JP2016029399A - Gas chromatograph - Google Patents

Abstract

PROBLEM TO BE SOLVED: To improve workability under a condition that since a sealing connection part of a column is arranged on an upper depth of an oven, the sealing connection part is shadowed by a hand and cannot be easily viewed in sealing connection work of the column.SOLUTION: A both-end opened tube 5 composed of quartz glass or the like having visible light transmissivity and heat resistance is inserted into an oven 1 and light is transmitted from a light source 8 arranged on the outside of the oven 1 through an inner space of the tube in order to suppress heat transmission from the inside of the oven 1 to illuminate sealing connection parts 10 and 11.SELECTED DRAWING: Figure 1

Description

  The present invention relates to a gas chromatograph, and more particularly to illumination inside an oven.

A gas chromatograph, which is a type of analyzer, continuously flows a carrier gas as a mobile phase through a column packed with a stationary phase, and instantaneously introduces the mixed sample from the inlet of the column so that the mixed sample and the mobile phase are mixed together. This is a device for performing quantitative qualitative analysis by separating each component using a difference in moving speed based on a difference in adsorption property (affinity) of each component with respect to a stationary phase and a partition coefficient while moving in a column.

  A part of the gas chromatograph is constituted by the column, the sample vaporization chamber and the detector unit that are hermetically connected to both ends of the column, respectively. The mixed sample passes through the sample vaporization chamber and the column together with the carrier gas, and is introduced into the detector unit together with the detector gas introduced from the detector gas introduction path.

  In analysis using a gas chromatograph, it is usually necessary to select a column according to the purpose of the analysis. In addition, it is necessary to detach the column during maintenance. The column is placed in an oven and connected to a sample vaporization chamber and a detector section for detecting the separated sample. Usually, the sample vaporizing chamber and the connecting part between the detector part and the column are arranged in the upper part of the oven.

  The inside of the sample vaporization chamber is set to a pressure higher than the atmospheric pressure to supply gas to the column. If the connection between the column and the sample vaporization chamber and the detector is incomplete, leakage will occur at the connection. Adversely affect the analysis results.

  For this purpose, for example, a ferrule made of graphite is attached to both ends of the column and tightened with a nut to secure the sealing property between the column, the sample vaporizing chamber, and the detector unit. Furthermore, the “column insertion length” from the ferrule is determined to ensure analysis performance, and the length is adjusted when the column is mounted.

  FIG. 6 shows an outline of a conventional gas chromatograph. In the gas chromatograph, the sample vaporizing chamber 52, the detector unit 53, and the column 54 arranged in the upper part of the oven 51 are hermetically coupled at hermetic coupling units 60 and 61, respectively. As shown in the drawing, the mixed sample is introduced together with the carrier gas through the sample vaporization chamber 52 through the column 54 and introduced into the detector unit 53 together with the introduced detector gas.

FIG. 7 shows the connection state of the sample vaporizing chamber 52 and the column 54, taking the sample vaporizing chamber 52 as an example. By tightening the threaded portion 64N of the nut 64 screwed into the threaded portion 52N of the sample vaporizing chamber 52, the conical portions of the ferrule 63 penetrating the column 54 are pressed together, and the sample vaporizing chamber 52 and the ferrule 63, And the ferrule 63 and the column 54 are connected, and as a result, the sample vaporizing chamber 52 and the column 54 are hermetically connected.

  Patent Document 1 states that “the sample vaporizing chamber and the column are maintained at a predetermined high temperature by providing an inert gas conduction path for conducting an inert gas in addition to the carrier gas in the sample vaporizing chamber; "Effective use of air mixing prevention function in replacement of the product" is disclosed.

JP 2009-92672 A

  The outer diameter of the column that is normally used is about 0.3 to 0.8 mm, and it is necessary to insert it into the sample vaporizing chamber and the detector portion and a portion having an inner diameter of 1 mm that is a hermetic connection portion of the column. Furthermore, as described above, it is necessary to adjust the “column insertion length” from the ferrule to a specified length. In addition, since the sealed connection portion of the column is disposed in the upper back of the oven, when the column is sealed and connected, it becomes a shadow of the hand and it becomes difficult to visually recognize the sealed connection portion.

  In order to solve the above problem, it is conceivable to arrange a light source behind the oven in order to brighten the sealed connection part of the sample vaporization chamber and the detector part. The temperature is high and the light source cannot withstand such temperatures. Therefore, improvement in workability under the above conditions is required.

In order to solve the above problems, the present invention includes an oven for heating a sample, a sample vaporizing chamber for vaporizing the injected sample, a column into which the sample vaporized in the sample vaporizing chamber is introduced, In a gas chromatograph comprising: a detector that detects the sample that has passed through a column; and a ferrule and a fastening nut for hermetically connecting the sample vaporization chamber and the detector to the column inserted therein A double-sided open tube having a permeability and heat resistance equal to or higher than the operating temperature of the gas chromatograph, disposed across the left and right lateral walls of the oven, in the vicinity of the sealed connection portion of the column disposed inside the oven; Provided in at least one of a punch hole provided in both the inner and outer wall surfaces of the oven on the same axis as the both-end release pipe, and an inner wall surface or an outer wall surface of the punch hole A shield having transparency and the heat resistance which is obtained by and a light source disposed on the oven outside of said coaxial.

The present invention also provides an oven for heating a sample, a sample vaporizing chamber for vaporizing the injected sample, a column into which the sample vaporized in the sample vaporizing chamber is introduced, and the sample that has passed through the column A gas chromatograph comprising a detector section for detecting gas, a ferrule and a tightening nut for sealingly connecting the sample vaporizing chamber and the detector section and the column inserted therein, and is disposed inside the oven. In the vicinity of the sealed connecting portion of the column, a distal end sealing tube that is vertically disposed on both sides of the lateral wall of the oven and has heat resistance equal to or higher than the operating temperature of the gas chromatograph, and the distal end sealing A punch hole provided on both sides of the oven inner and outer wall surfaces coaxial with the tube, and provided in at least one of the inner wall surface and the outer wall surface of the punch hole A shield having transparency and the heat resistance which is obtained by and a light source disposed on the coaxially on opposite sides of the oven outside.

  Furthermore, the present invention provides an oven for heating a sample, a sample vaporization chamber for vaporizing the injected sample, a column into which the sample vaporized in the sample vaporization chamber is introduced, and the sample that has passed through the column A gas chromatograph comprising: a detector section for detecting gas; a ferrule and a tightening nut for sealingly connecting the sample vaporizing chamber and the detector section and the column inserted therein; Permeability provided in the side wall of the oven coaxial with the hole and the operating temperature of the gas chromatograph in the vicinity of the sealing hole of the column disposed inside the oven Transparency provided on at least one of the plate-shaped transparent member having the above heat resistance and the outer wall surface of the punched hole and the heat resistance And 蔽物, in which and a light source disposed on the coaxially on opposite sides of the oven outside.

  Further, according to the present invention, a shielding plate or a convex shielding cap having permeability and heat resistance may be provided in the punched holes on both the inner and outer wall surfaces of the oven.

  In the present invention, a reflection plate can be provided inside the both-end release tube. Furthermore, a reflection plate can also be provided in the inner or outer peripheral portion of the distal end sealed tube.

  In addition, the present invention may include a control device that supplies or cuts power to the light source in conjunction with opening and closing of a door provided in the oven.

By brightening the sample vaporization chamber and the sealing connection between the detector and the column, operations such as column replacement and maintenance inside the oven are facilitated. Moreover, the durability of the light source can be ensured by installing a light source outside the oven and taking measures to block heat transfer from the oven as much as possible.

The outline | summary of the gas chromatograph which is an Example of this invention is shown. (A) is a front view, and (b) is a side view (AA cross-sectional view). The outline of a gas chromatograph which is a modification example of the present invention is shown. (A) is a front view, and (b) is a side view (BB cross-sectional view). The enlarged view of the internal reflecting plate used for the deformation | transformation Example of this invention is shown. (A) is a front view and (b) is a top view. As another modified embodiment of the present invention, an attached state of the internal reflector to the both-end release tube is shown. (A) is a front view and (b) is a top view. The outline | summary of the gas chromatograph which is another modified example of this invention is shown. A front view is shown to (a), and a side view (CC sectional drawing) is shown to (b). An outline of a conventional gas chromatograph is shown. The connection state of a sample vaporization chamber and a column is shown.

  FIG. 1 shows an outline of a gas chromatograph as an embodiment of the present invention. 1A is a front view, and FIG. 1B is a side view (A-A cross-sectional view).

  The gas chromatograph is mainly composed of a case 15 that forms an outer shape, an oven 1 installed in the case 15, a door 16 of the oven 1, and a sample vaporizing chamber 2 and a detector unit 3 disposed on the top of the oven 1. Has been.

  The oven 1 is composed of an oven inner wall 13 and an oven outer wall 14 in which a heat insulating material 12 is sealed, and an internal temperature of the oven 1 is set by a heater (not shown) and a fan (not shown) installed in the oven 1. Is adjusted to a predetermined temperature. The sealed connection parts 10 and 11 of the sample vaporizing chamber 2 and the detector part 3 are exposed inside the oven 1 and are hermetically connected to the column 4 in the oven 1. As in the description of FIG. 5, quantitative qualitative analysis using a gas chromatograph is performed by introducing a mixed sample together with a carrier gas through a column through a sample vaporization chamber and introducing the detector gas together with the introduced detector gas. Is called.

  The oven 1 includes a double-sided release pipe 5 disposed across the left and right lateral walls of the oven inner wall 13 in the vicinity of the sealing connecting portions 10 and 11 in the oven 1, an inner wall punch hole 19 coaxial with the double-sided release pipe 5, and 20 and the coaxial outer wall punching holes 21 and 22 on the outer wall 14 of the oven. The inner wall shielding plate 6 and the both-end release pipe 5 are provided on the inner surface side of the inner wall punching holes 19 and 20, respectively. The outer wall shielding plate 7 and the light source 8 are fixed by fixing flanges 9 to the outer surface side of each.

  Both ends open tube 5, inner wall shielding plate 6 and outer wall shielding plate 7 are made of a material having a visible light permeability and a heat resistance of 450 ° C. or higher which is a use temperature of a gas chromatograph, for example, quartz glass or borosilicate glass. Has been.

Both end release tubes 5 are held in a state of being sandwiched between inner wall shielding plates 6 on both sides, and light sources 8 (for example, LED lamps) are disposed outside the outer wall shielding plates 7 on both sides. Therefore, the light of the light source 8 passes from the shielding plate 7 for the outer wall through the outer wall punching hole 21 (or 22), and through the air layer 23 (or 24) between the inner and outer walls of the oven, to the inner wall punching hole 19 (or 20) and the inner wall. The light passes through the shielding plate 6 and passes through the inside of the both end release tube 5 to illuminate the outside of the both end release tube 5.

Further, an external reflecting plate 27 is attached to the both end release tube 5, and the illumination light emitted from the both end release tube 5 is guided in the direction of the sealing connecting portions 10 and 11. An arc-shaped band 28 made of a spring plate is joined to the external reflection plate 27, and the external reflection plate 27 is fixed to the double-end release tube 5 by gripping the double-end release tube 5 with the band 28. Can do.

  In the gas chromatograph of the present invention, a sensor 17 (photo sensor, magnet switch, etc.) is installed on the door 16 to detect the opening and closing of the door 16, and when the door is open, the light source 8 is turned on and the door is closed. A control device 18 for controlling the light source 8 to turn off is sometimes provided.

FIG. 2 shows an outline of a gas chromatograph which is a modified embodiment of the present invention. 2A is a front view, and FIG. 2B is a side view (BB cross-sectional view).

The gas chromatograph includes a case 45 that forms an outer shape, an oven 31 installed in the case 45, a door 46 of the oven 31, and a sample vaporization chamber 3 disposed on the top of the oven 31.
2 and a detector section 33.

The oven 31 includes an oven inner wall 43 and an oven outer wall 4 in which a heat insulating material 42 is enclosed.
4, the internal temperature of the oven 31 is adjusted to a predetermined temperature by a heater (not shown) and a fan (not shown) installed in the oven 31. Seal connection portions 40 and 41 of the sample vaporizing chamber 32 and the detector portion 33 are exposed to the inside of the oven 31 and are sealingly connected to the column 34 in the oven 31. The quantitative qualitative analysis by gas chromatograph is shown in FIG.
As in the description of, the mixed sample passes through the column through the sample vaporization chamber together with the carrier gas,
This is performed by being introduced into the detector section together with the introduced detector gas.

  The oven 31 includes a front end sealing tube 35 disposed perpendicular to the oven inner wall 43 in the vicinity of the sealing connection portion 40 in the oven 31, an inner wall punch hole 49 coaxial with the front end sealing tube 35, and the outside of the oven. A coaxial outer wall punching hole 66 is provided, an inner wall convex shielding cap 36 and a tip sealing tube 35 are provided on the inner surface side of the inner wall punching hole 49, and an outer wall convex shielding cap 37 is provided on the outer surface side of the outer wall punching hole 66. A light source 38 (for example, an LED lamp) is fixed by a fixing flange 39.

  Further, the oven 31 includes a front end sealing tube 57 disposed perpendicular to the oven inner wall 43 in the vicinity of the sealing connection portion 41 in the oven 31, an inner wall punch hole 50 coaxial with the front end sealing tube 57, and the outside of the oven 31. The inner wall convex hole 25 has an inner wall convex shielding cap 25 and a distal end sealing tube 57 on the inner surface side of the inner wall hole 50, and the outer wall shielding plate 26 and A light source 38 (for example, an LED lamp) is fixed by a fixing flange 39.

  The distal end sealing tubes 35 and 57, the inner wall convex shielding caps 25 and 36, the outer wall convex shielding cap 37, and the outer wall shielding plate 26 are 450 ° C. or higher, which is the visible light transmission property and the operating temperature of the gas chromatograph. Made of a heat-resistant material such as quartz glass or borosilicate glass.

  Light from the light source 38 is transmitted from the outer wall convex shielding cap 37 through the inner wall convex shielding cap 36 through the air layer 68 between the inner and outer walls of the oven to the inside of the distal end sealing tube 35. Illuminate the outside. On the other side of the oven 31, the light from the light source 38 is transmitted from the outer wall shielding plate 26 through the inner wall convex shielding cap 25 through the air layer 69 between the inner and outer walls of the oven to the inside of the distal end sealing tube 57. Then, the outside of the distal end sealed tube 57 is illuminated. However, when one of the light sources 38 installed on the left and right can illuminate the sealing connection portions 40 and 41, either one of the end sealed tubes is used, and the other is not installed.

  FIG. 3 shows an enlarged view of the internal reflector used in the modified embodiment of the present invention, and FIG. 3A shows a front view and FIG. 3B shows a top view. The internal reflector 29 is attached to guide the illumination light emitted from the distal end sealing tube 35 in the direction of the sealing connecting portion 40. As shown in the enlarged view of FIG. 3, the internal reflection plate 29 has a shape that is held by the inner diameter portion of the distal end sealed tube 35. The internal reflection plate 29 can be used for the distal end sealed tube 57 as well. Furthermore, it is possible to use the above-described external reflection plate 27 for the end sealed tubes 35 and 57 instead of the internal reflection plate 29.

  By reducing the volume of the air layers 68 and 69 by the convex shielding caps 25 and 36 for the inner wall and the convex shielding cap 37 for the outer wall, heat transfer from the oven 31 to the light source 38 due to air convection is suppressed. Further, a radiation fin (not shown) can be attached to the light source 38 for heat dissipation of the light source 38.

  In the gas chromatograph of the present invention, a sensor 47 (photo sensor, magnet switch, etc.) is installed on the door 46 to detect the opening / closing of the door 46. When the door is open, the light source 38 is turned on and the door is closed. A control device 48 for controlling the light source 38 to turn off is sometimes provided.

  In addition, the combination of the shielding plate and the shielding cap attached to the punched holes on the inner and outer wall surfaces of the oven in the embodiment of FIG. 1 and the modified embodiment of FIG. 2 can be arbitrarily selected, and is not limited to the combinations shown in FIGS. .

  FIG. 4 shows the state of attachment of the internal reflector to the both-end release tube as another modified embodiment of the present invention, and FIG. 4A shows a front view and FIG. 4B shows a top view. Thus, the internal reflector 30 can be used in place of the external reflector 27 described above.

  FIG. 5 shows an outline of a gas chromatograph which is another modified embodiment of the present invention. FIG. 5A shows a front view, and FIG. 5B shows a side view (CC cross-sectional view).

  The gas chromatograph is disposed on a case 85 forming an outer shape, a side plate 89 disposed on the inside of the case 85, an oven 71 disposed in the case 85, a door 87 of the oven 71, and an upper portion of the oven 71. It consists of a sample vaporizing chamber 72 and a detector unit 73.

  The oven 71 is configured by an oven inner wall 83 and an oven outer wall 84 in which a heat insulating material 82 is enclosed, and an internal temperature of the oven 71 is set by a heater (not shown) and a fan (not shown) installed in the oven 71. Is adjusted to a predetermined temperature. Seal connection portions 80 and 81 of the sample vaporizing chamber 72 and the detector portion 73 are exposed to the inside of the oven 71 and are sealed and connected to the column 74 in the oven 71. As in the description of FIG. 6, quantitative qualitative analysis using a gas chromatograph is performed by introducing a mixed sample together with a carrier gas through a column through a sample vaporization chamber and introducing the detector gas together with the introduced detector gas. Is called.

  The oven 71 includes an inner wall punching hole 90 and the coaxial outer wall punching hole 91 outside the oven in the vicinity of the sealing connection portions 80 and 81 in the oven 71, and a transparent member 75 is provided on the inner surface side of the inner wall punching hole 90. The outer wall convex shielding cap 77 is fixed to the outer surface side of the outer wall punching hole 91 by a fixing flange 79. Further, the light source 78 (for example, an LED lamp) is fixed to the inner surface of the side plate 89 by a fixing flange 79 together with the light source convex shielding cap 76.

  The transparent member 75 is made of a material having a visible light permeability and a heat resistance of 450 ° C. or higher, which is the operating temperature of the gas chromatograph, such as quartz glass or borosilicate glass. In the gas chromatograph of this modified embodiment, a sensor 47 (photo sensor, magnet switch, etc.) is installed on the door 87 to detect the opening and closing of the door 87. When the door is open, the light source 78 is turned on. A control device 48 is provided to control the light source 78 to be off when closed.

  Light from the light source 78 illuminates the inside of the oven 71 from the convex shielding cap 77 for the outer wall through the transparent member 75 through the air layer 88 between the inner and outer walls of the oven. In FIG. 5, a left-right symmetrical structure is shown, but when one of the light sources 78 installed on the left and right can illuminate the sealing connection portions 80 and 81, either one is applied. In addition, what is shown with the same code | symbol used in FIGS. 1-7 represents the same thing, and has the same function.

1, 31, 51, 71 Oven 2, 32, 52, 72 Sample vaporization chamber 3, 33, 53, 73 Detector section 4, 34, 54, 74 Column 5 Both ends release pipe 6 Inner wall shielding plate 7, 26 For outer wall Shield plate 8, 38, 78 Light source 9, 39, 79 Fixing flange 10, 40, 60, 80 Sealed connection 11, 41, 61, 81 Sealed connection 12, 42, 82 Insulation 13, 43, 83 Oven inner wall 14 , 44, 84 Oven outer wall 15, 45, 85 Case 16, 46, 87 Door 17, 47 Sensor 18, 48 Controller 19, 20, 49, 50, 90 Inner wall punching hole 21, 22, 66, 67, 91 Outer wall removed Holes 23, 24, 68, 69, 88 Air layers 25, 36 Convex shielding cap for inner wall 27 External reflector 28 Bands 29, 30 Internal reflectors 35, 57 End sealed tubes 37, 77 Wall convex shielding cap 52N, 64N threaded portion 63 the ferrule 64 the nut 75 transparent member 76 convex shielding cap 86 fixing plate 89 side plate source

Claims (9)

  An oven for heating the sample, a sample vaporizing chamber for vaporizing the injected sample, a column into which the sample vaporized in the sample vaporizing chamber is introduced, and a detector unit for detecting the sample that has passed through the column A gas chromatograph comprising a ferrule and a tightening nut for sealingly connecting the sample vaporizing chamber and the detector section to the column inserted therein, and sealing the column disposed in the oven In the vicinity of the connecting portion, a both-end open pipe having a permeability and a heat resistance equal to or higher than the operating temperature of the gas chromatograph disposed across the left and right lateral walls of the oven, and both the inner and outer wall surfaces of the oven coaxial with the both-end open pipe And the permeability and heat resistance provided on at least one of the inner wall or the outer wall of the hole.蔽物 a gas chromatograph, characterized in that it and a light source disposed on the coaxially on opposite sides of the oven outside. An oven for heating the sample, a sample vaporizing chamber for vaporizing the injected sample, a column into which the sample vaporized in the sample vaporizing chamber is introduced, and a detector unit for detecting the sample that has passed through the column A gas chromatograph comprising a ferrule and a tightening nut for sealingly connecting the sample vaporizing chamber and the detector section to the column inserted therein, and sealing the column disposed in the oven In the vicinity of the connecting portion, a front end sealing tube that is vertically disposed from both sides of the side wall of the oven and has heat resistance equal to or higher than the operating temperature of the gas chromatograph, and the end sealing tube that is coaxial with the front end sealing tube Perforations provided on both sides of the oven inner and outer wall surfaces, and permeability and / or permeability provided on at least one of the inner wall surface and the outer wall surface of the hole. Shield and a gas chromatograph, characterized in that it and a light source disposed on the coaxially on opposite sides of the oven exterior with the heat-resistant.   An oven for heating the sample, a sample vaporizing chamber for vaporizing the injected sample, a column into which the sample vaporized in the sample vaporizing chamber is introduced, and a detector unit for detecting the sample that has passed through the column And a ferrule and a tightening nut for sealingly connecting the sample vaporizing chamber and the detector section and the column inserted therein, provided on both sides of the both inner and outer wall surfaces of the oven. Permeability and heat resistance equal to or higher than the operating temperature of the gas chromatograph disposed in the side wall of the oven on the same axis as the vent hole in the vicinity of the sealing hole of the column disposed in the oven and the column. A plate-shaped transparent member, a transparent and heat-resistant shield provided on at least one of the outer wall surfaces of the punched hole, Gas chromatograph, characterized in that it comprises a light source disposed on either side of the down outside on the coaxial, the.   The gas chromatograph according to claim 1, wherein a reflection plate is provided inside or outside the both-end release pipe.   The gas chromatograph according to claim 2, wherein a reflection plate is provided inside or on an outer peripheral portion of the distal end sealed tube.   The hole according to any one of Claims 1, 2, 4, and 5 comprising a shielding plate or a convex shielding cap having permeability and the heat resistance in the punched holes on both inner and outer wall surfaces of the oven. Gas chromatograph.   The gas chromatograph according to claim 3, wherein a shielding plate or a convex shielding cap having permeability and heat resistance is provided in a hole in the outer wall surface of the oven.   The gas chromatograph according to any one of claims 1 to 7, wherein a sealed connection portion of the column is disposed in an upper part of the oven.   The gas chromatograph according to any one of claims 1 to 8, further comprising a control device that supplies or cuts off power to the light source in conjunction with opening and closing of a door provided in the oven.

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