80, second O-ring 80 is held in second groove 29 without coming off.
[0031] As shown in FIG. 7( a), when the housing 30 is exposed to the can interior 54 (see also FIG. 2( b)), the cylindrical body 16 is not in contact with the second O-ring 80. At this time, the second O-ring 80 is not subjected to compression and has a substantially circular cross section. In the state shown in FIG. 7( a), the first side wall 29a functions to position the second O-ring 80 (preventing the second O-ring 80 from moving toward the housing 30). As shown in FIG. 7( b), when the housing 30 is sealed (see also FIG. 2( a)), the cylindrical body 16 contacts the second O-ring 80, and the second O-ring 80 is subjected to compression and deforms. Compression of the second O-ring 80 seals the gap between the cylindrical body 16 and the second portion 28, sealing the housing 30. The second O-ring 80 contacts the curved portion connecting the inner circumferential surface and the end face of the cylindrical body 16. Furthermore, since the gap between the cylindrical body 16 and the second part 28 is sealed by the tight contact of the second O-ring 80, there is no need to polish or smooth the part of the cylindrical body 16 that comes into contact with the second O-ring 80 (there is no need to smooth the surface that the O-ring comes into contact with).
[0032] Experimental Example 1 The durability of the sampling device 10 was evaluated by varying the linear dimension 70R of the first O-ring 70, the width 25w of the first groove 25, and the filling rate of the first O-ring 70 in the space within the first groove 25. Specifically, sampling devices were fabricated in which the ratio of the width 25w to the linear dimension 70R (linear ratio) and the filling rate of the first O-ring 70 in the first groove 25 were varied as shown in Figure 8, and a durability test was conducted. The O-rings used were made of FFKM and had an inner diameter of approximately 50 mm and a linear dimension of 3.5 mm. In the durability test, the operation of opening and closing the lid 20 from the state shown in Figure 2(a) to the state shown in Figure 2(b) and then back to the state shown in Figure 2(a) was defined as one cycle, and the sealing ability of the storage section 30 was evaluated after 300, 2000, and 4000 cycles of opening and closing. The airtightness was evaluated by applying a pressure (air pressure) of 0.3 MPa to the inside of the housing portion 30 and checking for air leakage (pressure drop). The results of the durability test are shown in Figure 8. The crushed width of the O-ring and the operating pressure when the lid portion 20 was operated are also shown in Figure 8.
[0033] As shown in FIG. 8 , no air leakage was observed in samples 3 to 8 after 300 cycles of the durability test. In samples 3 to 8, the O-rings did not deteriorate even after the lid 20 was opened and closed 300 times, and good sealing performance was maintained. That is, it was confirmed that the first O-ring 70 exhibits good sealing performance by satisfying a filling rate of 70% to 95% and a linear ratio of 93% to 108%. Furthermore, no air leakage was observed in samples 4 to 8 even after 2,000 cycles of the durability test. All of these samples satisfied a filling rate of 78% to 95% and a linear ratio of 93% to 105%. Furthermore, no air leakage was observed in samples 5 to 7 even after 4,000 cycles of the durability test. All of these samples satisfied a filling rate of 80% to 90% and a linear ratio of 96% to 102%.
[0034] In addition, the crushed width of sample 1 was 0 mm, and no compressive force was applied to the O-ring. In other words, the O-ring was not in sufficient contact with the inner surface of the cylindrical body 16. Therefore, it is presumed that air leakage occurred after 300 cycles of the cycle test. Furthermore, in sample 2, twisting occurred in the O-ring after 300 cycles of the durability test. Therefore, it is presumed that air leakage occurred after 300 cycles of the cycle test. In sample 9, it was confirmed that the O-ring was worn down after 300 cycles of the durability test. Therefore, it is presumed that the sealing performance of the O-ring deteriorated, causing air leakage after 300 cycles of the cycle test.
[0035] Experimental Example 2 A durability test similar to that of Experimental Example 1 was conducted using a second O-ring 80 with an inner diameter of approximately 80 mm and a linearity of 6 mm. Furthermore, as a comparative example, a durability test was also conducted on a sampling device (sampling unit 114) having a typical lid seal structure as shown in FIG. 9 . The sampling unit 114 in FIG. 9 will be briefly described. The sampling unit 114 differs from the sampling unit 14 in the seal structure between the cylindrical body 16 and the lid unit 120. The sampling unit 114 includes a cylindrical body 16 and a lid unit 120 that moves forward and backward relative to the cylindrical body 16. A storage unit 30 for storing a sample substance (chemical substance) is formed between the cylindrical body 16 and the lid unit 120. A ring-shaped seal material 180 with a triangular cross section is disposed on the surface of the lid unit 120 facing the cylindrical body 16. The seal material 180 is made of PTFE resin. In the sampling unit 114, as shown in FIG. 9( a), when the lid unit 120 is open, the seal material 180 has a triangular cross section. On the other hand, as shown in FIG. 9B, when the lid 120 is closed, the sealant 180 is crushed between the cylindrical body 16 and the lid 120 to seal the gap between the cylindrical body 16 and the lid 120 .
[0036] In this experimental example, the airtightness inside the storage section 30 was evaluated after 300, 2000, and 4000 cycles of opening and closing, as in Experimental Example 1. In addition, in both the sampling section 14 (this experimental example) and the sampling section 114 (comparative example), a linear 1 mm wire was placed on the sealing material (second O-ring 80, sealing material 180) to evaluate deterioration of the sealing material.
[0037] As a result of this experiment, the sampling unit 14 maintained its sealing ability even after 4,000 cycles of opening and closing, while air leakage was confirmed in the sampling unit 114 after 300 cycles of opening and closing. Furthermore, the sampling unit 14 maintained its sealing ability even after 4,000 cycles of opening and closing with the wire in place. However, when the sampling unit 114 was opened and closed with the wire in place, the sealing material 180 deformed and no longer functioned as a sealing material. The sealing material 180 is made of PTFE resin. PTFE resin has higher hardness and weaker elastic recovery than an O-ring made of FFKM. Therefore, when the lid unit 120 was opened and closed with the wire in place, the contact portion of the sealing material 180 with the cylindrical body 16 (the apex of the triangle of the sealing material 180) deformed and did not immediately recover to its original shape. In other words, it is believed that a defect formed in the contact portion (circumferential portion) of the sealing material 180 with the cylindrical body 16 formed by the apex of the triangle, causing it to no longer function as a sealing material.
[0038] The above-described embodiments are merely examples embodying the technology disclosed herein. For example, in the above-described embodiments, three first O-rings 70 are disposed in the first portion 24 of the actuation portion 32. However, any number of first O-rings 70 may be disposed in the first portion 24, as long as at least one first O-ring 70 is disposed in the first portion 24. Furthermore, even when multiple O-rings are disposed in the first portion 24, not all of the O-rings need to be first O-rings 70. In other words, at least one first O-ring 70 may be disposed in the first portion 24, and the other O-rings may be O-rings different from the first O-ring 70 (e.g., O-rings coated with a material with a low coefficient of friction, such as PTFE).
[0039] Furthermore, a lubricant may be applied to the first O-ring 70. The sampling device 10 disclosed in the above embodiment can achieve good durability even without applying a lubricant to the first O-ring 70, and applying a lubricant to the first O-ring 70 is not prohibited.
[0040] In addition, on the upper side of the sampling section 14, an O-ring substantially identical to the first O-ring 70 arranged on the first part 24 of the actuating section 32 may be arranged between the shaft 17 and the cylinder 16, and / or the shaft 17 and the drive device 38.
[0041] The technology disclosed in this specification requires that the first O-ring 70 is disposed in the first portion 24 of the actuation portion 32, and the relationship between the first O-ring 70 and the first groove portion 25 satisfies the above-described conditions (1) and (2). Therefore, the seal between the second portion 28 and the cylindrical body 16 does not necessarily have to have the structure described in the embodiment. For example, the seal between the second portion 28 and the cylindrical body 16 may be achieved by a ring-shaped sealant with a triangular cross section on the cylindrical-side surface of the lid portion described in FIG. 9 . Alternatively, the seal between the second portion 28 and the cylindrical body 16 may have the same structure as the seal between the first portion 24 and the cylindrical body 16.
[0042] Although specific examples of the present invention have been described in detail above, these are merely examples and do not limit the scope of the claims. The claimed technology includes various modifications and variations of the specific examples exemplified above. Furthermore, the technical elements described in this specification or drawings exhibit technical utility alone or in various combinations, and are not limited to the combinations described in the claims at the time of filing. Furthermore, the technology exemplified in this specification or drawings can achieve multiple objectives simultaneously, and achieving one of these objectives alone is technically useful.
Claims
1. A sampling device for sampling liquid inside a reaction vessel, comprising: a first groove portion in which a first O-ring is placed is formed in an operating portion that operates during sampling; when the linear dimension of the first O-ring is taken as 100%, the width of the first groove portion is 93% or more and 108% or less; and the filling rate of the first O-ring in the space inside the first groove portion is 70% or more and 95% or less.
2. The sampling device described in claim 1, wherein the operating part comprises a first part that reciprocates in the axial direction of the cylinder inside the cylinder and contacts the inner surface of the cylinder via the first O-ring, and a second part that is connected to the first part and blocks the opening portion of the cylinder, the first part and the second part are provided at positions spaced apart in the axial direction, and a storage section in which a sample of the liquid is stored is formed by the first part, the second part and the inner wall of the cylinder.
3. The sampling device according to claim 2, wherein the inner surface of the cylindrical body, the surface of the first portion, and the surface of the second portion are formed with a glass lining.
4. A sampling device as described in claim 2 or 3, wherein a second groove portion in which a second O-ring is placed is formed on the outer peripheral surface of the second portion, the diameter of the side wall of the second groove portion on the first portion side is larger than the inner diameter of the second O-ring and smaller than the outer diameter of the second O-ring, the diameter of the side wall of the second groove portion opposite the first portion side is larger than the outer diameter of the second O-ring, and when the second portion blocks the opening portion, the second portion contacts the opening portion via the second O-ring.
5. A sampling device according to claim 2 or 3, further comprising a drive unit for reciprocating the operating unit in the axial direction of the cylindrical body.
6. The sampling device according to claim 1, wherein the sampling device has a function of a baffle body for disturbing the flow of liquid within the reaction vessel.
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