JP6565472B2 - Container lid, lid unit, reaction tank - Google Patents

Description

  The present invention relates to a container lid, a lid unit, and a reaction tank.

  2. Description of the Related Art Conventionally, apparatuses for measuring a measurement target substance contained in a sample solution by various methods are known. For example, the apparatus described in Patent Document 1 has a configuration in which a measurement target substance in a sample solution is vaporized, guided to an analysis apparatus, and quantified. In the measurement apparatus described in Patent Document 1, piping is drawn out from tanks connected to a plurality of reagents, and a plurality of types of reagents are sequentially supplied to containers for storing samples. By adopting such a configuration, the measurement apparatus described in Patent Document 1 can perform processing smoothly and simplify the apparatus configuration.

Japanese Patent Laid-Open No. 2004-212075

  In the apparatus described in Patent Document 1, piping for supplying each reagent is connected to a lid attached to the reaction tank so that each reagent can be supplied into the reaction tank. In such a structure, when the kind of reagent which should be supplied in a reaction tank increases, the planar view area of a lid | cover tends to become large. As a result, the reaction tank for covering is also enlarged, and the amount of sample necessary for measurement is likely to increase. As the number of samples required for measurement increases, the cost of reagents required for measurement and the maintenance man-hours for reagent replenishment tend to increase, and the amount of measurement waste liquid increases, so multiple pipes can be connected while suppressing an increase in size. A lid was sought.

  Moreover, even if the lid is connected to a plurality of pipes, the pipes need to be removed or attached during maintenance. As described above, when a lid capable of connecting a plurality of pipes while suppressing an increase in size is used, the pipes connected to the lids are densely packed. In such a configuration, when removing or attaching the pipe, the tool to be used may interfere with the surrounding pipe, which may reduce the work efficiency. Therefore, a lid that can easily remove and attach a plurality of pipes has been demanded.

  This invention is made | formed in view of such a situation, Comprising: It aims at providing the container lid which can connect several piping and can remove and attach several piping easily. Another object of the present invention is to provide a lid unit and a reaction tank that are provided with the container lid as described above and are easy to maintain and inspect.

  In order to solve the above problems, according to one aspect of the present invention, an opening provided at an upper end of a container main body is closed, and a plurality of through holes for inserting pipes are provided inside the container main body. A container lid, having a first connection portion provided in the center in plan view, and a second connection portion provided around the first connection portion in plan view, wherein the first connection portion is The upper surface of the first connection portion is formed to be higher than the second connection portion, and the plurality of through holes are provided in a first through hole provided in parallel with a vertical direction, and the first through hole. And an upper end of the first through hole is opened at the first connection portion, and an upper end of the second through hole is opened at the second connection portion. A container lid is provided.

  In one aspect of the present invention, a first opening that is an opening at an upper end of the first through hole is disposed along a first virtual circle set in the first connection portion in plan view, 2nd opening part which is an opening part of the upper end of 2 through-holes is set as the said 2nd connection part in planar view, and also as a structure arrange | positioned along the 2nd virtual circle which is concentric with the said 1st virtual circle Good.

  In one aspect of the present invention, the plurality of through holes include a plurality of the second through holes, and the plurality of second through holes have an axis passing through the center of the concentric circle and parallel to the vertical direction as a rotation axis. It is good also as a structure arrange | positioned along the side surface of a virtual cone.

  In one aspect of the present invention, a plurality of the second openings are formed in the second connection portion, the plurality of second openings are divided into a plurality of units, and each of the units is the first Two second openings adjacent to each other along the circumferential direction of two virtual circles, and the separation distance between the two units adjacent to each other along the circumferential direction is the two second openings included in the unit. It is good also as a structure longer than the separation distance of a part.

  In one aspect of the present invention, a plurality of the first openings are formed in the first connection portion, and overlap the second virtual circle between the two units adjacent along the circumferential direction. Assuming an arc, the first opening may be arranged in a fan-shaped region surrounded by the arc and a line segment connecting both ends of the arc and the center of the concentric circle. Good.

  One aspect of the present invention includes the above-described container lid, and a fixture that hermetically fixes the pipe to each of the plurality of through-holes provided in the container lid, and the through-hole has a female screw therein. The fixing device is provided with a lid unit having an insertion hole into which the pipe is inserted, a male screw formed on the outer periphery, and screwed to the through hole.

  One aspect of the present invention provides a reaction vessel comprising a bottomed cylindrical container body having an open upper end and the above-described lid unit that hermetically closes the opening of the upper end.

  In one aspect of the present invention, the container body includes a cylindrical first member having the opening and the same inner diameter as the opening, and a bottomed cylindrical first member having an inner diameter smaller than the opening. It is good also as a structure which 2 member is connected and the opening part of the said 1st through-hole of the said container lid which the said cover unit has and the said 2nd member have overlapped with planar view.

  According to the present invention, it is possible to provide a container lid in which a plurality of pipes can be connected and the plurality of pipes can be easily detached and attached. In addition, a lid unit and a reaction tank that are provided with the container lid as described above and can be easily maintained and inspected can be provided.

It is a schematic perspective view of the container lid and lid unit which concern on this embodiment. It is explanatory drawing of the container lid which concerns on this embodiment. It is explanatory drawing which shows the modification of the container lid which concerns on this embodiment. It is explanatory drawing of the reaction tank which concerns on this embodiment. It is explanatory drawing which shows a mode that a reaction tank is fixed to another member. It is explanatory drawing explaining the effect of the container lid which concerns on this embodiment. It is a schematic sectional drawing which shows the modification of the container lid which concerns on this embodiment. It is explanatory drawing of the measuring apparatus which has the reaction tank which concerns on this embodiment.

  Hereinafter, a container lid, a lid unit, and a reaction tank according to an embodiment of the present invention will be described with reference to FIGS. In all the drawings below, the dimensions and ratios of the constituent elements are appropriately changed in order to make the drawings easy to see.

(Container lid)
FIG. 1 is a schematic perspective view of a container lid 13 and a lid unit 19 according to this embodiment.

  The container lid 13 airtightly closes the opening 12x provided at the upper end of the container body 12. The container lid 13 includes a connection part 131 to which piping is connected, and a fitting part 132 that fits into the opening 12x of the container body 12 and closes the opening 12x.

  The fitting part 132 has a substantially columnar shape and has an annular seal part 138 on the outer periphery. As the seal portion 138, for example, an O-ring can be used.

  The connection part 131 is located above the fitting part 132. The connection part 131 of this embodiment has a rotationally symmetric shape having the same central axis as the central axis CA of the fitting part 132 having a cylindrical shape.

  The connection part 131 is formed in two steps so that the central part in plan view is higher than the peripheral part in plan view. In the central part of the connection part 131 in the plan view, the part where the upper surface is formed higher than the peripheral part in the plan view is the first connection part 131A, and the part provided around the first connection part 131A in the plan view is the second connection. This will be referred to as a part 131B.

  In the present embodiment, “plan view” refers to viewing an object such as the container lid 13 in a visual field from above in the vertical direction. In the case of the container lid 13 of the present embodiment, the direction of the central axis CA and the vertical direction are parallel.

  The connection part 131 is not only configured to be formed in two stages of the first connection part 131A and the second connection part 131B, but more than three stages so as to increase in order from the peripheral part in plan view toward the central part in plan view. A multi-stage configuration can also be employed.

  The upper surface 131A1 of the first connection portion 131A is orthogonal to the central axis CA of the fitting portion 132.

  The upper surface 131B1 of the second connection portion 131B is inclined with respect to the central axis CA. Specifically, the second connection portion 131B has a truncated cone shape whose diameter gradually decreases toward the first connection portion 131A.

  The container lid 13 has a plurality of through holes 13a into which pipes are inserted. The through hole 13a may have the same inner diameter from the upper end to the lower end. For example, the through hole 13a may have a configuration in which the inner diameter changes midway so that the opening diameter at the lower end is smaller than the opening diameter at the upper end.

  The container lid 13 of the present embodiment has three through holes 13a that open to the upper surface 131A1 of the first connection portion 131A and six through holes 13a that open to the upper surface 131B1 of the second connection portion 131B. Yes.

  The through hole 13a that opens to the upper surface 131A1 of the first connecting portion 131A is the “first through hole” in the present invention, and the through hole 13a that opens to the upper surface 131B1 of the second connecting portion 131B is the “second hole” in the present invention. It is a “through hole”. In the following description and drawings, the first through-hole may be indicated by using a symbol H1, and the second through-hole may be indicated by using a symbol H2.

  The first through hole H1 is provided in parallel with the central axis CA.

On the other hand, the second through hole is provided obliquely with respect to the central axis CA.
Specifically, the plurality of second through holes H2 are formed along the side surface of the virtual cone VC (or the generatrix of the virtual cone VC) with the central axis CA as the rotation axis. Accordingly, the second through hole H2 is inclined so that the distance from the central axis CA gradually decreases from the connection portion 131 toward the fitting portion 132.

  The container lid 13 has an annular locking portion 139 on the outer peripheral portion in plan view. The latching | locking part 139 is used when attaching the reaction tank 11 provided with the container lid 13 to another member.

(Lid unit)
The lid unit 19 includes a container lid 13 and a fixture 15 that hermetically fixes a pipe to each of the plurality of through holes 13 a provided in the container lid 13.

  An internal thread 13x is formed inside the opening at the upper end of the through hole 13a.

  The fixture 15 has a hexagon bolt shape and has an insertion hole 15a for inserting a pipe in the longitudinal direction. Moreover, the fixing tool 15 has a male screw 15x formed on the lower outer periphery corresponding to the screw portion of the bolt. The fixing tool 15 is inserted into the through-hole 13a, and is fixed by screwing the male screw 15x with the female screw 13x.

  The fixture 15 has a ferrule (not shown) inside. The ferrule is a member having a frustoconical outer shape, and for example, a resin can be used. The ferrule has a through hole along the rotational symmetry axis of the truncated cone. The inner diameter of the through hole of the ferrule is approximately equal to or slightly larger than the outer diameter of the pipe inserted into the insertion hole 15a.

  The fixture 15 has a ferrule so that the through-hole of the ferrule and the insertion hole 15a of the fixture are concentric. The pipe inserted into the insertion hole 15a is also inserted into the through hole of the ferrule. When the fixing tool 15 is screwed to the through-hole 13a in such a state, the ferrule clamps the inserted pipe while being crushed and deformed, and fixes it so as not to come off. Thereby, when the fixing tool 15 is screwed to the through hole 13a in a state where the pipe is inserted into the insertion hole 15a, the fixing tool 15 can be fixed and the pipe can be fixed in an airtight manner.

  FIG. 2 is an explanatory view of the container lid 13 according to the present embodiment, FIG. 2A is a plan view of the container lid 13, and FIG. 2B is a bottom view of the container lid 13.

  As shown in the figure, the container lid 13 of the present embodiment is formed such that the openings of the through holes 13a are rotationally symmetrical in plan view.

  First, the first opening H1x, which is the opening of the first through hole H1, is arranged along the first virtual circle IC1 set in the first connection portion 131A in plan view. Further, the second opening H2x that is the opening of the second through hole H2 is arranged along the second virtual circle IC2 that is set in the second connection portion 131B and is concentric with the first virtual circle IC1. In the plan view, the center C of the concentric circle and the center axis CA of the fitting portion 132 overlap.

  The plurality of second openings H2x are divided into a plurality of units. Specifically, the plurality of second openings H2x are divided into three units, with two second openings H2x adjacent along the circumferential direction of the second virtual circle IC2 as one unit. . In the figure, one set of units is surrounded by a broken line α.

  Each unit α is such that the distance W1 between the units α along the circumferential direction of the second virtual circle IC2 is longer than the distance W2 between the second openings H2x included in each unit α. Is set. The three units α are arranged at equal intervals along the circumferential direction of the second virtual circle IC2.

  Further, as shown in the bottom view of FIG. 2B, all the openings 13y on the fitting portion 132 side of the plurality of through holes 13a are set on the lower surface of the fitting portion 132 and are concentric with the first virtual circle IC1. Are arranged along the third virtual circle IC3.

  Here, as described above, the first through hole H1 is provided in parallel with the central axis CA, and the second through hole H2 is provided along the side surface of the virtual cone VC having the central axis CA as the rotation axis. Yes. Therefore, for example, when the first through hole H1 is provided so as to overlap the central axis CA, the first through hole H1 and the second through hole H2 are arranged to converge toward the apex of the virtual cone VC. If pipes are inserted into such first through holes H1 and second through holes H2, the pipes collide in the vicinity of the apex of the virtual cone VC, and there is a possibility that the tip of the pipe may not be in a desired position.

  Therefore, in the container lid 13, the first through hole H1 is provided at a position that does not overlap with the central axis CA.

  Further, assuming an arc Ar overlapping the second virtual circle IC2 between two units α adjacent along the circumferential direction of the second virtual circle IC2, the first opening H1x has an arc Ar and an arc Ar Are arranged in a fan-shaped region S surrounded by a line segment connecting the two ends and the center C of the concentric circle.

  By arranging the first through hole H1 and the second through hole H2 in such a manner, it is possible to suppress the collision between the inserted pipes, and the pipes in a desired posture (tilt with respect to the vertical direction, tip position). Can be inserted.

  In FIG. 2, the six second openings H2x are divided into three units, but the present invention is not limited to this. FIG. 3 is an explanatory view showing a modified example of the container lid according to the present embodiment, and corresponds to FIG.

  In the container lid 13H shown in FIG. 3, the second openings H2x provided in the second connection portion 131B are grouped into two sets of units α, with the two adjacent second openings H2x as one set. . Further, the remaining two second openings H2x are arranged one by one between two sets of units α adjacent in the circumferential direction of the second virtual circle IC2.

  As described above, in the container lid according to the present invention, when the plurality of second openings H2x are provided, all the second openings H2x are not necessarily combined into a plurality of sets of units α, and are appropriately arranged as necessary. Can be adjusted. Furthermore, in the container lid which concerns on this invention, when it has several 2nd opening part H2x, it is not necessary to put together for every unit (alpha).

(Reaction tank)
FIG. 4 is an explanatory diagram of the reaction tank 11 according to the present embodiment. The reaction tank 11 is a container that stores the sample liquid S1 and performs a process of taking out the measurement target substance contained in the sample liquid S1. For example, when the reaction tank 11 is used for a mercury meter, a process of converting mercury or a mercury compound contained in the sample liquid S1 into mercury gas in the reaction tank 11 is performed.

  The reaction tank 11 has a container body 12 and the lid unit 19 described above. In the figure, a state is shown in which a plurality of pipes L are airtightly fixed by the fixture 15 of the lid unit 19. The code | symbol attached | subjected to each piping respond | corresponds to the code | symbol of piping used by description of the measuring apparatus 1000 mentioned later.

  The container body 12 is a bottomed cylindrical container having an open upper end. In the present invention, the sample liquid S1 is stored in the container body. As long as the sample body S1 can be stored, the container body 12 can have various shapes depending on the type of measurement. For example, in order to increase measurement accuracy and measurement accuracy, a container body 12 as shown in the figure can be used.

  The container body 12 includes a cylindrical first member 12a having an opening 12x and the same inner diameter D1 as the opening 12x, and a bottomed cylindrical first member having an inner diameter D2 (D1> D2) smaller than the opening 12x. The two members 12b are formed in communication with each other. In the drawing, the connecting portion 12c between the first member 12a and the second member 12b having different inner diameters is shown as having an inverse taper shape in which the inner diameter gradually decreases from the first member 12a toward the second member 12b. Moreover, the upper end of the container main body 12 has an annular portion 121 protruding from the outer wall in a direction intersecting with the extending direction of the container main body 12.

  On the lower end side of the second member 12b, a tapered portion 12d whose inner diameter gradually decreases from D2 is provided, and the lower end portion has a rounded shape. Since the lower end side has a shape in which such a tapered portion 12d and a rounded lower end portion are combined, in the container main body 12, after the sample liquid S1 is sucked out from the internal space of the container main body 12, The amount of remaining sample liquid is reduced. Therefore, the measurement accuracy of the sample solution S1 can be increased, and the measurement accuracy of the measurement target substance contained in the sample solution S1 can be increased.

  As the forming material of the container main body 12, various materials can be used as long as they do not cause a change that affects the measurement result such as alteration or dissolution in the processing of the sample liquid S1. Especially, the container main body 12 which uses glass as a forming material is preferable because it is easy to visually confirm the reaction occurring in the inner space and is inexpensive.

  In the container body 12, for example, the inner diameter D1 of the first member 12a is 30 mm, the inner diameter D2 of the second member 12b is 14 mm, and the overall height is 137 mm.

  FIG. 5 is an explanatory diagram showing a state in which the reaction tank 11 is fixed to another member. In the figure, the reaction tank 11 is shown fixed between the first locking member 91 and the second locking member 92.

  The first locking member 91 is a substantially cylindrical member having an annular shape in plan view provided larger than the container lid 13 in plan view. In the center of the first locking member 91, a circular through hole 911 that is larger than the connection portion 131 of the container lid 13 and smaller than the locking portion 139 in a plan view is provided. When the first locking member 91 is put on the container lid 13, the connection portion 131 is exposed from the through hole 911.

  Further, the first locking member 91 is provided with a concave portion 91a below. A female screw 91x is formed on the side wall of the recess 91a.

  The second locking member 92 is a substantially cylindrical member having an annular shape in plan view and provided larger than the container lid 13 in plan view. A through hole 921 into which the container main body 12 is inserted is provided at the center of the second locking member 92, and has a ring shape that is closed in plan view. The through hole 921 is larger than the first member 12a in plan view and smaller than the annular part 121, and the through hole 921 is smaller than the locking part 139 in plan view.

  The second locking member 92 is fixed to another member such as a base to which the reaction tank 11 is attached. The second locking member 92 is provided with a convex portion 92a that fits into the concave portion 91a. A male screw 92x is formed on the side wall of the convex portion 92a.

  Although the second locking member 92 has been described as an annular member closed in a plan view, it may be an annular member partially opened in a plan view.

  The container lid 13 is configured such that the fitting portion 132 is inserted into and fitted into the opening 12 x of the container main body 12 to constitute the reaction tank 11. The container body 12 of the reaction tank 11 is inserted into the through hole 921 from the convex portion 92a side of the second locking member 92. Further, the first locking member 91 is inserted into the first locking member 91 and the second locking member 92 by the female screw 91x with the locking portion 139 and the annular portion 121 of the container lid 13 being sandwiched between the first locking member 91 and the second locking member 92. 2 It is screwed to the male screw 92x of the locking member 92. In this way, the reaction vessel 11 can be fixed to another member.

  FIG. 6 is an explanatory diagram for explaining the effect of the container lid 13 described above, and is a diagram in which the container lid 13 is viewed in plan. 6A shows a conventional container lid 13Z in which through holes are arranged in a line along the circumferential direction, and FIG. 6B shows the container lid 13 (lid unit 19) of the present invention.

  First, as described above, the container lid 13 of the present embodiment is screwed with the fixture 15 that fixes the pipe in an airtight manner. Therefore, for example, when exchanging dirty piping at the time of maintenance inspection or when tightening the fixing tool 15 when it is suspected that the airtightness has been broken at the position of the fixing tool 15, use a tool. The operation | work which turns the tool 15 arises.

  However, in the case of the container lid 13 </ b> Z shown in FIG. 6A, there are no gaps for the tool T to enter because many fixing tools 15 are arranged in the circumferential direction. In addition, when the fixing tool 15 is rotated with the tool T, the tool T interferes with the surrounding fixing tool 15, so that the fixing tool 15 may not be removed.

  Furthermore, if it is going to provide a clearance gap between the fixing tools 15 so that the fixing tool 15 can be removed, it will be necessary to enlarge container lid 13Z itself or to reduce the number of through-holes.

  On the other hand, as shown in FIG. 6B, in the case of the container lid 13 of the present embodiment, the plurality of through holes are divided into the first connection part 131A and the second connection part 131B having different heights. Has been. Therefore, even when the same number of through holes as the container lid 13Z shown in FIG. Further, since the upper surface 131A1 of the first connecting portion 131A is higher than the second connecting portion 131B, when the fixing tool 15 attached to the first connecting portion 131A is turned with the tool T or the like, other fixing tools are used. 15 is difficult to interfere with.

  The second connection portion 131B is formed in a truncated cone shape, and the upper surface 131B1 is inclined in a tapered shape. Therefore, the upper end of the fixture 15 is inclined in the outer peripheral direction as compared with the case where the upper surface 131B1 is configured to be orthogonal to the vertical direction like the upper surface 131A1 of the first connecting portion 131A. Thereby, even when a large number of fixtures 15 are mounted, it is easy to ensure a gap for the tool T to enter.

  Furthermore, in the second connection portion 131B, the through hole is divided into two units α, and there is a sufficient distance between the divided units α (the relationship of W1> W2 shown in FIG. 2). ). Therefore, it is easy to ensure a gap for the tool T to enter, and a reduction in work efficiency can be suppressed.

  According to the container lid 13 having the above-described configuration, it is possible to provide a container lid that can connect a plurality of pipes and that can be easily detached and attached.

  Moreover, according to the lid unit 19 and the reaction tank 11 having the above-described configuration, it is possible to provide a lid unit and a reaction tank that can be easily maintained and inspected.

  In the present embodiment, the fitting portion 132 is inserted and fitted into the opening 12x of the container body 12, but this is not a limitation.

  FIG. 7 is a schematic cross-sectional view showing a modified example of the container lid.

  The container lid 17 shown in FIG. 7A includes a connection part 171 to which piping is connected, and a fitting part 172 that fits into the opening 12x of the container body 12 and closes the opening 12x. . The connection unit 171 can have the same configuration as the connection unit 131 described above.

  The fitting portion 172 is formed, for example, in a cylindrical shape, and has an internal thread 172x formed therein. A male thread 12y is formed on the outer peripheral surface of the container body 12 on the opening 12x side. In the container lid 17 having such a configuration, the container main body 12 is inserted into the fitting portion 172, and the fitting portion 172 covers the opening 12 x of the container main body 12 and is screwed, thereby airtightly closing the container main body 12. To do.

  In such a fitting part 172, it is not limited to the structure screwed with respect to the container main body 12. FIG. For example, an O-ring may be provided on the outer periphery of the container body 12, and the container body 12 may be inserted and fitted inside the fitting portion 172. In such a configuration, the fitting portion 172 does not have to be cylindrical.

  The container lid 18 shown in FIG. 7B includes a connection part 181 to which piping is connected, and a fitting part 182 that fits into the opening 12x of the container body 12 and closes the opening 12x. . The connection unit 181 can have the same configuration as the connection unit 131 described above. In the container lid 18, the fitting portion 182 hermetically closes the container main body 12 while contacting both the inside and the outside of the opening 12x.

  In the container lid, the container body may be hermetically closed as in the above-described modification.

  In the present embodiment, the plurality of second through holes H2 are provided along the side surface of the virtual cone VC. However, the present invention is not limited to this. For example, the plurality of second through holes H2 may be formed so as to be inclined in the same direction along the circumferential direction of the second virtual circle IC2 from the arrangement along the side surface of the virtual cone VC. In such a container lid, the plurality of second through holes H2 are formed in a spiral shape in plan view.

  Further, in the present embodiment, in explaining the arrangement of the plurality of second through holes H2, the virtual cone VC is provided along the side surface of the virtual cone VC. However, the virtual cone VC is strictly defined by a mathematical definition. It does not have to be a regular cone.

  In the present embodiment, in describing the arrangement of the first opening H1x, which is the opening of the first through hole H1, the first virtual circle IC1 is assumed and the second opening H2x is the opening of the second through hole H2. In describing the arrangement of the two openings H2x, the second virtual circle IC2 is assumed, and in describing the arrangement of the openings 13y, the third virtual circle IC3 is assumed. However, the first virtual circle IC1 and the second virtual circle are assumed. The IC2 and the third virtual circle IC3 do not have to be a strict exact circle according to a mathematical definition.

  Even with such a container lid, collision between the pipes inserted into the first through hole and the second through hole can be suppressed, and the pipe is inserted in a desired posture (tilt with respect to the vertical direction, tip position). can do.

(measuring device)
FIG. 8 is an explanatory diagram of a measuring apparatus 1000 having the reaction tank 11 according to the present embodiment. In the present embodiment, a mercury meter will be described as an example of the measuring device.

  The measuring device 1000 is a device that quantifies mercury and mercury compounds contained in the sample liquid S1. As shown in the figure, the measuring device 1000 includes a pretreatment device 500 that converts mercury and mercury compounds in the sample liquid S1 into mercury gas, and a detector 4 that detects mercury gas generated in the pretreatment device 500. I have.

  The pretreatment device 500 is a device that converts mercury and a mercury compound contained in the sample liquid S1 into mercury gas. As shown in the figure, the pretreatment apparatus 500 includes a reaction vessel 11, a sample solution introduction unit 20, a decomposition reagent introduction unit 30, a mercury reduction reagent introduction unit 40, a ventilation unit 50, a control unit 80, It has.

  The detector 4 is an atomic absorption analyzer. A low-pressure mercury discharge tube can be used as the light source of the detector 4. A photodiode can be used as the light receiver of the detector 4. The detection wavelength is preferably 230 to 270 nm. For example, it can be 254 nm.

  The pretreatment device 500 and the measurement device 1000 are configured by appropriately combining a plurality of pipes, a plurality of valves, a plurality of pumps, and a plurality of tanks. In the following explanation, after first explaining each of these members, each means constituted by combining these members will be explained.

  It is preferable that all of the pipes L1 to L7, the pipes L10 to L14, and the pipes L21 to L29 are made of soft tubes. Appropriate materials are selected for the material of each pipe in consideration of heat resistance, chemical resistance, and the like. For example, thermoplastic resins such as Farmed (registered trademark) tubes can be used as the pipes L1 to L6, and ethylene tetrafluoride tubes can be used as the pipes L7, L10 to L14, and L21 to L29. The thickness of each pipe can be determined as appropriate in consideration of the amount of liquid to be fed and the pipe resistance. For example, a pipe having an outer diameter of 3 mm and an inner diameter of 2 mm can be used.

Of the valves V1 to V10, the valves V1, V4, V6 and V7 are three-way valves, and the other are two-way valves.
Valves V1, V4, V6 and V7 are shown as white triangles with normally open ports, black triangles with normally closed ports, half white and half with black triangles. is there.
Among the two-way valves, the valves V5 and V8 indicated by two white triangles are normally open valves, and the valves V2, V3, V9 and V10 indicated by two black triangles are normally closed valves.

  All of the pumps P1 to P9 are peristal type pumps. Peristal type pumps use a roller to squeeze a soft tube with liquid or feed air, and are also called tube pumps or roller pumps. By reversing the direction of ironing with a roller, the direction of liquid feeding or air feeding can be reversed. A peristal pump (registered trademark) can be used as a commercially available peristal pump. The pump P10 is a diaphragm type air pump.

  The tanks T1 to T9 are tanks that store liquids such as the sample liquid S1 and the decomposition reagent. As the tanks T <b> 1 to T <b> 9, various commercially available products can be used as long as they do not corrode or change due to the stored liquid.

(Ventilation means)
The aeration means 50 is used for gasifying metal mercury generated in the reaction tank 11. The ventilation means 50 includes pipes L22, L24, L26, a gas introduction pipe L23, a gas discharge pipe L25, valves V2 to V5, V8, V9, and a pump P10.

The gas introduction pipe L <b> 23 is connected to a common port of the valve V <b> 4 whose upstream end is a three-way valve, and its downstream end is inserted into the reaction tank 11. The downstream end of the gas introduction pipe L <b> 23 is disposed in the vicinity of the lowermost part of the reaction tank 11.
The gas introduction pipe L23 penetrates the lid unit 19 of the reaction tank 11 while maintaining airtightness.

  The decomposition tank 2 is provided in the middle of the gas introduction pipe L23. Further, a valve V3 is provided on the upstream side and a valve V2 is provided on the downstream side so as to sandwich the decomposition tank 2.

  The pipe L22 has one end released to the atmosphere as an upstream end, and the downstream end is connected to a normally closed port of a valve V4 that is a three-way valve.

The gas discharge pipe L25 has an upstream end inserted into the reaction tank 11 and a downstream end serving as an exhaust port. The upstream end of the gas discharge pipe L25 is disposed at a position above the liquid surface when the total volume of the sample liquid S1 and the reagents 1 to 5 is introduced into the reaction tank 11.
The gas discharge pipe L25 penetrates the lid unit 19 of the reaction tank 11 in an airtight vicinity in the vicinity of the upstream end thereof.

  In the middle of the gas discharge pipe L25, a dehumidifier 3, a normally closed valve V9, a detector 4, and a pump P10 are provided in this order from the upstream side. A branch point g is provided between the valve V9 and the detector 4. As the dehumidifier 3, for example, an electronic cooling type can be used.

The pipe L26 has one end released to the atmosphere as an upstream end and the downstream end connected to the branch point g.
A valve V8 that is a normally open valve is provided in the middle of the pipe L26.

One end of the pipe L24 is opened to the atmosphere, and the other end is inserted into the reaction tank 11. The other end of the pipe L24 is disposed at a position above the liquid surface when the total volume of the sample liquid S1 and the reagents 1 to 5 is introduced into the reaction tank 11.
The pipe L24 penetrates the lid unit 19 of the reaction tank 11 while maintaining airtightness.
A valve V5 which is a normally open valve is provided in the middle of the pipe L24.

(Sample solution introduction means)
The sample solution introducing means 20 is used for introducing the sample solution S1 into the reaction vessel 11. The sample solution introducing means 20 has pipes L7, L11 to L14, valves V1 and V7, tanks T7 to T9, and a pump P7.

  The sample liquid S1 is stored in the tank T7, pure water is stored in the tank T8, and the cleaning liquid is stored in the tank T9.

  The pipe L7 is connected to the common port of the valve V7 whose upstream end is a three-way valve, and the downstream end is inserted into the reaction tank 11. The downstream end of the pipe L7 is arranged at a position above the liquid level when the total volume of the sample liquid S1 and the reagents 1 to 5 is introduced into the reaction tank 11.

The pipe L7 penetrates through the lid unit 19 of the reaction tank 11 in the vicinity of the downstream end thereof while maintaining airtightness.
A pump P7 is provided in the middle of the pipe L7.

  The pipe L11 has an upstream end connected to a common port of the valve V1, which is a three-way valve, and a downstream end connected to a normally open port of the valve V7, which is a three-way valve. The pipe L12 has an upstream end inserted into the sample liquid S1 accommodated in the tank T7, and a downstream end connected to the normally open port of the valve V1. The tank T7 is a water receiving tank, and a new sample solution S1 always flows in.

  The pipe L13 has an upstream end inserted into pure water accommodated in the tank T8, and a downstream end connected to the normally closed port of the valve V1. The pipe L14 has an upstream end inserted into the cleaning liquid stored in the tank T9, and a downstream end connected to the normally closed port of the valve V7. An alkaline solution is used as the cleaning liquid. As the alkaline solution, a sodium hydroxide solution or a potassium hydroxide solution is preferable. In this embodiment, it is a sodium hydroxide solution, specifically a 4 g / L sodium hydroxide solution.

(Introduction means such as decomposition reagents)
The decomposing reagent introduction means 30 is used to introduce the sample solution S1 into the reaction vessel 11. The decomposing reagent introduction means 30 has pipes L1 to L5, L10 and L21, a valve V10, tanks T1 to T5, and pumps P1 to 5 and P8.

The reagent 1 is stored in the tank T1. The reagent 1 is a sulfuric acid solution that is one of the decomposition reagents in the present invention, and specifically, a (1 + 1) sulfuric acid solution.
The reagent 2 is stored in the tank T2. The reagent 2 is a nitric acid solution that is one of the decomposing reagents in the present invention, specifically, a (1 + 3) nitric acid solution.
The reagent 3 is stored in the tank T3. The reagent 3 is a potassium permanganate solution that is one of the decomposition reagents in the present invention, and specifically a 50 g / L potassium permanganate solution.
The reagent 4 is stored in the tank T4. Reagent 4 is a sodium peroxodisulfate solution or potassium peroxodisulfate solution, which is one of the decomposition reagents in the present invention, specifically, a 50 g / L sodium peroxodisulfate solution or a 50 g / L potassium peroxodisulfate solution. is there.
The reagent 5 is stored in the tank T5. The reagent 5 is a hydroxylamine hydrochloride solution, specifically, an 80 g / L hydroxylamine hydrochloride solution.

  The pipe L21 has one end released to the atmosphere as an upstream end, and the downstream end is connected to a normally open port of a valve V4 that is a three-way valve. A pump P8 is provided in the middle of the pipe L21. A branch point f is provided on the downstream side of the pump P8.

The pipe L10 has a branch point f in the middle of the pipe L21 as an upstream end, and the downstream end is inserted into the reaction vessel 11. The downstream end of the pipe L10 is arranged at a position below the liquid level when the sample liquid S1 is introduced into the reaction tank 11.
The pipe L10 passes through the lid unit 19 of the reaction tank 11 in the vicinity of the downstream end thereof while maintaining airtightness.

A valve V10 that is a normally closed valve is provided in the vicinity of the upstream end of the pipe L10.
A branch point a, a branch point b, a branch point c, a branch point d, and a branch point e are provided downstream from the position where the valve V10 of the pipe L10 is provided.
The pipe L1 is connected to the branch point a, the pipe L2 is connected to the branch point b, the pipe L4 is connected to the branch point c, the pipe L5 is connected to the branch point d, and the pipe L3 is connected to the branch point e. .

  The upstream end of the pipe L1 is inserted into the reagent 1 accommodated in the tank T1, and the branch point a is the downstream end. A pump P1 is provided in the middle of the pipe L1.

The upstream end of the pipe L2 is inserted into the reagent 2 accommodated in the tank T2, and the branch point b is the downstream end.
A pump P2 is provided in the middle of the pipe L2.

  The pipe L3 has an upstream end inserted into the reagent 3 accommodated in the tank T3, and the branch point e is the downstream end. A pump P3 is provided in the middle of the pipe L3.

  The pipe L4 has an upstream end inserted into the reagent 4 accommodated in the tank T4, and the branch point c is the downstream end. A pump P4 is provided in the middle of the pipe L4.

  The upstream end of the pipe L5 is inserted into the reagent 5 accommodated in the tank T5, and the branch point d is the downstream end. A pump P5 is provided in the middle of the pipe L5.

(Mercury reducing reagent introduction means)
The mercury reducing reagent introduction means 40 is used to introduce a mercury reducing reagent into the reaction tank 11. The mercury reducing reagent introduction means 40 has a pipe L6, a tank T6, and a pump P6.

  The reagent 6 is stored in the tank T6. The reagent 6 is a tin (II) chloride solution, specifically, a 100 g / L tin (II) chloride solution.

  The pipe L6 has an upstream end inserted into the reagent 6 accommodated in the tank T6, and a downstream end inserted into the reaction tank 11. The downstream end of the pipe L6 is arranged at a position above the liquid surface when the total volume of the sample liquid S1 and the reagents 1 to 5 is introduced into the reaction tank 11.

  The pipe L6 passes through the lid unit 19 of the reaction tank 11 in the vicinity of the downstream end thereof while maintaining airtightness. A pump P6 is provided in the middle of the pipe L6.

(Sample solution discharge means)
The pretreatment apparatus 500 of this embodiment has a sample solution discharge means 70. The sample liquid discharge means 70 is used for discharging the sample liquid S1 introduced into the reaction tank 11 to the outside of the reaction tank 11. The sample solution discharge means 70 includes pipes L27 to L29, a valve V6, and a pump P9.

  The pipe L27 has one end connected to a normally open port of a valve V6 that is a three-way valve, and the other end inserted into the reaction tank 11. The other end of the pipe L27 is disposed in the vicinity of the lowermost portion of the reaction tank 11. The pipe L27 penetrates the lid unit 19 of the reaction tank 11 while maintaining airtightness.

  One end of the pipe L28 is connected to the common port of the valve V6, and the other end is a drain. A pump P9 is provided in the middle of the pipe L28.

One end of the pipe L29 is connected to the normally closed port of the valve V6, and the other end is inserted into the reaction tank 11. The other end (lower end) of the pipe L29 is a position below the liquid level when the total volume of the sample liquid S1 and the reagents 1 to 5 is introduced into the reaction tank 11, and the downstream end of the pipe L10. It is arrange | positioned in the position which becomes above.
The pipe L29 penetrates the lid unit 19 of the reaction tank 11 while maintaining airtightness.

(Control part)
The control unit 80 controls the sample solution introduction unit 20, the decomposition reagent introduction unit 30, the mercury reducing reagent introduction unit 40, the aeration unit 50, the transfer unit 60, and the sample solution discharge unit 70 described above. Specifically, the control unit 80 controls the opening and closing of the valves included in each unit and the operation and stop of the pump.

(How to use the measuring device)
The measuring apparatus 1000 having such a configuration is used as follows, for example.

In the following description, the pumps P1 to P9 are not operating unless otherwise specified. The pump P10 is always operating.
Further, in the following description, operating the pumps P1 to P8 means sending or feeding liquid toward the reaction tank 11, and operating the pumps P1 to P6 and P8 in reverse means that the reaction tank 11 is operated. It means that liquid is sent or air is sent in the opposite direction. In addition, operating the pump P9 means sending the liquid in the direction opposite to the reaction tank 11. The pump P10 is constantly supplying air in the direction opposite to the reaction tank 11.
When the pumps P1 to P9 are not operating, neither gas nor liquid is circulated, and the pumps P1 to P9 are kept airtight or liquidtight.

  In the following description, the valve is not operated unless otherwise specified. In addition, operating the three-way valve means that the common port and the normally closed port of the three-way valve can flow, and stopping the operation of the three-way valve means that the common port and the normally open port of the three-way valve are not connected. It means returning to a state where it can be distributed. In addition, operating the normally open valve means disabling the flow between the two ports, and stopping the operation of the normally open valve means returning to a state where the both ports can flow. Further, operating the normally closed valve means enabling the flow between the two ports, and stopping the operation of the normally closed valve means returning to a state where the both ports cannot flow.

  First, the pump P7 of the sample solution introduction means 20 is operated to introduce the sample solution S1 in the tank T7 into the reaction vessel 11. The flow rate and operation time of the pump P7 are sufficient flow rate and operation time for the liquid level of the sample liquid S1 introduced into the reaction tank 11 to be higher than the height of the lower end of the pipe L29.

  Thereafter, the pump P7 is stopped, the valve V6 and the pump P9 are operated, the sample liquid S1 in the reaction tank 11 is sucked from the lower end of the pipe L29 and discharged from the pipe L28, and the liquid level of the sample liquid S1 in the reaction tank 11 Is lowered to the height of the lower end of the pipe L29. Thereby, a fixed amount of sample liquid S1 can be measured to the reaction tank 11. FIG.

  Next, the reagent 1 to the reagent 4 which are decomposition reagents are sequentially introduced into the reaction tank 11 using the decomposition reagent introduction means 30. The amount of each reagent to be introduced is set to a predetermined amount sufficient to decompose the mercury compound that may be present in the sample solution S1 into mercury (II) ions.

  First, in order to introduce the reagent 1, the pump P1 is operated. Thereby, the reagent 1 is pushed out from the pipe L1 and filled into the pipe L10. The flow rate and operation time of the pump P1 are set so that the reagent 1 is filled in the pipe L10 by a predetermined amount.

  Next, the operation of the pump P1 is stopped, and the pump P8 is operated with the valve V10 being operated. Thereby, the reagent 1 with which the piping L10 was filled is discharged to the reaction tank 11 with pressurized air.

  Hereinafter, the reagent 2 to the reagent 4 are similarly introduced into the reaction tank 11 using the pump P8, the valve V10, and pipes and pumps connected to the tanks in which the respective reagents are stored.

Next, the liquid (sample liquid S1 and decomposition reagent) in the reaction tank 11 is introduced into the decomposition tank 2 using the pump P8 and heated.
Specifically, the liquid in the reaction tank 11 is transferred to the decomposition tank 2 by reversing the pump P8 while the valves V2 and V3 are operated. Thereafter, in the decomposition tank 2, the liquid is heated at 100 ° C. for 20 to 30 minutes.

While the liquid is heated in the decomposition tank 2, the reaction tank 11 is washed in parallel. Specifically, the pump P7 is operated with the valve V1 operated to introduce pure water from the tank T8 into the reaction tank 11. The operation of the pump P7 continues for a time sufficient for the level of pure water introduced into the reaction tank 11 to be higher than the level of the mixed liquid of the sample liquid S1 and the reagents 1 to 4.
Then, after stopping the operation of the pump P7 and the valve V1, the pump P9 is operated, and almost all of the pure water in the reaction tank 11 is discharged.
Thereby, the inside of the reaction vessel 11 can be emptied while being washed.

  Next, the reagent 5, which is a hydroxylamine hydrochloride solution, is introduced into the reaction vessel 11 using the decomposition reagent introduction means 30. The introduction method of the reagent 5 is the same as that of the reagents 1-4 mentioned above.

  Thereafter, the decomposition solution S2 obtained in the decomposition tank 2 is introduced into the reaction tank 11 by operating the valves V2, V3 and the valve V4. The potassium permanganate remaining in the dropped decomposition solution S2 reacts with the reagent 5 introduced into the reaction tank 11 and is reduced. The decomposition liquid S2 is cooled to about 50 ° C. using a fan (not shown).

  Next, the reagent 6 which is a tin (II) chloride solution is introduced into the reaction vessel 11 using the mercury reducing reagent introduction means 40. For introduction of the reagent 6, a pump P6 is used. As a result, the reagent 6 is pushed out from the pipe L6 and discharged into the reaction tank 11. By the reagent 6, mercury (II) ions contained in the decomposition solution S2 are reduced to metal mercury.

  Next, mercury gas is generated by gasifying the metal mercury generated in the decomposition solution S2 using the ventilation means 50. In the measuring apparatus 1000 of the present embodiment, mercury gas is generated and the generated mercury gas is sent to the detector 4 outside the reaction tank 11.

  Specifically, the valves V2 to V5, V8, and V9 are operated, and the pump P10 is operated. Thereby, the inside of the reaction tank 11 is set to a negative pressure, air is drawn in from the upstream end of the pipe L22 released to the atmosphere, and bubbles are bubbled into the decomposition solution S2 through the gas introduction pipe L23. As a result, metallic mercury contained in the decomposition solution S2 can be transferred to the gas phase as mercury gas.

  The mercury gas transferred to the gas phase is discharged to the outside of the reaction tank 11 through the gas discharge pipe L25. The mercury gas is dehumidified by the dehumidifier 3 and then introduced into the detector 4. As a result, mercury or a mercury compound present in the sample solution S1 can be detected as mercury gas.

  Since the measuring apparatus 1000 having the above configuration uses the reaction tank 11 according to one aspect of the present invention, maintenance and inspection are facilitated.

  Moreover, in the said embodiment, although the mercury meter was mentioned as a structural example, it is not restricted to this. The container lid, the lid unit, and the reaction tank of the present invention can be used in other measuring devices for various substances to be measured such as COD, phosphoric acid, nitric acid, and volatile hydride.

  The preferred embodiments of the present invention have been described above with reference to the accompanying drawings, but it goes without saying that the present invention is not limited to such examples. Various shapes, combinations, and the like of the constituent members shown in the above-described examples are examples, and various modifications can be made based on design requirements and the like without departing from the gist of the present invention.

  C ... center, 11 ... reaction vessel, 12 ... container body, 12a ... first member, 12b ... second member, 12x, 13y ... opening, 12y, 15x, 92x ... male screw, 13, 13H, 13Z, 17, 18 ... Container lid, 13a, 911, 921 ... Through hole, 13x, 91x, 172x ... Female thread, 15 ... Fixing tool, 15a ... Insertion hole, 19 ... Lid unit, CA ... Central axis, D1, D2 ... Inner diameter, H1 ... No. 1 through hole, H1x ... first opening, H2 ... second through hole, H2x ... second opening, L1, L2, L3, L4, L5, L6, L7, L10, L11, L12, L13, L14, L21 , L22, L24, L26, L27, L28, L29 ... piping, L23 ... gas introduction pipe, L25 ... gas discharge pipe, VC ... virtual cone, 131, 171, 181 ... connection part, 132, 172, 182 ... fitting part 131 ... first connecting portion, 131B ... second connecting portion

Claims (8)

A container lid provided with a plurality of through-holes for closing the opening provided at the upper end of the container body and inserting a pipe into the container body,
A first connecting portion provided in the center in plan view;
A second connection portion provided around the first connection portion in plan view,
The first connection portion is formed such that an upper surface of the first connection portion is higher than the second connection portion,
The plurality of through holes are a first through hole provided in parallel with the vertical direction;
A second through hole provided obliquely with respect to the first through hole,
An upper end of the first through hole opens at the first connection portion,
The upper end of the second through hole opens at the second connection portion ,
The first opening which is the opening at the upper end of the first through hole is arranged along a first virtual circle set in the first connection part in plan view,
The second opening, which is the opening at the upper end of the second through hole, is set along the second virtual circle that is set in the second connection portion and is concentric with the first virtual circle in plan view. lid. The plurality of through holes include a plurality of the second through holes,
The plurality of second through holes, the container lid of claim 1, which is arranged along the side of the virtual cone to the rotation axis of the axial center is parallel to the through vertical direction of the concentric circles. A plurality of the second openings are formed in the second connection portion,
The plurality of second openings are divided into a plurality of units,
Each of the units is composed of two second openings adjacent to each other along the circumferential direction of the second virtual circle,
The container lid according to claim 2 , wherein a separation distance between two units adjacent to each other in the circumferential direction is longer than a separation distance between two second openings included in the unit. A plurality of the first openings are formed in the first connection portion,
When an arc that overlaps the second virtual circle is assumed between the two units adjacent to each other along the circumferential direction,
4. The container lid according to claim 3 , wherein the first opening is disposed in a fan-shaped region surrounded by the arc and a line segment connecting both ends of the arc and the center of the concentric circle.   Located below the first connection part and the second connection part, and having a fitting part that fits into the opening part and closes the opening part,
  The opening at the lower end of the first through hole and the opening at the lower end of the second through hole are set on the lower surface of the fitting portion along a third virtual circle that is concentric with the first virtual circle. The container lid according to any one of claims 1 to 4, which is arranged. A container lid according to any one of claims 1 to 5;
A fixing tool for hermetically fixing the pipe to each of the plurality of through holes provided in the container lid,
The through hole has a female screw formed therein,
The fixing device has an insertion hole into which the pipe is inserted, a male screw is formed on the outer periphery, and the lid unit is screwed to the through hole. A bottomed cylindrical container body with an open top;
And a lid unit according to claim 6 that hermetically closes the opening at the upper end. The container main body communicates with a cylindrical first member having the opening and having the same inner diameter as the opening, and a bottomed cylindrical second member having an inner diameter smaller than the opening. And
The reaction tank according to claim 7, wherein the opening of the first through hole of the container lid of the lid unit and the second member overlap each other in plan view.

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