JP6590897B2 - Jig for mounting coiled specimen - Google Patents

Description

  The present invention relates to a coiled sample collection piece mounting jig for mounting a coiled sample collection piece on a sampling unit for collecting a sample used in an analysis method such as gas chromatography-mass spectrometry.

  Conventionally, a metal microcoil as a sampling piece is attached to a sampling rod of a sampling unit that directly collects a liquid sample or a solid sample of fine powder used in a thermal analysis method such as evolved gas analysis or pyrolysis gas chromatograph-mass spectrometry. A welded sampling unit has been proposed (see Non-Patent Document 1).

Kaneko et al., "Trial production of GC sampling device using microcoil and its application", BUNSEKI KAGAKU, Vol.4, No.5, pp.365-369 (2015)

  In the sampling unit described in Non-Patent Document 1, it is conceivable that the surface of the metal microcoil is deactivated and covered with a resin. When doing so, if the polarity of the resin that covers the surface of the deactivated metal microcoil is different, the sample that is adsorbed and absorbed by the resin is also different. It is considered that various components in the sample can be selectively analyzed by using different samples.

  However, in the conventional sampling unit, since the metal microcoil is welded to the sampling rod, in order to use different resins with different polarities depending on the analysis object, sampling is performed for each resin polarity. Different sampling units must be prepared. Therefore, the metal microcoil can be detachably attached to the tip of the sampling rod, and a plurality of the metal microcoils are prepared for each polarity of the resin. It is conceivable to attach the appropriate metal microcoil to the tip of the sampling rod.

  However, the metal microcoil has a length of 2 to 20 mm, an inner diameter of 0.15 to 0.3 mm, and an outer diameter of 0.17 to 0.36 mm. The diameter is 0.13 using tweezers or the like. There is an inconvenience that a high degree of skill is required to attach to the sampling rod having a sharp tip connected to a base of ˜0.15 mm.

  The present invention eliminates such inconvenience, and allows a coiled sample sampling piece to be easily attached to the tip of the sampling rod of the sampling unit by a metal coil as a coiled sampling piece. An object is to provide a mounting jig.

  In order to achieve such an object, the coiled sample collection piece mounting jig of the present invention is a coiled sample collection piece mounting jig for attaching a coiled sample collection piece to the tip of the sampling rod of the sampling unit. A cylindrical jig main body, a first guide portion that gradually decreases in diameter in the axial direction from the one end side of the jig main body, and the other end side of the jig main body. A second guide portion that gradually decreases in diameter in the axial direction, a communication hole that communicates the first guide portion and the second guide portion, and the sampling rod guides to the first guide portion. When the coiled sample collection piece guided from the second guide portion to the communication hole is pushed toward the sample collection rod when inserted into the communication hole, the tip of the sample collection rod is The coiled sample is press-fitted into the coiled sample collecting piece and is attached to the tip of the sample collecting rod. Characterized in that it comprises a pressing member for mounting the Tohen.

  In the coiled sample collection piece mounting jig of the present invention, first, the sample collection rod of the sampling unit is inserted into the communication hole by being guided by the first guide portion. By doing so, the coiled sample collection piece mounting jig of the present invention is mounted on the sample collection rod.

  Next, with respect to the sample collection rod inserted into the communication hole, a coiled sample collection piece is guided to the communication hole via the second guide portion, so that the sample collection rod is formed in the communication hole. The coiled sample-collecting piece is made to face the tip of the plate.

  Next, when the coiled sample collection piece is pressed in the direction of the sample collection rod by the pressing member, the coiled sample collection piece is opposed to the tip of the sample collection rod in the communication hole. The tip of the rod is press-fitted into the coiled sample collection piece. Therefore, according to the coiled sample collection piece mounting jig of the present invention, anyone can easily attach the coiled sample collection piece to the tip of the sample collection rod without requiring skill. .

  In the coiled specimen mounting jig of the present invention, the sampling unit includes, for example, a hollow cylindrical cylinder having a cylindrical connecting portion at the tip, and a slidable push along the inner wall of the cylinder It is possible to use a syringe comprising a member, a cylindrical needle communicating with the cylinder via the connecting portion, and a sampling rod connected to the distal end of the pushing member and freely retractable from the needle. .

  In the coiled sample collection piece mounting jig of the present invention, when the sampling unit includes the syringe, the communication hole communicates with a large diameter portion communicating with the first guide portion and the second guide portion. A small-diameter portion, and the large-diameter portion preferably has a length capable of accommodating the needle. As a result, in a state where the needle is accommodated in the large diameter portion, the push member is pushed to cause the sample collection rod to protrude from the tip of the needle and enter the small diameter portion. Then, by guiding the coiled sample collection piece through the second guide portion into the small diameter portion of the communication hole, the coiled sample collection piece is surely opposed to the tip of the sample collection rod. Can do.

  The coiled sample collection piece mounting jig of the present invention includes, for example, a base portion in which the sample collection rod has a diameter in a range of 0.13 to 0.15 mm, and a sharp tip portion connected to the base portion, It can be suitably used when the coiled sample collection piece has an inner diameter in the range of 0.15 to 0.3 mm and an outer diameter in the range of 0.17 to 0.36 mm.

The typical sectional view showing the example of 1 composition of the gas phase ingredient analyzer. A is a schematic cross-sectional view showing one configuration example of a sampling unit on which a coiled sample collection piece is mounted, and B is a schematic cross-sectional view showing a state in which the coiled sample collection piece is accommodated in the sampling unit of A. The typical sectional view showing the example of 1 composition of the jig for coiled sample collection piece attachment of the present invention. 1 shows a method of using a jig for mounting a coiled sample collection piece of the present invention, wherein A is a schematic cross-sectional view showing a state in which a coiled sample collection piece is opposed to the tip of a sample collection rod in a communication hole, and B is a coil Schematic cross-sectional view showing a state where the pressing member is prepared to press the sample sample piece, C is a schematic cross-sectional view showing a state where the coiled sample piece is pressed by the pressing member and attached to the tip of the sample collecting rod. . The typical sectional view showing other examples of composition of the jig for coiled sample collection piece attachment of the present invention.

  Next, embodiments of the present invention will be described in more detail with reference to the accompanying drawings.

  As shown in FIG. 1, a gas phase component analyzer 1 used for an analysis method such as gas chromatograph-mass spectrometry includes a thermostat 10, a heating unit 11 provided above the thermostat 10, and an opening of the heating unit 11. From a septum 12 that closes the end, a carrier gas introduction pipe 13 connected to the heating unit 11 outside the thermostat 10, a separation column 14 such as a capillary column disposed inside the thermostat 10, and a mass spectrometer And a detecting unit 15. The separation column 14 is connected to the lower end of the heating unit 11 at one end and is connected to the detection unit 15 at the other end. Moreover, the heater 16 is arrange | positioned inside the heating part 11, and the split vent pipe 17 is connected to the lower part.

  According to the gas phase component analyzer 1, a sample introduced by the sampling unit 2 punctured in the septum 12 is heated by the heater 16 in the heating unit 11, thereby generating a gas phase component composed of a mixture of a plurality of compounds. Let The generated gas phase component is introduced into the separation column 14 by the carrier gas introduced from the carrier gas introduction pipe 13.

  At this time, the split vent pipe 17 opens part of the on-off valve 18 to discharge a part of the gas phase component generated in the heating unit 11 and adjust the amount of the gas phase component introduced into the separation column 14. can do. When the amount of the gas phase component is very small, the entire amount of the generated gas phase component may be introduced into the separation column 14 by closing the on-off valve 18 of the split vent pipe 17.

  The thermostatic chamber 10 is heated to a predetermined temperature, and the gas phase component is separated into each compound constituting the gas phase component by the separation column 14 at the predetermined temperature. Then, each separated compound is detected by the detection unit 15.

  For example, as shown in FIG. 2A, the sampling unit 2 is attached to a cylindrical cylinder 20, a plunger 21 as a pushing member that is slidable along the inner wall of the cylinder 20, and the tip of the cylinder 20. A syringe 24 including a cylindrical connecting portion 22 and a cylindrical needle 23 connected to the tip of the cylinder 20 via the connecting portion 22 is provided.

  The plunger 21 includes a gasket 25 at the tip, and the base end portion of the sampling rod 26 is fixed to the gasket 25. The sample collection rod 26 is moved forward and backward by the plunger 21 so as to be able to protrude and retract from the needle 23, and a metal coil 27 as a coiled sample collection piece is attached to the distal end portion 26 a of the sample collection rod 26. .

  In addition, the cylinder 20 includes a retaining portion 28 that is screwed to the proximal end portion side of the gasket 25. The tip of the retaining portion 28 protrudes into the cylinder 20 and acts as a retainer for the plunger 21 when the gasket 25 abuts. The retaining portion 28 may be configured such that a part of the cylinder 20 is melted and protruded to the inside, or the tip of a screw or the like may be protruded to the inside of the cylinder 20.

  In the sampling unit 2, the sampling rod 26 has, for example, a base having a diameter in the range of 0.13 to 0.15 mm and a sharp tip 26a connected to the base. On the other hand, the metal coil 27 is formed by spirally winding a metal wire such as stainless steel, has a length of 2 to 20 mm, has an inner diameter in the range of 0.15 to 0.3 mm, and 0.17 to And an outer diameter in the range of 0.36 mm. The metal coil 27 may include an undercoat layer that covers and inactivates the surface of the metal coil 27, and a resin coating layer that covers the surface of the undercoat layer. You may provide the filler which consists of adsorption agents, such as resin filled with the space enclosed, or activated carbon.

The undercoat layer may be any material as long as it can coat and inactivate the surface of the metal coil 27. For example, a silicon coating layer, a quartz coating layer, a titanium coating layer, etc. Can be mentioned. Further, the resin coating layer and the resin filler are made of a soft resin capable of adsorbing and absorbing a sample, and resins having different polarities can be used depending on the analysis target, and are identified for each polarity of the resin. Colored possible. The coloring can be performed, for example, by mixing the resin coating layer with an inorganic pigment capable of maintaining the molecular structure when heated by the heating unit 11. The metal coil 27 is surrounded by a spiral metal wire. The sharp tip of the sample collection rod 26 is press-fitted into the space to be mounted on the tip portion 26 a of the sample collection rod 26. In addition, when the space is filled with the resin filling material made of a soft resin, the metal coil 27 is formed by puncturing the sharp tip portion 26a of the sampling rod 26 in the resin filling material. 26 is attached to the distal end portion 26a.

  As shown in FIG. 2A, the sampling unit 2 pushes the plunger 21 to advance the sample collection rod 26, thereby moving the tip 26a of the sample collection rod 26 and the metal coil 27 attached to the tip 26a. It can be made to protrude from the needle 23. Further, as shown in FIG. 2B, the sampling unit 2 pulls the plunger 21 to retract the sample collection rod 26, whereby the tip 26a of the sample collection rod 26 and the metal coil 27 attached to the tip 26a are removed. It can be accommodated in the needle 23.

  Next, FIG. 3 shows a coiled sample collection piece mounting jig 31 according to the first aspect of the present embodiment. The coil-shaped sample collection piece mounting jig 31 of the first aspect is a jig for mounting the metal coil 27 on the tip end portion 26a of the sample collection rod 26 of the sampling unit 2 shown in FIG. 2, and is made of metal. A first guide portion 33 that gradually decreases in diameter in the axial direction from one end side of the columnar jig main body 32, and gradually from the other end side of the jig main body 32 in the axial direction. A second guide portion 34 having a reduced diameter, and a communication hole 35 communicating the first guide portion 33 and the second guide portion 34 are provided.

  The communication hole 35 includes a large-diameter portion 36 that communicates with the first guide portion 33 and a small-diameter portion 37 that communicates with the second guide portion 34, and the small-diameter portion 35 of the second guide portion 34. The opposite end communicates with a hole 38 having the same diameter as the end, and the hole 38 opens at the end of the jig body 32.

  The jig body 32 includes a protrusion 39 that protrudes to the side of the end on the side where the hole 38 opens, and a lid member 40 that closes the end on the protrusion 39. The lid member 40 is pivotally supported by a shaft 41 provided on the projection 39 and is provided with a pressing member 43 that presses the metal coil 27 in a through hole 42 provided in the center thereof. .

  The pressing member 43 includes a shaft portion 44 slidable along the inner wall of the through hole 42 and a head portion 45 provided at an end portion of the shaft portion 44 on the outer side of the lid member 40. As will be described later, when the pressing member 43 is pressed until the head 45 is in contact with the outer surface of the lid member 40, the metal coil 27 pressed by the shaft portion 44 is applied to the distal end portion 26 a of the sampling rod 26. It is configured to be mounted.

  The jig body 32 of the coiled sample collection piece mounting jig 31 is divided into, for example, a part having a large diameter part 36 and a part having a small diameter part 37, and drilling is performed for each of the large diameter part 36 and the first part. After forming the guide portion 33, the small diameter portion 37, the second guide portion 34, and the hole portion 38, one can be formed by screwing together with one being a male screw and the other being a female screw.

  Next, with reference to FIGS. 4A to 4C, a method of using the coiled sample collection piece mounting jig 31 shown in FIG. 3 will be described.

  When using the coiled sample collection piece mounting jig 31, first, as shown in FIG. 4A, the first guide portion 33 guides the needle 23 of the sampling unit 2 to the large diameter portion 36 of the communication hole 35. Insert into. At this time, the tip 26 a of the sample collection rod 26 is immersed in the needle 23. The large-diameter portion 36 has a slight clearance with respect to the outer peripheral surface of the needle 23 to be inserted. When the connection portion 22 of the sampling unit 2 is brought into contact with the inner surface of the first guide portion 33, the needle 23 has a length that does not reach the small diameter portion 37.

  If the needle 23 is inserted into the large-diameter portion 36 of the communication hole 35, then the plunger 21 is pushed to advance the sample collection rod 26, and the sample collection rod 26 is protruded from the needle 23 to make the small-diameter portion of the communication hole 35. On the other hand, the metal coil 27 is inserted from the hole 38 using tweezers or the like and guided to the small diameter portion 37 via the second guide portion 34.

  The small-diameter portion 37 has a slight clearance with respect to the outer peripheral surfaces of the sampling rod 26 and the metal coil 27. As a result, as shown in FIG. 4A, the distal end portion 26a of the sampling rod 26 in the small-diameter portion 37. The metal coil 27 is in a state of facing.

  Next, as shown in FIG. 4B, the lid member 40 is rotated with respect to the shaft 41 to close the opening of the hole 38, while the pressing member 43 is erected with respect to the jig body 32. State.

  4C, when the head 45 of the pressing member 43 is pressed until it abuts against the outer surface of the lid member 40, the tip of the shaft 41 that slides along the inner surface of the through hole 42 contacts the metal coil 27. The metal coil 27 is pressed in the direction of the sampling rod 26. As a result, the distal end portion 26 a of the sample collection rod 26 is press-fitted into a space surrounded by the spiral metal wire of the metal coil 27, and the metal coil 27 is attached to the distal end portion 26 a of the sample collection rod 26. When the metal coil 27 includes the resin filling body, the tip end portion 26a of the sample collection rod 26 is punctured into the resin filling body, and the metal coil 27 is attached to the tip end portion 26a of the sample collection rod 26. .

Next, FIG. 5 shows a coiled sample collection piece mounting jig 51 according to a second aspect of the present embodiment.
2 is a jig for attaching the metal coil 27 to the tip end portion 26a of the sampling rod 26 of the sampling unit 2 shown in FIG. A first guide portion 53 that gradually decreases in diameter in the axial direction from the one end portion side of the cylindrical jig main body 52, and from the other end portion side of the jig main body 52 in the axial direction. A second guide portion 54 that gradually decreases in diameter, and an inner cylinder 55 made of a synthetic resin that allows the first guide portion 53 and the second guide portion 54 to communicate with each other. It has become. Further, the end portion of the second guide portion 54 opposite to the communication hole 56 communicates with a hole portion 57 having the same diameter as the end portion, and the hole portion 57 opens at the end portion of the jig main body 52. is doing.

  The coiled sample collection piece mounting jig 51 has the inner cylinder 55 disposed on the outer peripheral side of the needle 23 of the sampling unit 2, while the second guide 54 and the end of the inner cylinder 55 opposite to the needle 23 are arranged. In a state where a member having the inner surface shape of the hole portion 57 is mounted, the whole can be covered with a tube made of a heat-shrinkable resin, and the tube can be heated and contracted.

  As in the case of the coiled sample collection piece mounting jig 31, the coiled sample collection piece mounting jig 51 is guided by the first guide portion 53, and the needle 23 of the sampling unit 2 is inserted into the communication hole 56. Inserting and pushing the plunger 21 to cause the sampling rod 26 to protrude from the needle 23, the metal coil 27 is inserted from the hole 57 and guided to the communication hole 56 via the second guide 54. Then, as shown in FIG. 5, after the metal coil 27 faces the tip end portion 26a of the sampling rod 26 in the communication hole 56, the metal coil 27 is moved in the direction of the sampling rod 26 by a pressing member (not shown). By pressing, the metal coil 27 is attached to the distal end portion 26 a of the sampling rod 26.

  2 ... Sampling unit, 23 ... Needle, 26 ... Sample collection rod, 27 ... Metal coil (coiled sample collection piece), 31 ... Jig for mounting coiled sample collection piece (first mode), 32 ... Jig body 33 ... 1st guide part, 34 ... 2nd guide part, 35 ... Communication hole, 36 ... Large diameter part, 37 ... Small diameter part 37, 43 ... Pressing member, 51 ... Jig for coiled sample collection piece mounting | wearing (1st aspect), 52 ... jig main body, 53 ... 1st guide part, 54 ... 2nd guide part, 56 ... Communication hole.

Claims (4)

A coiled sample collection piece mounting jig for mounting a coiled sample collection piece on the tip of a sampling rod of a sampling unit,
A cylindrical jig body, a first guide portion that gradually decreases in diameter in the axial direction from one end side of the jig body, and an axial direction from the other end side of the jig body A second guide portion that gradually decreases in diameter toward the head, a communication hole that connects the first guide portion and the second guide portion,
When the sample collection rod is guided by the first guide and inserted into the communication hole, the coiled sample collection piece guided from the second guide to the communication hole is removed from the sample collection rod. A pressing member that presses in the direction, presses the tip of the sampling rod into the inside of the coiled sampling piece, and attaches the coiled sampling piece to the tip of the sampling rod. Coil sample collection piece mounting jig.   2. The coiled sample collection piece mounting jig according to claim 1, wherein the sampling unit includes a hollow cylindrical cylinder having a cylindrical connecting portion at a tip thereof, and a pushing member slidable along an inner wall of the cylinder. And a cylindrical needle that communicates with the cylinder via the connecting portion, and a syringe that includes a sample collection rod that is connected to the tip of the pusher member and that can freely protrude and retract from the needle. Sample collection piece mounting jig.   3. The coiled sample collection piece mounting jig according to claim 2, wherein the communication hole includes a large diameter portion communicating with the first guide portion and a small diameter portion communicating with the second guide portion. A diameter-shaped part is provided with the length which can accommodate the said needle, The coiled sample collection piece mounting jig characterized by the above-mentioned.   4. The coiled sample collection piece mounting jig according to claim 1, wherein the sample collection rod is connected to a base portion having a diameter in a range of 0.13 to 0.15 mm and the base portion. A coiled-shaped sample piece having an inner diameter in the range of 0.15 to 0.3 mm and an outer diameter in the range of 0.17 to 0.36 mm. Sample collection piece mounting jig.