JP5772376B2 - Sample inlet using septum - Google Patents

Description

The present invention relates to a sample injection port provided in a sample introduction part of an analyzer , and relates to a sample injection port using a septum.

  For example, in a total organic carbon analyzer, a sample inlet is provided at the upper end of a combustion tube (TC combustion tube) for burning or decomposing a liquid sample (for example, water containing a suspension). The inlet is sealed with a disc-shaped septum to prevent leakage of carrier gas and generated carbon dioxide. When injecting a sample into the combustion tube, the injection needle of the injector that can be raised and lowered A sample injection nozzle is inserted into the septum and penetrates to the upper end of the combustion tube. The above septum is a molded body made of a fluororesin or the like, and is generally used for a sample inlet of a column such as a gas chromatograph.

JP 2007-93209 A JP-A-5-52827

  By the way, when a sample is injected from the sample injection port, there is a problem that the septum is slightly damaged by the sample injection nozzle, and the fine particle fragments enter the combustion tube. In particular, in the above-mentioned total organic carbon analyzer, since water containing a suspension is injected as a sample, there is a tendency that a nozzle having a relatively large diameter tends to be used, and septum fragments are likely to be generated. As a result, in the signal analysis, a carbon component signal of the septum itself is generated, which is an impediment to improvement in analysis accuracy.

The present invention has been made in view of the above circumstances, and its purpose is a sample injection port provided in a sample introduction part of an analyzer, which does not affect the analysis and has higher accuracy. and to provide a sample inlet using a septum that allows for analysis.

  In order to solve the above problems, in the septum of the present invention, an inverted frustoconical or cylindrical recess is provided in the disc-shaped septum body from the upper surface side, and the bottom of the recess is curved into a semicircular surface. At the same time, by forming a straight notch penetrating to the back surface at the center of the bottom, when the sample injection nozzle of the injector is inserted, the notch is pushed open and the sample injection nozzle passes, and the sample injection nozzle is removed. In this case, the notch is sealed by the restoring force of the material and the curved structure of the bottom. In the sample injection port of the present invention, the injector sample is formed by coaxially connecting three or more blocks each provided with a nozzle insertion hole in the center and arranging the above septum between the blocks. Airtightness was improved when the injection nozzle was inserted and when the sample injection nozzle was removed.

That is, the first gist of the present invention is a sample injection port for injecting a liquid sample into the sample introduction part of the analyzer, and a nozzle insertion hole through which a needle-like sample injection nozzle is inserted is provided at the center. is three or more blocks coupled to the coaxial configurations, between each block, respectively, septum through which the said sample injection nozzle when the liquid sample injection is interposed, the septum is elastic The outer shape is formed in a disc shape, and an inverted frustoconical or cylindrical recess is provided on the front surface of the disk, and the bottom of the recess has a shape curved in a semicircular surface, and the bottom In the center of the sample inlet , a notch extending in a direction orthogonal to the bending direction and penetrating to the back surface is provided.

The second gist of the present invention is a sample injection port for injecting a liquid sample into the combustion tube of the total organic carbon analyzer, centering on a nozzle insertion hole through which an injection needle-shaped sample injection nozzle is inserted. The upper block, the intermediate block and the lower block provided are configured to be coaxially coupled, and the lower end side of the lower block is configured to be attachable to the upper end of the combustion pipe, and between the upper block and the intermediate block, In addition, a septum is inserted between the intermediate block and the lower block so as to penetrate the sample injection nozzle when the liquid sample is injected, and the septum is formed of a rubber-elastic material and has a disk shape. In addition, an inverted frustoconical or cylindrical recess is provided on the front surface of the board, and the bottom of the recess has a shape curved in a semicircular surface, and the center of the bottom is orthogonal to the bending direction. It consists in the sample inlet, characterized in that cut through to and back side are extended in the direction.

  According to the present invention, when the sample injection nozzle of the injector is inserted into the sample introduction part of the analyzer, the septum itself is not damaged, the sample injection nozzle can be smoothly inserted, and when the sample injection nozzle is removed, Since the introduction portion can be hermetically sealed, there is no occurrence of an abnormal signal due to the septum, and a more accurate analysis is possible.

It is a figure which shows the structure of the septum which concerns on this invention, a part view (a) is a top view, a part view (b) is a bottom view, a part view (c) followed the AA line of the part view (a). The longitudinal sectional view and the fractional view (d) are longitudinal sectional views along the line BB in the fractional view (a). It is a figure which shows an example of the sample injection port which concerns on this invention, and is the longitudinal cross-sectional view fractured | ruptured along the centerline. It is a perspective view which shows the external appearance of the nozzle part of the sample injection port which concerns on this invention, and an injector.

  Embodiments of a septum and a sample inlet (hereinafter referred to as “injector”) according to the present invention will be described with reference to the drawings. The inlet of the present invention is applied to a sample introduction part for introducing a liquid sample of an analyzer, for example, a combustion tube (TC combustion tube) of a total organic carbon analyzer, a capillary column of a gas chromatograph, and the septum of the present invention. Is used for the above inlet.

  First, the septum of the present invention will be described. As shown in FIG. 2, the septum of the present invention denoted by reference numeral 1 in the figure is attached as a partition wall to the inlet 1A of the sample introduction part (for example, the combustion tube 8) of the analyzer as described above, and is used for liquid sample injection. At this time, it is used by penetrating an injection needle-like sample injection nozzle (hereinafter referred to as “injection nozzle”) 70. The septum 1 of the present invention is made of a flexible material having excellent heat resistance and chemical resistance and rubber elasticity, such as fluorine rubber, silicon rubber, and isoprene rubber, and is usually manufactured by injection molding these materials. The

  As shown in FIG. 1, in the septum 1, the outer shape of the main body 10 is formed in a disk shape, and an inverted frustoconical or cylindrical recess 11 is provided on the front surface (upper surface side) of the disk. Although it varies depending on the analyzer to be applied, the outer diameter of the main body 10 is about 8 to 14 mm, the thickness of the main body 10 is about 2 to 6 mm, the diameter of the depression 11 is about 3.5 to 10 mm, and the depression 11 described later. The thickness of the bottom is designed to be about 0.3 to 0.5 mm. As shown in FIGS. 1A, 1 </ b> C, and 1 </ b> D, an annular protrusion 12 that protrudes along the edge of the recess 11 is provided on the upper surface of the main body 10. Such a protrusion 12 is provided as a displacement stopper for axial alignment with the block when the septum 1 is interposed between the blocks of the injection port described later.

  Further, as shown in FIGS. 1B and 1C, on the bottom surface (lower surface) of the main body portion 10, an annular rib 13 having an outer diameter smaller than that of the protrusion 12 is concentric with the main body portion and the bottom surface. It is provided in a state protruding from. The outer diameter of the annular rib 13 is set to a size substantially corresponding to the inner diameter of the recess 11. The annular rib 13 is provided as a misalignment stop for axial alignment with the block, similarly to the projection 12 described above, and is provided to reinforce the bottom of the thin recess 11 and increase its restoring force. Although not shown, in order to further reinforce the bottom portion of the recess 11 and increase its restoring force, the center of the bottom surface (back surface) of the main body portion 10 has a linear shape extending over the annular rib 13. A rib may be provided along the bending direction of the bottom of the recess 11 described later.

  In the present invention, when the injection nozzle 70 of the injector is inserted into the injection port 1A (see FIG. 3), the injection nozzle 70 is smoothly passed through without damaging the septum 1, and the injection nozzle 70 is removed reliably. In order to seal the injection port, as shown in FIG. 1 (c), the bottom of the recess 11 has a shape curved in a semicircular surface, and FIGS. ), A notch 15 extending in the direction orthogonal to the bending direction and penetrating to the back surface is provided at the center of the bottom of the recess 11.

  Specifically, the bottom of the recess 11 has a curved surface that approximates the inner peripheral surface when the cylindrical body is broken along its center line. Further, the extending direction of the notch 15 is a direction along the direction in which the bottom of the recess 11 is not curved. The length of the cut 15 varies depending on the size and use of the main body 10, but is usually a length corresponding to 40 to 70% of the inner diameter of the recess 11.

  Next, the inlet of the present invention will be described. The injection port of the present invention is a device for injecting a liquid sample into the sample introduction part of the analyzer, and a nozzle insertion hole through which an injection needle-like injection nozzle 70 (see FIGS. 2 and 3) is inserted is provided at the center. It is configured by connecting three or more blocks coaxially. The septum 1 is interposed between the blocks. Hereinafter, the inlet 1A provided in the combustion pipe 8 of the total organic carbon analyzer will be described as an example.

  As shown in FIG. 2, the inlet 1A of the present invention is an inlet for injecting a liquid sample (water containing a suspension) into a combustion tube 8 which is a sample introduction part of the total organic carbon analyzer. The upper block 2, the intermediate block 3 and the lower block 4 each having a nozzle insertion hole 2 c, 3 c, and 4 c through which the injection needle-like injection nozzle 70 is inserted are coaxially connected. And the lower end side of the lower block 4 is comprised so that attachment to the upper end of the combustion pipe 8 is possible.

  The upper block 2 is formed in a two-stage cylindrical shape having a small diameter at the lower stage, and a nozzle insertion hole 2c is provided at the center thereof. A screw for coupling to the intermediate block 3 is provided on the outer peripheral surface of the small diameter portion 23 of the upper block 2. The upper portion of the nozzle insertion hole 2c has a funnel shape that is gradually expanded in diameter toward the upper end of the upper block 2 in order to smoothly guide the injection nozzle into the nozzle insertion hole 2c when the injection nozzle 70 of the injector is inserted. It is formed. The lower end of the nozzle insertion hole 2c is expanded in diameter as an inverted shallow dish-shaped space into which the upper end of the septum 1 is fitted.

  Similar to the upper block 2 described above, the intermediate block 3 has an outer shape formed in a two-stage cylindrical shape having a small diameter at the lower stage, and a nozzle insertion hole 3c is provided at the center thereof. A screw for coupling to the lower block 4 is provided on the outer peripheral surface of the small diameter portion 34 of the intermediate block 3. A block coupling hole 32 for screwing the small diameter portion 23 of the upper block 2 is provided on the upper end side of the intermediate block 3, and the upper end of the nozzle insertion hole 3 c opened to the block coupling hole 32 is connected to the septum 1. The diameter of the space is increased. Further, the lower end of the nozzle insertion hole 3c is expanded in diameter as an inverted shallow dish-like space portion into which the upper end portion of the second septum 1 is fitted.

  The lower block 4 has an outer shape formed in a two-stage cylindrical shape with a small diameter at the lower stage, and is provided with a flange portion used for an attaching / detaching operation to a main body block 5 described later, and a nozzle at the center of the lower block 4 An insertion hole 4c is provided. A screw for coupling to the main body block 5 is provided on the outer peripheral surface of the large diameter portion 45 of the lower block 4. On the upper end side of the large diameter portion 45 of the lower block 4, a block coupling hole 43 for screwing the small diameter portion 34 of the intermediate block 3 is provided. Furthermore, the upper end of the nozzle insertion hole 4 c that opens in the block coupling hole 43 is expanded in diameter as a space for accommodating the septum 1.

  The small diameter portion 46 of the lower block 4 is provided with a gas introduction chamber 40 that communicates with the nozzle insertion hole 4c and is open to the lower end side of the lower block. Further, the lower side of the gas introduction chamber 40 is formed as a short-axis cylindrical space portion whose diameter is expanded to a size that allows the upper end of the combustion pipe 8 to be loosely fitted, and further, below the small-diameter portion 46 of the lower block 4. The end surface is formed into an inversely tapered surface that is gradually expanded in diameter from the short-axis cylindrical space.

  In order to ensure airtightness with the main body block 5 to be described later, a circumferentially continuous groove is provided on the outer peripheral surface of the substantially middle portion of the small-diameter portion 46 of the lower block 4 and an O-ring is provided in the groove. 61 is mounted. Furthermore, an O-ring 62 for ensuring airtightness with the upper end of the combustion pipe 8 is disposed inside the reverse tapered surface of the lower end surface of the small diameter portion 46. Further, in order to introduce the carrier gas into the gas introduction chamber 40 at a portion below the O-ring 61 of the small diameter portion 46, a gas introduction groove 41 continuous in the circumferential direction is provided, and gas is introduced from the gas introduction groove. A plurality of gas introduction holes 42 communicating with the introduction chamber 40 are opened.

  On the other hand, in the analyzer, the main body block 5 is attached to the place where the combustion tube 8 is disposed, specifically, the upper frame (frame) 90 of the electric furnace 91 as the mounting structure portion of the lower block 4. The main body block 5 is formed in a two-stage cylindrical shape, and the upper cylindrical portion is configured as a block coupling hole 54 into which the large-diameter portion 45 of the lower block 4 is screwed. The lower cylindrical portion of the main body block 5 is configured as a block fitting hole 56 into which the small diameter portion 46 of the lower block 4 is fitted. A combustion tube mounting hole 58 having a smaller diameter than the block fitting hole 56 and capable of being inserted through the upper end portion of the combustion tube 8 is opened below the block fitting hole 56, that is, at the center of the lower end portion of the main body block 5. The

  A gas supply port 51 that communicates with the gas introduction groove 41 of the small diameter portion 46 when the lower block 4 is coupled is provided in the lower cylindrical portion of the main body block 5 along the radial direction of the cylindrical portion. The gas supply port 51 is a connection port for connecting a carrier gas flow path. That is, in the inlet 1A shown in FIG. 2, the carrier gas supplied from the gas supply port 51 is introduced into the gas introduction chamber 40 through the gas introduction groove 41 and the gas introduction hole 42 of the lower block 4 and supplied to the combustion pipe 8. Configured to be.

  In the inlet 1A of the present invention, by disposing a plurality of septums 1, leakage of gas from the combustion pipe 8 is surely prevented. That is, the septum 1 is interposed between the upper block 2 and the intermediate block 3 and between the intermediate block 3 and the lower block 4.

  Specifically, the first septum 1 (the upper septum in FIG. 2) is accommodated in the expanded diameter space at the upper end of the nozzle insertion hole 3 c that opens in the block coupling hole 32 on the upper end side of the intermediate block 3. When the upper block 2 is screwed to the intermediate block 3, the upper end of the septum 1 is fitted into the inverted shallow dish-like space on the lower end side of the small diameter portion 23 of the upper block 2, and the septum 1 is slightly pressurized. As a result, the airtightness between the upper block 2 and the intermediate block 3 is ensured, and the nozzle insertion hole 2c and the nozzle insertion hole 3c are separated from each other by the septum 1.

  Similarly, the second septum 1 (the lower septum in FIG. 2) is accommodated in the enlarged diameter space at the upper end of the nozzle insertion hole 4 c that opens in the block coupling hole 43 of the large diameter portion 45 of the lower block 4. . When the intermediate block 3 is screwed to the lower block 4, the upper end of the septum 1 is fitted into the inverted shallow dish-like space on the lower end side of the small diameter portion 34 of the intermediate block 3, and the septum 1 is slightly pressurized. By doing so, the airtightness between the intermediate block 3 and the lower block 4 is ensured, and the nozzle insertion hole 3c and the nozzle insertion hole 4c are isolated by the septum 1.

  In order to mount the injection port 1A of the present invention in the analyzer, for example, first, the septum 1 (second septum) is arranged at the bottom of the block coupling hole 43 of the lower block 4 and the block coupling hole 43 of the lower block 4 is placed. The intermediate block 3 is coupled to the lower block 4 by tightening the small diameter portion 34 of the intermediate block 3. Next, the septum 1 (first septum) is disposed at the bottom of the block coupling hole 32 of the intermediate block 3, and the small-diameter portion 23 of the upper block 2 is tightened into the block coupling hole 32 of the intermediate block 3. The upper block 2 is coupled to the above.

  Subsequently, an O-ring 61 is attached to the outer peripheral surface of the small diameter portion 46 of the lower block 4. On the other hand, an O-ring 62 is also attached in advance to the upper end portion of the combustion tube 8 arranged in the analyzer. Then, by inserting the small diameter portion 46 of the lower block 4 into the block fitting hole 56 of the main body block 5 and tightening the large diameter portion 45 of the lower block 4 into the block coupling hole 54 of the main body block 5, The lower block 4 is joined. Regarding the assembly order, the upper block 2 and the intermediate block 3 may be combined first, and then the intermediate block 3 may be connected to the lower block 4.

  In the inlet 1A assembled as described above, the nozzle insertion holes 2c, 3c and 4c of the upper block 2, the intermediate block 3 and the lower block 4 are connected coaxially, and these nozzle insertion holes are the first and second nozzle insertion holes. Sealed with a second septum 1. The gas supply port 51 of the main body block 5 is connected to the gas introduction chamber 40 via the gas introduction groove 41 and the gas introduction hole 42 of the lower block 4, the combustion pipe 8 opens into the gas introduction chamber 40, and the gas introduction The interior of the chamber 40 and the combustion pipe 8 is kept airtight by O-rings 61 and 62.

  In the total organic carbon analysis, first, in order to measure the concentration of total carbon (TC) in the sample, while supplying high-purity air as a carrier gas from the gas supply port 51 to the combustion tube 8 through the gas introduction chamber 40, A liquid sample (water with suspension) is injected with an injector. As shown in FIG. 3, the injector for sample injection includes a syringe (not shown) for collecting a sample from a sample column, and a movable nozzle portion 7 for injecting a sample pushed out from the syringe into the analyzer. An injection nozzle 70 is provided at the lower end of the nozzle portion.

  When injecting a liquid sample with an injector, as shown in FIG. 3, the nozzle part 7 of the injector located at the upper part of the injection port 1A is lowered, and the injection nozzle 70 is inserted from the nozzle insertion hole 2c of the upper block 2, The injection nozzle 70 is inserted to the combustion pipe 8 through the nozzle insertion hole 3 c of the intermediate block 3 and the nozzle insertion hole 4 c of the lower block 4. In that case, in each septum 1, since the notch 15 is pushed open by the injection nozzle 70, the injection nozzle 70 can be passed smoothly without the septum itself being damaged.

  After inserting the injection nozzle 70 into the upper part of the combustion tube 8 and operating the syringe of the injector to inject the liquid sample, the nozzle part 7 is raised and the injection nozzle 70 is removed from the injection port 1A. At that time, in each septum 1, the cut 15 is sealed by the restoring force of the material and the curved structure of the bottom of the recess 11, so that no gas leaks out of the combustion tube 8.

  In addition, in the injection port 1A of the present invention, the three blocks of the upper block 2, the intermediate block 3, and the lower block 4 are connected coaxially, and the septum 1 is disposed between each block, so that the injection nozzle Airtightness can be further enhanced in the operation of inserting 70 and the operation of removing injection nozzle 70.

  That is, according to the septum 1 and the injection port 1A of the present invention, when the injection nozzle 70 of the injector is inserted into the combustion tube 8 which is the sample introduction part of the total organic carbon analyzer, the septum 1 itself is not damaged and is smoothly When the injection nozzle 70 can be inserted and the injection nozzle 70 is removed, the combustion tube 8 can be hermetically sealed, so that an abnormal signal due to the septum 1 is not generated and analysis with higher accuracy is possible. Further, according to the present invention, if a failure occurs in the analyzer and the pressure in the combustion pipe 8 rises abnormally, the septum 1 can also function as a relief valve. The present invention is not limited to the total organic carbon analyzer, and can be applied to sample inlets of various analyzers that inject and analyze a liquid sample.

DESCRIPTION OF SYMBOLS 1: Septum 10: Main-body part 11: Recess 15: Notch 1A: Sample injection port 2: Upper block 2c: Nozzle insertion hole 3: Intermediate block 3c: Nozzle insertion hole 4: Lower block 40: Gas introduction chamber 4c: Nozzle insertion hole 5: Body block 51: Gas supply port 58: Combustion tube mounting hole 61: O ring 62: O ring 7: Injector nozzle portion 70: Sample injection nozzle 8: Combustion tube (sample introduction portion of analyzer)
91: Electric furnace

Claims (2)

A sample injection port for injecting a liquid sample into the sample introduction portion of the analyzer, and three or more blocks having a nozzle insertion hole through which a needle-like sample injection nozzle is inserted at the center are coaxially coupled. Each of the blocks is provided with a septum that penetrates the sample injection nozzle when the liquid sample is injected. The septum is formed of a rubber-elastic material and has a disk shape. In addition, an inverted frustoconical or cylindrical depression is provided on the front surface of the board, and the bottom of the depression has a shape curved in a semicircular surface, and the center of the bottom is in a direction perpendicular to the bending direction. And a notch extending through the back surface is provided . A sample injection port for injecting a liquid sample into the combustion tube of the total organic carbon analyzer, an upper block, an intermediate block, and a lower block provided with a nozzle insertion hole through which a needle-like sample injection nozzle is inserted at the center And the lower end of the lower block is configured to be attachable to the upper end of the combustion pipe, and between the upper block and the intermediate block and between the intermediate block and the lower block. Each of them is provided with a septum that penetrates the sample injection nozzle during liquid sample injection, and the septum is formed of a rubber elastic material in a disk shape and has an inverted frustoconical shape on the front surface of the disk. Alternatively, a cylindrical recess is provided, and the bottom of the recess has a shape curved in a semicircular surface, and the center of the bottom is extended in a direction perpendicular to the bending direction and penetrates to the back surface. Sample inlet, characterized in that the notch is provided.

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